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  • 101
    Electronic Resource
    Electronic Resource
    Neue Phosphor-verbrückte Übergangsmetallcarbonyl-Komplexe Die Kristallstrukturen von [Re2(CO)7(PtBu)3], [Co4(CO)10(PtBu)2], [Ir4(CO)6(PtBu)6] und [Ni4(CO)10(PiPr)6] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 58-66 
    Details
    ISSN: 0044-2313
    Keywords: Cyclotriphosphanes ; multinuclear phosphorus-bridged complexes of Re, Mn, Co, Ir and Ni ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Phosphorus-bridged Transition Metal Carbonyl Complexes. The Crystal Structures of [Re2(CO)7(PtBu)3], [Co4(CO)10(PtBu)2], [Ir4(CO)6(PtBu)6], and [Ni4(CO)10(PiPr)6],(PtBu)3 reacts with [Mn2(CO)10], [Re2(CO)10], [Co2(CO)8] and [Ir4(CO)12] to form the multinuclear complexes [M2(CO)7(PtBu)3] (M = Re (1), Mn (5)), [Co4(CO)10(PtBu)2] (2) and [Ir4(CO)6(PtBu)6] (3). The reaction of (PiPr)3 with [Ni(CO)4] leads to the tetranuclear cluster [Ni4(CO)10(PiPr)6] (4). The complex structures were obtained by X-ray single crystal structure analysis: (1: space group P1 (Nr. 2), Z = 2, a = 917.8(3) pm, b = 926.4(3) pm, c = 1 705.6(7) pm, α = 79.75(3)°, β = 85.21(3)°, γ = 66.33(2)°; 2: space group C2/c (Nr. 15), Z = 4, a = 1 347.7(6) pm, b = 1 032.0(3) pm, c = 1 935.6(8) pm, β = 105.67(2)°; 3: space group P1 (Nr. 2), Z = 4, a = 1 096.7(4)pm, b = 1 889.8(10)pm, c = 2 485.1(12) pm, α = 75.79(3)°, β = 84.29(3)°, γ = 74.96(3)°; 4: space group P21/c (Nr. 14), Z = 4, a = 2 002.8(5) pm, b = 1 137.2(8) pm, c = 1 872.5(5) pm, β = 95.52(2)°).
    Notes: Das Cyclotriphosphan (PtBu)3 reagiert mit [Mn2(CO)10], [Re2(CO)10], [Co2(CO)8] und [Ir4(CO)12] unter Bildung der Mehrkernkomplexe [M2(CO)7(PtBu)3] (M = Re (1), Mn (5)), [Co4(CO)10(PtBu)2] (2) und [Ir4(CO)6(PtBu)6] (3). Die Umsetzung von (PiPr)3 mit [Ni(CO)4] führt zu dem vierkernigen Cluster [Ni4(CO)10(PiPr)6] (4). Die Strukturen der Komplexe konnten durch Einkristall-Röntgenstrukturanalyse aufgeklärt werden (1: Raumgruppe P1 (Nr.2), Z = 2, a = 917,8(3)pm, b = 926,4(3)pm, c = 1 705,6(7)pm, α = 79,75(3)°, β = 85,21(3)°, γ = 66,33(2)°; 2: Raumgruppe C2/c (Nr. 15), Z = 4, a = 1 347,7(6) pm, b = 1 032,0(3) pm, c = 1 935,6(8) pm, β = 105,67(2)°; 3: Raumgruppe P1 (Nr. 2), Z = 4, a = 1 096,7(4) pm, b = 1 889,8(10) pm, c = 2 485,1(12) pm, α = 75,79(3)°, β = 84,29(3)°, γ = 74,96(3)°; 4: Raumgruppe P21/c (Nr. 14), Z = 4, a = 2 002,8(5) pm, b = 1 137,2(8) pm, c = 1 872,5(5) pm, β = 95,52(2)°).
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200110
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  • 102
    Electronic Resource
    Electronic Resource
    Synthese und Struktur von (Ph3PAu)3Mn(CO)4Professor Wolfgang Sawodny zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 786-790 
    Details
    ISSN: 0044-2313
    Keywords: Trigold manganese cluster ; (Ph3PAu)3Mn(CO)4 ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of (Ph3PAu)3Mn(CO)4Photolysis of (Ph3PAu)Mn(CO)5, Ph3PAuN3 and Ph3PAuNCO yields (Ph3PAu)3Mn(CO)4 (1). 1 crystallizes in the monoclinic space group P21/n with a = 1 031.3(1); b = 3 095.2(3), c = 3 386.3(3) pm; β = 97.58(3)°; Z = 8. The crystal structure contains two symmetry independent clusters 1 of the same geometry. Their inner core MnAu3 forms a rhombus with distances Mn—Au of about the same lengths between 258.4(4) and 262.0(4) pm. The distances Au—Au range from 276.6(2) to 281.3(2) pm. The bonding in 1 is discussed and compared with those of (Ph3PAu)3Co(CO)3 having the same total number of electrons but a tetrahedral framework.
    Notes: Photolyse einer Mischung von (Ph3PAu)Mn(CO)5, Ph3PAuN3 und Ph3PAuNCO in THF führt zur Bildung von (Ph3PAu)3Mn(CO)4 (1). 1 kristallisiert in der monoklinen Raumgruppe P21/n mit a = 1 031,3(1); b = 3 095,2(3), c = 3 386,3(3) pm; β = 97,58(3)°; Z = 8. Die Kristallstruktur enthält zwei symmetrieunabhängige Cluster 1 gleicher Gestalt, deren MnAu3-Gerüst die Struktur einer Raute mit nahezu gleich langen Mn—Au-Abständen zwischen 258,4(4) und 262,0(4) pm aufweist. Die Au—Au-Abstände liegen zwischen 276,6(2) und 281,3(2) pm. Die Bindungsverhältnisse in 1 werden diskutiert und mit denjenigen des Clusters (Ph3PAu)3Co(CO)3 mit gleicher Gesamtelektronenanzahl aber tetraedrischer Gerüststruktur verglichen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200504
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  • 103
    Electronic Resource
    Electronic Resource
    Zur Kenntnis eines Kalium-Barium-Oxogallat/-zinkats KBa6Ga7Zn4O21 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 155-159 
    Details
    ISSN: 0044-2313
    Keywords: Pottasium ; barium ; gallium ; zinc oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Potassium-Barium-Oxogallate/-zincate KBa6Ga7Zn4O21Single crystals of KBa6Ga7Zn4O21 were prepared by a flux technique and investigated by X-ray work. It crystallizes with trigonal symmetry, space group C43v-P31c, a = 10.790, c = 11.822 Å, Z = 2. The crystal structure is characterized by a Ga/ZnO4-tetrahedra network filled by K+ and Ba2+ ions.
    Notes: Einkristalle von KBa6Ga7Zn4O21 wurden mit Schmelzmitteltechnik dargestellt und röntgenographisch untersucht. Diese Verbindung kristallisiert mit trigonaler Symmetrie, Raumgruppe C43v-P31c mit a = 10,790, c = 11,822 Å, Z = 2. Die Kristallstruktur ist durch ein Ga/ZnO4-Tetraedergerüst ausgezeichnet, welches mit K+- und Ba2+-Ionen aufgefüllt ist.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200125
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  • 104
    Electronic Resource
    Electronic Resource
    Alkaline Earth Transition Metal Antimonides AT4Sb12 (A = Ca, Sr, Ba; T = Fe, Ru, Os) with LaFe4P12-Structure (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1028-1032 
    Details
    ISSN: 0044-2313
    Keywords: Synthesis ; crystal structure ; CaFe4Sb12 ; SrRu4Sb12 ; BaRu4Sb12 ; polyantimonides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Erdalkali-Übergangsmetall-Antimonide AT4Sb12 (A = Ca, Sr, Ba; T = Fe, Ru, Os) mit LaFe4P12-StrukturDie Titelverbindungen wurden durch Reaktion von CaSb2, SrSb2 bzw. BaSb3 mit den Übergangsmetallen und Antimon in evakuierten Quarzglasröhrchen hergestellt. Sie kristallisieren in der kubischen LaFe4P12-Struktur, die aus Röntgen-Einkristall-Daten für CaFe4Sb12, SrRu4Sb12 und BaRu4Sb12 zu Restwerten von R = 0,014, 0,016 bzw. 0,014 verfeinert wurde. Die thermischen Parameter der Erdalkaliionen nehmen mit abnehmender Ionengröße zu. Die Sb—Sb-Abstände sind in der Eisen-Verbindung größer als in den beiden Ruthenium-Verbindungen, was sich auf eine stärkere Besetzung von antibindenen Sb—Sb-Zuständen bei der Eisen-Verbindung zurückführen läßt.
    Notes: The title compounds were prepared by reaction of CaSb2, SrSb2, or BaSb3 with the transition metals and antimony in sealed silica tubes. They crystallize with the cubic LaFe4P12-structure, which was refined from single-crystal X-ray data of CaFe4Sb12, SrRu4Sb12, and BaRu4Sb12 to residuals of R = 0.014, 0.016, and 0.014, respectively. The thermal parameters of the alkaline earth ions increase with decreasing ionic size. The Sb—Sb distances are greater in the iron compound than they are in the two ruthenium compounds. This is rationalized to be due to a larger portion of electrons in antibonding Sb—Sb states in the iron compound.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200613
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  • 105
    Electronic Resource
    Electronic Resource
    Synthese und Struktur von [(Ph3PAu)6Co(CO)2](PF6) und [(Ph3PAu)7Co(CO)2](PF6)2 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 192-198 
    Details
    ISSN: 0044-2313
    Keywords: Gold cluster compounds ; cobalt carbonyl gold cluster compounds ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of [(Ph3PAu)6Co(CO)2](PF6) and [(Ph3PAu)7Co(CO)2](PF6)2By the reaction of (Ph3PAu)4Co[(CO)3]+ with OH- in the presence of excess Ph3PAuCl the larger cluster cations [(Ph3PAu)6Co(CO)2]+ (1) and [(Ph3PAu)7Co(CO)2]2+ (2) can be built up with 1 being the main product. 1 crystallizes with PF-6 as counterion in the monoclinic space group C2/c with a = 3008.3(6); b = 1339.1(2); c = 2909.4(6) pm; β = 103.08(1)°; Z = 4. The inner core of the cluster cation 1 with the symmetry C2 has the form of a bicapped trigonal bipyramid with the heteroatom in equatorial position, and distances Au—Au between 280.4(1) and 288.4(1) pm and Co—Au between 254.9(1) and 257.1(2) pm. 2 · (PF6)2 crystallizes in the triclinic space group P1 with a = 2155.7(1); b = 1720.6(1); c = 3543.6(1) pm; α = 91.89(1)°; β = 97.51(1); γ = 89.92(1)°; Z = 4. The unit cell contains two symmetry independent cluster cations 2 of about the same geometry. The cluster skeleton Au7Co can be described as fragment of an icosahedron formed by seven gold atoms with the Co atom in its center. The Au—Au distances range from 274.8(3) to 332.6(3) pm, and the Co—Au distances are 256.8(6) to 264.7(5) pm. The bonding in 1 and 2 is discussed.
    Notes: Durch Reaktion von [(Ph3PAu)4Co(CO)3]+ mit OH- in Gegenwart von überschüssigem Ph3PAuCl können die goldreicheren Clusterkationen [(Ph3PAu)6Co(CO)2]+ (1) und [(Ph3PAu)7Co(CO)2]2+ (2) aufgebaut werden, wobei 1 als Hauptprodukt anfällt. 1 kristallisiert mit PF-6 als Gegenion in der monoklinen Raumgruppe C2/c mit a = 3008,3(6); b = 1339,1(2); c = 2909,4(6) pm; β = 103,08(1)°; Z = 4. Im Clusterkation 1 mit der Symmetrie C2 bildet das CoAu6-Gerüst die Struktur einer zweifach überkappten trigonalen Bipyramide mit dem Heteroatom in äquatorialer Position. Die Au—Au-Abstände liegen zwischen 280,4(1) und 288,4(1) pm die Co—Au-Abstände zwischen 254,9(1) und 257,1(2) pm. 2 · (PF6)2 kristallisiert triklin in der Raumgruppe P1 mit a = 2155,7(1); b = 1720,6(1); c = 3543,6(1) pm; α = 91,89(1)°; β = 97,51(1)°; γ = 89,92(1)°; Z = 4. Die Elementarzelle enthält zwei symmetrieunabhängige Clusterkationen 2 mit nahezu gleicher Gestalt, deren Au7Co-Gerüst als leicht verzerrtes Ikosaederfragment aus sieben Au-Atomen mit dem Co-Atom im Zentrum beschrieben werden kann. Die Au—Au-Abstände variieren von 274,8(3) bis 332,6(3) pm, die Co—Au-Abstände betragen 256,8(6) bis 264,7(5) pm. Die Bindungsverhältnisse in 1 und 2 werden diskutiert.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200203
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  • 106
    Electronic Resource
    Electronic Resource
    Ein neuer Strukturtyp bei Oxoiridaten mit quadratisch-planaren [IrO4]4--Gruppen: K2Na2[IrO4], ein Raumnetz ∞3[Na2IrO4] mit Kanälen. (Mit einer Anmerkung zu Rb2Na2[IrO4]) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 225-233 
    Details
    ISSN: 0044-2313
    Keywords: Oxoiridates ; [IrO4]4- groups ; crystal structure ; magnetic measurements ; MAPLE calculation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Type of Structure in Oxoiridates with Square-planar Groups [IrO4]4-: K2Na2[IrO4], a Network ∞3[Na2IrO4] with Channels (With a Remark on Rb2Na2[IrO4])For the first time magnificent dark red cuboid single crystals of K2Na2[IrO4] were prepared by annealing intimate mixtures of a) KO0.51, Na2O2, IrO2 and Ir-powder (molar proportions 3.02 : 1.40 : 1.00 : 1.00; Ag-bomb, 740°C, 54 d) and of b) KO0.51, Na2O and IrO2 (molar proportions K : Na : Ir = 2.20 : 2.20 : 1.00; Ag-bomb, 760°C, 57 d) respectively. The oxide crystallizes mP36, space group P21/c with a = 600.35(6) pm, b = 1111.2(1) pm, c = 933.0(1) pm and β = 113.14(1)°.Structure determination via four-circle diffractometer data (Siemens AED 2, Mo-Kα-Radiation) for all 2347 unique reflexions (merged from 9397 Io(hkl) gave R = 0.0357 and Rw = 0.0340. K2Na2[IrO4] crystallizes in a new type of structure. The oxide is antiferromagnetic as magnetic measurements showed (TN = 32 K, Θ = -60.2 K (single crystals) and -49.2 K (powder) respectively, μ = 3.06 μB (single crystals) and 2.93 μB (powder) respectively).Effective coordination numbers ECoN, mean fictive ionic radii MEFIR and the Madelung part lattice energy MAPLE as well as the charge distributions CHARDI and CHARDINO are calculated and discussed.
    Notes: Erstmals wurde K2Na2[IrO4] durch Tempern inniger Gemenge von (a) KO0,51, Na2O2, IrO2 und Ir-Pulver (molares Verhältnis 3,02 : 1,40 : 1,00 : 1,00; Ag-Bombe, 740°C, 54 d) bzw. (b) KO0,51, Na2O und IrO2 (molares Verhältnis K : Na : Ir = 2,20 : 2,20 : 1,00; Ag-Bombe, 760°C, 57 (d) in Form prächtiger, dunkelroter, quaderförmiger Einkristalle erhalten. Das Oxid kristallisiert in P36, Raumgruppe P21/c mit a = 600,35(6) pm; b = 1111,2(1) pm; c = 933,0(1) pm und β = 113,14(1)°. Die Struktur wurde anhand von Vierkreisdiffraktometerdaten aufgeklärt (Siemens AED 2, Mo-Kα-Strahlung, Graphit). Für alle 2347 symmetrieunabhängigen Reflexe (gemittelt aus 9397 gemessenen Io(hkl)) war schließlich R = 0,0357 und Rw = 0,0340. K2Na2[IrO4] kristallisiert in einem neuen Strukturtyp. Magnetische Messungen zeigten, daß das Oxid antiferromagnetisch ist (TN = 32 K, Θ = -60,2K (Einkristalle) bzw. -49,2K (Pulver); μ = 3,06 μB (Einkristalle) bzw. 2,93 μB (Pulver)).Effektive Koordinationszahlen ECoN, Mittlere Fiktive Ionenradien MEFIR und der Madelunganteil der Gitterenergie MAPLE sowie die Ladungsverteilungen nach CHARDI und CHARDINO werden berechnet und diskutiert.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200206
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  • 107
    Electronic Resource
    Electronic Resource
    Das erste Titanat mit „Stuffed Pyrgoms“: RbNa3Li12[TiO4]4 = RbNa3Li8{Li[TiO4]}4Professor Gerhard Fritz zum 75. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2064-2069 
    Details
    ISSN: 0044-2313
    Keywords: RbNa3Li12[TiO4]4 ; orthotitanate ; crystal structure ; MAPLE ; CHARDI ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Titanate with „Stuffed Pyrgoms“: RbNa3Li12[TiO4]4 = RbNa3Li8{Li[TiO4]}4By heating a well grounded mixture of the binary oxides Rb2O, Na2O, Li2O, and TiO2 [Rb:Na:Li:Ti = 1.1:3.1:12.5:4.0; 780°C, 41 d] we obtained RbNa3Li8{Li[TiO4]}4 as colourless platelike crystals. This first titanate with „stuffed pyrgoms“ is isostructural with RbNa3Li8{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4 and CsKNaLi9{Li[SiO4]}4 [2]. The compound crystallizes tetragonal I4/m with a = 1 125.8(1) pm and c = 652.4(1) pm (Guinier-Simon-Data, Z = 2). The structure was determined by four-cyrcle-data (Siemens AED2, MoKα-) and leds to the residual values R = 3.7% and Rw = 3.1% (additional data see text). The Madelung Part of Lattice Energy (MAPLE), Effective Coordination Numbers (ECoN), Mean Fictive Ionic Raddii (MEFIR) and the Charge Distribution in Solids (CHARDI) are calculated and discussed.
    Notes: Durch Tempern eines innigen Gemenges der binären Oxide Rb2O, Na2O, Li2O und TiO2 [Rb:Na:Li:Ti = 1,1:3,1:12,5:4,0; 780°C, 41 d] wurde RbNa3Li8{Li[TiO4]}4 in Form von farblosen Plättchen erhalten. Das erste Titanat mit „stuffed pyrgoms“ ist isotyp zu RbNa3Li8{Li[SiO4]}4, CsKNa2Li8{Li[SiO4]}4 und CsKNaLi9{Li[SiO4]}4 [2]. Die Verbindung kristallisiert tetragonal I4/m mit den Gitterkonstanten a = 1 125,8(1) pm und c = 652,4(1) pm (Guinier-Simon-Daten, Z = 2). Die Struktur wurde mit Vierkreisdiffraktometerdaten (Siemens AED2, 657Io(hkl), MoKα-) aufgeklärt und führte zu den Residualwerten R = 3,7% und Rw = 3,1% (weitere Daten siehe Text). Der Madelunganteil der Gitterenergie (MAPLE), Effektive Koordinationszahlen (ECoN), Mittlere Fiktive Ionenradien (MEFIR) sowie die Ladungsverteilung (CHARDI) werden berechnet und diskutiert.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946201208
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  • 108
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    Electronic Resource
    Chalkogenohalogenogallate(III) und -indate(III): Eine neue Verbindungsklasse in der dritten Hauptgruppe. Synthese und Struktur von [Ph4P]2[In2SX6], [Et4N]3[In3E3Cl6] · MeCN und [Et4N]3[Ga3S3Cl6] · THF (X = Cl, Br; E = S, Se)Professor Wilhelm Preetz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1234-1246 
    Details
    ISSN: 0044-2313
    Keywords: Thio-chloro-indates ; thio-bromo-indates ; seleno-chloro-indates ; thio-chloro-gallates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chalcogenohalogenogallates(III) and -indates(III): A New Class of Compounds for Elements of the Third Main Group. Preparation and Structure of [Ph4P]2[In2SX6], [Et4N]3[In3E3Cl6] · MeCN and [Et4N]3[Ga3S3Cl6] · THF (X = Cl, Br; E = S, Se)[In2SCl6]2-, [In2SBr6]2-, [In3S3Cl6]3-, [In3Se3Cl6]3-, and [Ga3S3Cl6]3- were synthesised as the first known chalcogenohalogeno anions of main group 3 elements. [Ph4P]2[In2SCl6] (1) (P1; a = 10.876(4) Å, b = 12.711(6) Å, c = 19.634(7) Å, α = 107.21(3)°, β = 96.80(3)°, γ = 109.78(3)°; Z = 2) and [Ph4P]2[In2SBr6] (2) (C2/c; a = 48.290(9) Å, b = 11.974(4) Å, c = 17.188(5) Å, β = 93.57(3)°, Z = 8) were prepared by reaction of InX3, (CH3)3SiSSi(CH3)3 and Ph4PX (X = Cl, Br) in acetonitrile. The reaction of MCl3 (M = Ga, In) with Et4NSH/Et4NSeH in acetonitrile gave [Et4N]3[In3S3Cl6] · MeCN (3) (P21/c; a = 17.328(4) Å, b = 12.694(3) Å, c = 21.409(4) Å, β = 112.18(1)°, Z = 4), [Et4N]3[In3Se3Cl6] · MeCN (4) (P21/c; a = 17.460(4) Å, b = 12.816(2) Å, c = 21.513(4) Å, β = 112.16(2)°, Z = 4), and [Et4N]3[Ga3S3Cl6] · THF (5) (P21/n; a = 11.967(3) Å, b = 23.404(9) Å, c = 16.260(3) Å, β = 90.75(2)°, Z = 4). The [In2SX6]2- anions (X = Cl, Br) in 1 and 2 consist of two InSX3 tetrahedra sharing a common sulfur atom. The frameworks of 3, 4 and 5 each contain a six-membered ring of alternating metal and chalcogen atoms. Two terminal chlorine atoms complete a distorted tetrahedral coordination sphere around each metal atom.
    Notes: [In2SCl6]2-, [In2SBr6]2-, [In3S3Cl6]3-, [In3Se3Cl6]3- und [Ga3S3Cl6]3- wurden als erste bisher bekannte Chalkogenohalogenoanionen von Elementen der 3. Hauptgruppe dargestellt. [Ph4P]2[In2SCl6] (1) (P1; a = 10,876(4) Å, b = 12,711(6) Å, c = 19,634(7) Å, α = 107,21(3)°, β = 96,80(3)°, γ = 109,78(3)°; Z = 2) und [Ph4P]2[In2SBr6] (2) (C2/c; a = 48,290(9) Å, b = 11,974(4) Å, c = 17,188(5) Å, β = 93,57(3)°, Z = 8) werden durch Reaktion von InX3, (CH3)3SiSSi(CH3)3 und Ph4PX (X = Cl, Br) in Acetonitril gebildet. [Et4N]3[In3S3Cl6] · MeCN (3) (P21/c; a = 17,328(4) Å, b = 12,694(3) Å, c = 21,409(4) Å, β = 112,18(1)°, Z = 4), [Et4N]3[In3Se3Cl6] · MeCN (4) (P21/c; a = 17,460(4) Å, b = 12,816(2) Å, c = 21,513(4) Å, β = 112,16(2)°, Z = 4) und [Et4N]3[Ga3S3Cl6] · THF (5) (P21/n; a = 11,967(3) Å, b = 23,404(9) Å, c = 16,260(3) Å, β = 90,75(2)°, Z = 4) können durch Umsetzung von MCl3 (M = Ga, In) mit Et4NSH (3), (5) bzw. Et4NSeH (4) in Acetonitril (3), (4) bzw. Tetrahydrofuran (5) erhalten werden. In den Kristallstrukturen der Titelverbindungen 1 bis 5 liegen isolierte Anionen und Kationen vor. Die [In2SCl6]2-- und [In2SBr6]2--Anionen in 1 und 2 lassen sich als Anordnung zweier über ein gemeinsames Schwefelatom eckenverknüpfter InSCl3- bzw. InSBr3- Tetraeder beschreiben. Die anionischen Teilstrukturen in 3, 4 und 5 werden durch drei Metallatome, die über μ2-E-Atome (E = Schwefel, Selen) zu einem Sechsring miteinander verbunden sind, aufgebaut, wobei zwei Chloratome an jedem Metallatom dessen verzerrt-tetraedrische Koordination vervollständigen.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200718
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    Einführung eines terminalen Halogenoliganden in diorgano-verbrücke Dirhenium- und Molybdän-Rhenium-Komplexanionen in Gegenwart eines Amidinkations (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1664-1668 
    Details
    ISSN: 0044-2313
    Keywords: Dirhenium complex anion ; rheniummolybdenum complex anion ; NMR data ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Insertion of a Terminal Halogeno Ligand into Diorgano-bridged Dirhenium and Rhenium-Molybdenum Complex Anions in the Presence of an Amidin Cation and the Isomerization ProcessesThe equimolar reaction of in situ generated anion Anions Re2(μ-PCy2)(CO)8- (Re—Re) in the presence of a steric expansive amidine cation DBUH+ with bromine and iodine in tetrahydrofuran solution gave the two isomers Re2(PCy2)(CO)8X (Re—Re) and Re2(μ-PCy2)(μ-X)(CO)8 (X = Br, I), of which the isomer with a terminal X ligand as major product was formed under maintenance of the Re—Re bond. The monotropic isomerization process of Re2(μ-PCy2)(CO)8I runs thermically relative slowly, but more rapid in photochemical and electrochemical processes. The analogeous reaction of the heterometallic anion ReMo(η5-C5H5)(μ-PPh2)(CO)6- with iodine delivers opposite to the former reaction mainly the bridged isomer ReMo(η5-C5H5)(μ-PPh2μ-I)(CO)6 besides ReMo(η5-C5H5)(μ-PPh2)(CO)6I. The obtained complexes were characterized by means of v(CO) and 31P NMR spectroscopic measurements. Single-crystal analyses led to the subsequent metal - metal bond lengths: Re—Re of 308.0(1) pm in Re2(μ-PCy2)(CO)8Br and Re—Mo of 313.6(1) pm in ReMo(η5-C5H5)(μ-PPh2)(CO)6I.
    Notes: Die äquimolare Umsetzung des in situ gebildeten Anions Re2(μ-PCy2)(CO)8 (Re—Re) in Gegenwart eines sterisch anspruchsvollen Amidinkations DBUH+ mit Brom und Jod in Tetrahydrofuranlösung bei 20°C ergab jeweils von beiden Isomeren Re2(μ-PCy2)(CO)8X (Re—Re) und Re2(μ-PCy2)(μ-X)(CO)8 (X = Br, I) überwiegend dasjenige mit terminal gebundenem Halogenoliganden unter Aufrechterhaltung der Re—Re-Bindung. Die monotrope Isomerisierung von Re2(μ-PCy2)(CO)8I verläuft thermisch relativ langsam, aber photochemisch und elektrochemisch schneller. Die analoge Umsetzung des heterometallischen Anions ReMo(η5-C5H5)(μ-PPh2)(CO)6 mit Jod lieferte demgegenüber bevorzugt das verbrückte Isomer ReMo(η5-C5H5)(μ-PPh2)(μ-I)(CO)6 neben ReMo(η5-C5H5)(μ-PPh2)(CO)6I. Die erhaltenen Komplexe wurden durch v(CO)- und 31P NMR-spektroskopische Daten charakterisiert. Einkristall-Röntgenstrukturanalysen führten zu folgenden Metall - Metall-Bindungslängen: Re—Re von 308,0(1) pm in Re2(μ-PCy2)(CO)8Br und Re—Mo von 313,6(1) pm in ReMo(η5-C5H5)(μ-PPh2)(CO)6I.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200927
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    Neue ternäre Selenide der Lanthanide durch Reduktion der SesquiselenideProfessor Reinhard Schmutzler zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1698-1701 
    Details
    ISSN: 0044-2313
    Keywords: Ternary selenides of lanthanides ; preparation ; crystal structure ; electronic structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Ternary Selenides of Lanthanoides by Reduction of SesquiselenidesThe compounds MLn2Se3 (M = Na; Ln = La—Sm) and MLn8Se12 (M = Na, Ca; Ln = La—Sm) were prepared by reduction of the corresponding lanthanide sesquiselenides with sodium and calcium, respectively, for the first time. Further-more MLa8Se12 (M = Sr, Eu) could be obtained in an analogous way. All compounds were characterized by chemical analysis and X-ray powder diffraction. The electronic structures of these compounds were investigated by band structure calculations and magnetic measurements.
    Notes: Die Verbindungen MLn2Se3 (M = Na, Ln = La—Sm) und MLn8Se12 (M = Na, Ca; Ln = La—Sm) wurden durch Reduktion der entsprechenden Lanthanidsesquiselenide mit Natrium bzw. Calcium erstmals dargestellt. Weitere Selenide MLa8Se12 (M = Sr, Eu) konnten analog erhalten werden. Die dargestellten Verbindungen wurden analytisch und röntgenographisch charakterisiert. Zur Bestimmung der elektronischen Struktur dieser Verbindungen wurden Bandstrukturrechnungen und magnetische Messungen durchgeführt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201006
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  • 111
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    Diorganoindium-Kationen. Die Kristallstruktur von [Mes2In][BF4] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 847-850 
    Details
    ISSN: 0044-2313
    Keywords: Diorganoindium cations ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Diorganoindium Cations. The Crystal Structure of [Mes2In][BF4](PhCH3)2In and Mes3In react with BF3 · OEt2 in a ratio of 3:4 at 80°C in toluene to the corresponding salts [R2In][BF4] [R = PhCH2 (1), Mes (2)]. The same results could be obtained, when the diorganoindium fluorides (PhCH2)2InF and Mes2InF were treated with BF3 · OEt2 at 80°C in toluene. 1 und 2 were characterized by NMR-, IR- und MS-techniques. The arrangement of the ions in 2 could be established by an X-ray structure determination. The cations and anions of 2 are forming infinite chains. The metal centers are coordinated by two BF4--ions, so that every In atom possesses a distorted octahedral coordination sphere.
    Notes: (PhCH2)3In und Mes3In reagieren mit BF3 · OEt2 im Verhältnis 3:4 bei 80°C in Toluol zu den entsprechenden Salzen [R2In][BF4] [R = PhCH2 (1), Mes (2)]. Zum selben Ergebnis gelangt man, wenn die Diorganoindiumfluoride (PhCH2)2InF und Mes2InF mit BF3 · OEt2 bei 80°C in Toluol behandelt werden. 1 und 2 wurden mittels NMR- und IR-Spektroskopie sowie Massenspektrometrie charakterisiert. Die Anordnung der Ionen in 2 konnte durch eine Röntgenstrukturanalyse aufgeklärt werden. 2 bildet danach unendliche Ketten aus Kationen und Anionen, wobei durch eine chelatartige Anordnung zweier BF4--Ionen an jedes Metallzentrum eine verzerrt oktaedrische Koordinationssphäre der Indiumatome resultiert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200516
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    Kristallstruktur von Hexamincyclotriphosphazen, P3N3(NH2)6Professor Friedo Huber zum 65. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 965-968 
    Details
    ISSN: 0044-2313
    Keywords: Hexamine cyclotriposphazene ; crystal growth ; crystal structure ; hydrogen-bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Hexamine Cyclotriphosphazene, P3N3(NH2)6In the presence of KNH2 hexamine cyclotriphosphazene semi ammoniate (molar ratio 12:1) in NH3 gives crystals of solvent free P3N3(NH2)6 within 5 d at 130°C and p(NH3) = 110 bar. The structure was solved by X-rax methods: P3N3(NH2)6: P21/c, Z = 4, a = 10.889(6) Å, b = 5.9531(6) Å, c = 13.744(8) Å, β = 97.83(3)°, Z(Fo) = 1 721 with (Fo)2 ≥ 3σ(Fo)2, Z(var.) = 157, R/Rw = 0,036/0,041The structure contains columns of molecules P3N3(NH2)6 all in the same orientation. The six-membered rings within one molecule have boat conformation. The columns are stacked together in a way that one is surrounded by four others shifted by half a lattice constant in direction [010]. Strong hydrogen bridge-bonds N—H…N connect molecules within the columns and between them.
    Notes: Bei Umsetzungen von Hexamincyclotriphosphazensemiammoniakat mit KNH2 (Molverhältnis 1:12, 5 d, T = 130°C, P(NH3) = 110 bar) in NH3 wurden Kristalle von ammoniakfreiem P3N3(NH2)6 als Nebenprodukt erhalten. Die Struktur dieser Verbindung wurde röntgenographisch bestimmt: P3N3(NH2)6: P21/c, Z = 4, a = 10,889(6) Å, b = 5,9531(6) Å, c = 13,744(8) Å, β = 97,83(3)°, Z(Fo) = 1 721 für (Fo)2 ≥ 3σ(Fo)2, Z(Parameter) = 157, R/Rw = 0,036/0,041In der Struktur liegen Säulen deckungsgleich gestapelter Moleküle P3N3(NH2)6 mit wannenförmiger Konformation vor. In nächster Umgebung befinden sich vier weitere Säulen, die um eine halbe Gitterkonstante in Richtung [010] entlang der Staperlrichtung gegenüber einer Bezugssäule versetzt sind. Starke Wasserstoffbrückenbidungen N—H⋅⋅⋅N verknüpfen die Moleküle sowohl zwischen den Säulen als auch in Säulenrichtung.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200602
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    AuTa14S2  -  Zentrierte (Au,Ta)13-Ikosaeder organisiert nach dem Motiv einer kubisch dichten PackungProfessor Friedo Huber zum 65. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 969-976 
    Details
    ISSN: 0044-2313
    Keywords: AuTa14S2 ; tantalum sulfides ; crystal structure ; metal icosahedra ; tetrahedral close packed structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: AuTa14S2 - Centred (Au,Ta)13 Icosahedra Organized According to the Motif of a Cubic Close PackingThe tantalum-rich phases of composition AuxTa15-xS2 (0.4 〈 x 〈 1.1) were prepared by arc-melting of appropriate compressed mixtures (Au, Ta, Ta1.35S2) and subsequent annealing of the samples in sealed molydenum crucibles. Brittle crystals with silver lustre were grown in tantalum ampoules at 1 700 K within two days using iodine as a chemical transport agent.In contrast to Vegard's rule the lattice parameters of the rhombohedral phases which are isostructural with Pd15P2, shrink with increasing gold content. The structures were determined from Rietveld fits of powder X-ray diffraction spectra and confirmed by a crystal structure analysis of a merohedral twinned crystal of Au0.7Ta14.3S2: a = 747.7(2) pm, α = 59.84(2)°, R3, Z = 1, 760 reflections (F2 〉 2σ(F2)), 30 variables, R(F) = 0.048. The parts of the volumina of the domains with distinct orientations are 0.346(4) and 0.654.Topologically the structure corresponds to a cubic close packed arrangement of Ta12-icosahedra with all non-tetrahedral interstices being filled. Gold accumulates preferentially in the centres of the icosahedra. The remaining metal atoms - two per formula and site - populate the „octahedral sites“ which are encased in stretched polyhedra limited by 32 triangulated faces. The „tetrahedral sites“ are occupied by the sulfur atoms which themselves have a ninefold, triangulated tetrakaidecahedral coordination. The complete occupation of interstices together with the specific orientation of the gold stabilized icosahedral (Au,Ta)13-clusters ensure a tetrahedral close packing of all atoms. The distortions of the packing are quantitatively analysed in terms of dihedral angles and deviations of the tetrahedral edge lengths from the mean and are compared with those of other tcp structures.
    Notes: Die tantalreichen Phasen AuxTa15-xS2 (0,4 〈 x 〈 1,1) wurden durch Aufschmelzen entsprechender Gemenge von Ta1,35S2 und den Metallen und nachfolgendes Tempern der Reguli in zugeschweißten Molybdäntiegeln hergestellt. Silbern glänzende, spröde Kristalle der neuen Phase wurden mit Iod als chemischem Transportmittel in einer Tantalampulle bei 1 700 K in 2 Tagen gezüchtet.Die Gitterkonstanten der rhomboedrisch kristallisierenden, mit Pd15P2 isostrukturellen Phasen kontrahieren mit zunehmendem Goldgehalt. Die Struktur wurde über Rietveld-Anpassungen von Röntgen-Diffraktogrammen bestimmt und durch die Strukturverfeinerung eines meroedrisch verzwillingten Kristalls der Zusammensetzung Au0,7Ta14,3S2 bestätigt: a = 747,7(2) pm, α = 59,84(2)°, R3, Z = 1, 760 Reflexe (F2 〉 2σ(F2)), 30 Variable, R(F) = 0,048. Die Volumenanteile der unterschiedlich orientierten Domänen sind 0,346(4) und 0,654.Die Struktur entspricht topologisch einer kubisch dichten Packung von Ta12-Ikosaedern, in der alle, nicht von Tetraedern eingeschlossenen Hohlräume von Atomen besetzt sind: Gold reichert sich bevorzugt im Zentrum der Ikosaeder an, die verbleibenden zwei Metallatome, die sich im Innern eines gestreckten, von Dreiecken begrenzten 32-Flächners befinden, besetzen die „Oktaederlücken“. In den „Tetraederlücken“ befinden sich die Schwefelatome. Sie sind neunfach tetrakaidekaedrisch von Tantalatomen koordiniert. Die durch Gold stabilisierten (Au,Ta)13-Cluster sind so zueinander orientiert, daß sie zusammen mit den Atomen in den anderen Lücken eine tetraedrisch dicht gepackte (tcp-) Struktur bilden, deren Verzerrungsgrad über eine Analyse der Diederwinkel und Kantenlängen der Tetraeder quantifiziert und mit dem anderer tcp-Strukturen verglichen wird.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200603
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    Structural investigations and luminescence of In2Ge2O7 and In2Si2O7Dedicated to Professor Heinrich Oppermann on his 60th Birthday (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1965-1970 
    Details
    ISSN: 0044-2313
    Keywords: Indium digermanate ; indium disilicate ; crystal structure ; indium luminescence ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturuntersuchungen und Lumineszenz von In2Ge2O7 und In2Si2O7Eine Rietveld-Pulverdiagramm-Methode erlaubt die Bestimmung der genauen Strukturen von Thortveitit verwandten In2Ge2O7 und In2Si2O7 Oxyden (Raumgrupe C2/m, Z = 2). Die Verbindungen wurden unter normalem Druck hergestellt. Die Lumineszenz unter 160 und 200 K sollte die Messung der Umwelt Neutrinobestrahlung erlauben. Sie scheint die Folge eines inneren Ladungstransfers in den Indium Sauerstoff Polyedern zu sein. Die optischen Resultate wurden an Hand der bestimmten Strukturen und der chemischen Bindungen diskutiert und mit Werten für andere Indiumoxyde verglichen.
    Notes: The crystal structures of the ordinary pressure forms of indium digermanate In2Ge2O7 and disilicate In2Si2O7 have been studied from X-ray powder diffraction data by Rietveld refinement. They are closely related to that of the thortveitite which crystallizes in the monoclinic system with the space group C2/m and Z = 2. They show luminescence properties below 160 K and 200 K respectively. The luminescence is discussed in terms of crystal structure and compared to that of some other luminescent indium oxides.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201121
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    Tellur-Polykationen stabilisiert durch Nioboxidhalogenide: Synthese und Kristallstrukturen von Te7NbOBr5 und Te7NbOCl5Professor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1971-1975 
    Details
    ISSN: 0044-2313
    Keywords: Tellurium ; niobium oxytrihalides ; poly(heptatellurium(2+)) ; tetrachlorooxoniobate (1-) ; tetrabromooxoniobate (1-) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tellurium Cations stabilized by Niobium Oxytrihalides: Synthesis and Crystal Structure of Te7NbOBr5 and Te7NbOCl5The reaction of Te2Br with NbOBr3 in a sealed evacuated glass ampoule at 225°C yields Te7NbOBr5 in form of bright black needles. Te7NbOCl5 is obtained from tellurium, TeCl4 and NbOCl3 at 220°C. Both compounds crystallize orthorhombic in the space group Pcca (Te7NbOBr5: a = 2 651,9(4) pm, b = 836.6(1) pm, c = 794.6(1) pm; Te7NbOCl5: a = 2 597.7(5) pm, b = 805.1(1) pm, c = 791.2(1) pm). The crystal structure determinations show that Te7NbOBr5 and Te7NbOCl5 are built of one-dimensional polymeric tellurium cations, one-dimensional associated pyramidal NbOX4 groups (X = Cl, Br) and isolated halide anions. Magnetic properties of Te7NbOX5 were determined and confirm the expected diamagnetism. Te7NbOX5 can thus be formulated as ∞1[Te72+] ∞1[NbOX4-] (X-). The charge distribution in the structure type Te7MOX5 (M = W, Nb; X = Cl, Br) became clear by synthesis and characterisation of the two niobium containing compounds.
    Notes: Durch Reaktion von Te2Br mit NbOBr3 in einer evakuierten Glasampulle bei 225°C entsteht Te7NbOBr5 in Form von schwarzglänzenden, stäbchenförmigen Kristallen. Te7NbOCl5 wird aus Te, TeCl4 und NbOCl3 bei 220°C erhalten. Beide Verbindungen kristallisieren im orthorhombischen Kristallsystem in der Raumgruppe Pcca (Te7NbOBr5: a = 2 651,9(4) pm, b = 836,6(1) pm, c = 794,6(1) pm; Te7NbOCl5: a = 2 597,7(5) pm, b = 805,1(1) pm, c = 791,2(1) pm). Die Kristallstrukturanalysen zeigen, daß Te7NbOBr5 und Te7NbOCl5 aus eindimensionalen polymeren Tellur-Kationen, eindimensionalen Strängen von pyramidalen, über O-Atome assoziierten NbOX4-Einheiten und aus isolierten Halogenidionen aufgebaut sind. Magnetische Messungen bestätigen den erwarteten Diamagnetismus und zeigen, daß Nb in der formalen Oxidationsstufe + V vorliegt. Die ionische Schreibweise lautet daher ∞1[Te72+] ∞1[NbOX4-] (X-). Die Synthese und Charakterisierung der beiden niobhaltigen Vertreter klärt die Ladungsverteilung im Strukturtyp Te7MOX5 (M = W, Nb; X = Cl, Br).
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201122
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    Ein neues Samariumnitridsulfid: Sm4N2S3 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2003-2007 
    Details
    ISSN: 0044-2313
    Keywords: Samarium nitride sulfide ; Sm4N2S3 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Samarium Nitride Sulfide: Sm4N2S3The oxidation of samarium with sulfur in the presence of SmCl3 and NaN3 as nitrogen source (molar ratio: 12:9:4:2, evacuated silica vessel, some NaCl as flux, 850°C, 7 d) yields Sm4N2S3 as lath-shaped, dark red single crystals. The by-products (NaCl and NaSm2Cl6) are rinsed with water from the crude product.The crystal structure of Sm4N2S3 (monoclinic, C2/m (no. 12), Z = 2, a = 1 318.04(12), b = 391.57(2), c = 1 031.76(9) pm, β = 130.874(6)°, R = 0.036, Rw = 0.031) contains two crystallographically different Sm3+, both in sixfold coordination of the anions. Besides distorted octahedra [(Sm1)N3S3] and [(Sm2)NS5], tetrahedra [(N3-)(Sm43+)] connected via two cis-oriented edges to form chains ∞1[N(Sm1)3/3(Sm2)1/1]3+ build up the Mayn structural feature. These are arranged in the fashion of a closest packing of rods and held together by two crystallographically different S2- anions which take care for charge neutrality and three-dimensional interconnection.
    Notes: Bei der Oxidation von Samarium mit Schwefel in Gegenwart von SmCl3 und NaN3 als Stickstoff-Quelle (molares Verhältnis: 12:9:4:2, evakuierte Quarzglasampulle, etwas NaCl als Flußmittel, 850°C, 7 d) fällt Sm4N2S3 in Form von stäbchenförmigen, dunkelroten Einkristallen an. Die Nebenprodukte (NaCl und NaSm2Cl6) werden mit Wasser aus dem Rohprodukt herausgelöst.In der Kristallstruktur von Sm4N2S3 (monoklin, C2/m (Nr. 12), Z = 2, a = 1 318,04(12); b = 391,57(2); c = 1 031,76(9) pm; β = 130,874(6)°; R = 0,036; Rw = 0,031) liegen zwei kristallographisch unterschiedliche Sm3+ in jeweils sechsfacher Koordination der Anionen vor. Neben verzerrten Oktaedern [(Sm1)N3S3] und [(Sm2)NS5] bilden Tetraeder [(N3-)(Sm3+)4], über zwei cis-ständige Kanten zu Ketten ∞1[(Sm1)3/3(Sm2)1/1]3+ verknüpft, das strukturelle Hauptmerkmal. Nach Art einer dichtesten „Stabpackung“ gebündelt, werden letztere durch zwei kristallographisch unterschiedliche S2- zusammengehalten, die für den Ladungsausgleich und die drei-dimensionale Vernetzung sorgen.
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    URL: http://dx.doi.org/10.1002/zaac.19946201128
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    Nitrido-Sodalithe. I Synthese, Struktur und Eigenschaften von Zn7-xH2x[P12N24]Cl2 mit 0 ≤ x ≤ 3 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2014-2019 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorus nitrides ; nitrido sodalites ; synthesis ; crystal structure ; i.r. data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitrido Sodalites. I Synthesis, Crystal Structure, and Properties of Zn7-xH2x [P12N24]Cl2 with 0 ≤ x ≤ 3The nitrido sodalites Zn7-xH2x[P12N24]Cl2 with 0 ≤ x ≤ 3 are obtained by heterogeneous pressure-ammonolysis of P3N5 at presence of ZnCl2 (T = 650°C). These compounds are available too by reaction of ZnCl2, (PNCl2)3, and NH4Cl at 700°C. The crystal structures of four representatives of the above mentioned compounds have been refined by the Rietveld full-profile technique using X-ray powder diffractometer data (I43m, a = 821.61(4) to 824.21(1) pm, Z = 1). In the solid a three-dimensional framework of corner-sharing PN4-tetrahedra occurs (P—N: 163.6 pm, P—N—P: 125.6°, mean values) which is isosteric with the sodalite type of structure. In the center of the β-cages Cl- ions have been found, which are tetrahedrally coordinated by Zn2+ ions. The Zn2+ ions are statistically disordered. According to the phase-width observed (0 ≤ x ≤ 3) the Zn2+ ions may be partially replaced each by two hydrogen atoms which on the other hand are covalently bonded to nitrogen atoms of the P—N framework. The IR-spectra of these compounds show characteristic vibrations.
    Notes: Die Nitrido-Sodalithe Zn7-xH2x[P12N24]Cl2 mit 0 ≤ x ≤ 3 wurden durch heterogene Druckammonolyse von P3N5 in Gegenwart von ZnCl2 (T = 650°C) dargestellt. Die Verbindungen sind auch zugänglich durch Umsetzung von ZnCl2, (PNCl2)3 und NH4Cl bei 700°C. Die Kristallstrukturen von vier ausgewählten Vertretern der obigen Verbindungsreihe wurden auf der Basis von Röntgen-Pulverdiffraktometerdaten mit Hilfe der Rietveld-Methode verfeinert (I43m, a = 821,61(4) bis 824,21(1) pm, Z = 1). Im Festkörper liegt eine dreidimensionale Gerüststruktur allseitig eckenverknüpfter PN4-Tetraeder vor (P—N: 163,6 pm, P—N—P: 125,6°, Mittelwerte), die dem Sodalith-Typ entspricht. Im Zentrum der β-Käfige befinden sich Cl--Ionen, die ihrerseits tetraedrisch durch Zn2+-Ionen umgeben sind. Die Zn2+-Positionen sind statistisch besetzt und gemäß der angegebenen Phasenbreite (0 ≤ x ≤ 3) kann ein Teil der Zn2+-Ionen durch jeweils zwei H-Atome ersetzt werden, die ihrerseits kovalent an Stickstoffatome des P—N-Gerüstes gebunden sind. Im IR-Spektrum der Verbindungen werden charakteristische Schwingungsbanden beobachtet.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201130
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    Rheniumselenidtelluride Re2SexTe5-x: Die Struktur von Re6Se8Te7Institut für Anorganische Chemie der Universität Gerhard-Domagk-Str. 1 D-53121 Bonn (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1861-1866 
    Details
    ISSN: 0044-2313
    Keywords: Re6Se8Te7 ; rhenium chalcogenides cluster compounds ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Rhenium Selenidetellurides Re2SexTe5-x: The Structure of Re6Se8Te7Well-crystallized rhenium selenidetellurides of the Re2Te5-type structure were prepared from the elements in evacuated sealed quartz glas tubes at 1 130 K within 14 d. The orthorhombic lattice parameters of the phases shrink with increasing selenium content from a = 1 304.9(1) - 1 255.8(2) pm, b = 1 297.5(1) - 1 260.0(2) pm, and c = 1 425.1(1) - 1 408.2(1) pm. The phase width ends at composition Re2Se2.7Te2.3. An X-ray structure analysis of a crystal of composition Re6Se8Te7 was performed. Selenium and tellurium atoms differ structurally completely: Whereas the selenium atoms are separated within distorted octahedral [Re6Se8] clusters, the tellurium atoms form homonuclear bonded bicyclic [Te(Te3)2] units. They also link the clusters which are arranged according to the motif of a cubic closest packing.
    Notes: Gemischte Selenidtelluride vom Re2Te5-Typ sind durch Umsetzung der Elemente in evakuierten Quarzglasampullen unter systemeigenem Dampfdruck (1 130 K, 14 d) grobkristallin zugänglich. Die Gitterkonstanten der orthorhombisch kristallisierenden Phasen kontrahieren mit zunehmendem Selengehalt: a = 1 304,9(1) bis 1 255,8(2) pm, b = 1 297,5(1) bis 1 260,0(2) pm, c = 1 425,1(1) bis 1 408,2(1) pm. Das Homogenitätsgebiet endet bei der Zusammensetzung Re2Se2,7Te2,3. Von einem nahe der Sättigungsgrenze gewachsenen Kristall der Zusammensetzung Re6Se8Te7 wurde eine Röntgenstrukturanalyse durchgeführt. Danach kommt den Selen- und Telluratomen eine völlig verschiedene strukturchemische Funktion zu: Während sich die Selenatome innerhalb verzerrt oktaedrischer [Re6Se8]-Cluster befinden, sind jeweils sieben Telluratome über homonukleare Bindungen zu bizyklischen [Te(Te3)2]-Baueinheiten gruppiert, welche die nach dem Motiv einer kubisch dichtesten Packung angeordneten Cluster verknüpfen.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201105
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    Metall-Koordinationsverbindungen aus Essigsäure. I Chlorometallate(III) des Eisens, Chroms und VanadiumsProfessor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1943-1946 
    Details
    ISSN: 0044-2313
    Keywords: Ternary chlorometalates(III) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal Coordination Compounds Prepared in Acetic Acid. I. Chlorometalates(III) of Iron, Chromium, and VanadiumTernary chloride-hydrates A2MCl5 · H2O (A = Cs, Rb, (K)) can be precipitated with HCl from solutions of MCl3 · 6 H2O, (M = Fe, Cr, V) and alkali metal acetates in acetic acid. Under special conditions also compounds of the composition Cs3MCl6 · H2O can be obtained. After dehydration of the solutions with acetyl chloride, anhydrous compounds are formed: Cs3Fe2Cl9; A3CrCl6 and A3Cr2Cl9 with A = Cs, Rb; Cs3VCl6 and Cs3V2Cl9. VIII is partially oxidized to VIV by an excess of acetyl chloride. Compounds A2VCl6 with A = Cs, Rb can be obtained more conveniently by the reaction of VOCl2 · H2O in acetic acid with acetyl chloride.The lattice parameters of some compounds were determined from powder patterns in analogy to known structure families.
    Notes: Aus Lösungen der Chloridhydrate MCl3 · 6 H2O (M = Fe, Cr, V) in Eisessig lassen sich nach Zugabe von Alkalimetallacetaten mit HCl ternäre Chloridhydrate A2MCl5 · H2O (A = Cs, Rb, z. T. K), unter speziellen Bedingungen auch Verbindungen der Zusammensetzung Cs3MCl6 · H2O fällen. Werden die Ausgangslösungen mit Acetylchlorid dehydratisiert, so entstehen wasserfreie Chlorometallate(III): Cs3Fe2Cl9; A3CrCl6 und A3Cr2Cl9 mit A = Cs, Rb; Cs3VCl6 und Cs3V2Cl9. Vanadium(III) kann teilweise zu VIV oxidiert werden. Chlorovanadate A2VCl6 mit A = Cs, Rb lassen sich aber günstiger aus Lösungen von VOCl2 · 2 H2O in Eisessig mit Acetylchlorid erhalten.Von einigen strukturell noch nicht untersuchten Verbindungen sind durch Analogindizierungen von Pulveraufnahmen die Gitterparameter bestimmt worden.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19946201118
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    Synthese und Struktur von Li3RhH6, einem ternären Hydrid mit isolierten [RhH6]3--OktaedernProfessor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1983-1985 
    Details
    ISSN: 0044-2313
    Keywords: Metal hydrides ; rhodium ; lithium ; crystal structure ; neutron diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Li3RhH6  -  a Ternary Hydride with Isolated [RhH6]3- OctahedraThe ternary rhodium hydride Li3RhH6 was synthesized by the reaction of lithium hydride with rhodium under a hydrogen pressure of 80 bar. X-ray investigations on powdered samples and an elastic neutron diffraction experiment on the deuterated compound led to the complete structure determination (space group: Pnma, Z = 4). The atomic arrangement is isotypic to the Na3RhH6 structure type. The crystal structure contains isolated [RhH6]3- octahedra, which are separated by the lithium ions.
    Notes: Die Synthese von Li3RhH6 gelingt durch Umsetzung von Lithiumhydrid mit feinverteiltem Rhodium unter einem Wasserstoffdruck von 80 bar. Röntgenographische Untersuchungen an pulverförmigen Proben und ein elastisches Neutronenbeugungsexperiment an der deuterierten Verbindung führten zur Strukturaufklärung (Raumgruppe: Pnma, Z = 4). Die Verbindung ist isotyp zu der von Na3RhH6 und enthält isolierte [RhH6]3--Oktaeder, die durch die Lithiumionen separiert werden.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201124
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    Nitridsulfidchloride der Lanthanide: I. Der Formeltyp M4NS3Cl3 (M = La—Nd) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1998-2002 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanides ; nitride sulfide chlorides ; M4NS3Cl3 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitride Sulfide Chlorides of the Lanthanides. I. The Composition M4NS3Cl3 (M = La—Nd)The oxidation of the „light“ lanthanides (M = La—Nd) with sulfur and NaN3 the presence of the chlorides MCl3 results in the formation of the first lanthanide nitride sulfide chlorides M4NS3Cl3 when appropriate molar ratios of the reactants are used. The addition of some NaCl (or an excess of MCl3) as a flux secures complete and fast reaction (7 d) at 850°C in evacuated silica vessels as well as single-crystalline products. Since these nitride sulfide chlorides (fine transparent needles) are not sensitive against hydrolysis, the surplus chloride can be removed easily with water.The crystal structure was determined from X-ray single crystal data for the example of La4NS3Cl3 (hexagonal, P63mc (no. 186), Z = 2, a = 941.40(3), c = 700.36(3) pm, R = 0.026, Rw = 0.021) and the nitride sulfide chlorides M4NS3Cl3 with M = Ce—Nd proved to be isostructural from Guinier powder data. According to their Ba3OCl6-analogue structure, two crystallographically different M3+ cations are present (CN(M1) = 10, CN(M2) = 8). „Isolated“ tetrahedra [(N3-)(M3+)4] build up the Mayn structural feature according to ∞0[NM4]S3Cl3. They are hexagonally closest packed and interconnected via the crystallographically different but by X-ray diffraction indistinguishable anions S2- and Cl-, which take care for charge neutrality.
    Notes: Durch Oxidation der „leichten“ Lanthanide (M = La—Nd) mit Schwefel und NaN3 in Gegenwart der Chloride MCl3 erhält man aus Gemengen mit entsprechenden molaren Verhältnissen der Ausgangsstoffe erstmals Nitridsulfidchloride der Lanthanide: M4NS3Cl3. Geringer Zusatz von NaCl (bzw. MCl3 im Überschuß) als Flußmittel gewährleistet vollständige und schnelle Umsetzung (7 d) bei 850°C in evakuierten Quarzglasampullen sowie einkristalline Produkte. Wegen der Unempfindlichkeit dieser Nitridsulfidchloride (feine, transparente Kristallnadeln) gegenüber Hydrolyse kann überschüssiges Chlorid leicht mit Wasser entfernt werden.Die Kristallstruktur wurde anhand von röntgenographischen Einkristalldaten am Beispiel von La4NS3Cl3 (hexagonal, P63mc (Nr. 186), Z = 2; a = 941,40(3); c = 700,36(3) pm; R = 0,026; Rw = 0,021) bestimmt und die Nitridsulfidchloride M4NS3Cl3 mit M = Ce—Nd sind nach Ausweis von Guinier-Pulveraufnahmen isotyp. Demnach liegt eine Ba4OCl6-analoge Struktur vor, in der zwei kristallographisch unterschiedliche M3+-Kationen auftreten (CN(M1) = 10, CN(M2) = 8). „Isolierte“ Tetraeder [(N3-)(M3+)4] bilden gemäß ∞0[NM4]S3Cl3 das strukturelle Hauptmerkmal und sind nach Art einer hexagonal-dichtesten Kugelpackung angeordnet. Der Ladungsausgleich erfolgt über die kristallographisch unterschiedlichen, röntgenographisch jedoch nicht unterscheidbaren Anionen S2- und Cl-.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201127
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    Synthesis and Structure of Ba[ZrN2] and Ba2[NbN3] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2008-2013 
    Details
    ISSN: 0044-2313
    Keywords: Barium nitrido zirconate, Ba[ZrN2] ; barium nitrido niobate, Ba2[NbN3] ; synthesis ; crystal structure ; neutron diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Struktur von Ba[ZrN2] und Ba2[NbN3]Ba3N2 reagiert im Stickstoffstrom bei 950°C mit Zr unter Bildung von luftempfindlichem, dunkelrotem Ba[ZrN2]. Es kristallisiert tetragonal in der Raumgruppe P4/nmm mit a = 416,10(2), c = 839,2(1) pm und Z = 2. Die Kristallstruktur wurde anhand von Röntgen- und Neutronenbeugungsdaten des Kristallpulvers verfeinert. Im Nitridozirconat [ZrN2]2- ist das Zr-Atom quadratisch-pyramidal von fünf N-Atomen im Abstand von 201(3) und 220,2(2) pm koordiniert. Die Koordinationspolyeder sind in der Pyramidenbasis über alle Kanten verknüpft und bilden Schichten parallel (001) mit den Pyramidenspitzen alternierend nach oben und nach unten weisend. Die Ba2+-Kationen sind auf der Höhe der Pyramidenspitzen in diese Schichten integriert. Die Struktur kann als aufgefüllter PbFCl-Typ interpretiert werden. Ba2[NbN3] entsteht aus Ba3N2 und NbN oder aus Ba und Nb im Stickstoffstrom bei ca. 1 000°C. Es kristallisiert isotyp zu Ba2[TaN3] in der monoklinen Raumgruppe C2/c mit a = 613,2(3), b = 1 176,8(3), c = 1 322,9(4) pm, β = 91,65(2)°, Z = 8. Die Nitridoniobat-Anionen bilden Ketten aus eckenverknüpften NbN4-Tetraedern mit Abständen Nb—N zwischen 188(1) und 199,9(9) pm.
    Notes: Ba3N2 reacts at 950°C under pure N2 with Zr to yield dark red, air-sensitive Ba[ZrN2]. This new compound crystallizes in the tetragonal space group P4/nmm with a = 416.10(2), c = 839.2(1) pm and Z = 2. The crystal structure was solved and refined using X-ray and neutron powder diffraction data. In the nitrido zirconate [ZrN2]2- the Zr atoms exhibit a square-pyramidal coordination by five N atoms at distances of 201(3) and 220.2(2) pm. The pyramids share all the edges in the basal plane to form layers parallel to (001) with their apices alternately pointing up and down. The Ba2+ cations are integrated into these layers at the levels of the pyramidal apices. The structure can be interpreted as a stuffed PbFCl type. Ba2[NbN3] is formed by the reaction of Ba3N2 and NbN or of Ba and Nb at 1 000°C under N2. Isostructural to Ba2[TaN3] it crystallizes in the monoclinic space group C2/c with a = 613.2(3), b = 1 176.8(3), c = 1 322.9(4) pm, β = 91.65(2)°, Z = 8. The nitrido niobate anions form chains of corner sharing NbN4 tetrahedra with distances Nb—N between 188(1) and 199.9(9) pm.
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    URL: http://dx.doi.org/10.1002/zaac.19946201129
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    From crystalline boryl-substituted and boryl-coupled 2,2,4,4,6,6-hexamethyl-cyclotrisilazanes to β-SiC and BNFurther data are available from the Cambridge Crystallographic Data Centre, Cambridge, UK. (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 8 (1994), S. 491-498 
    Details
    ISSN: 0268-2605
    Keywords: Cyclosilazane ; BF-coupled rings ; crystal structure ; pyrolysis ; β-SiC/BN composites ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [Me2SiNBFN(SiMe3)2]3 (1) is synthesized in the reaction of trilithiated hexamethylcyclotrisilazane with F2BN(SiMe3)2. The mono- and dilithium derivatives of the six-membered ring (Me2SiNH)2 Me2SiNSiFMe2 react with the F2B-substituted cyclotrisilazane F2B(NSiMe2)3(SiFMe2)2 in the molar ratio 1:1 or 1:2 to give the BF-coupled rings 2 and 3. The crystal structure analysis of 1 and 3 and pyrolysis of 1 and 3 with formation of silicon boron carbonitride and its crystallisation to composite powders at very high temperatures are reported.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/aoc.590080509
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    Synthesis and Crystal Structure of Hg5Sb2I6 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 389-392 
    Details
    ISSN: 0044-2313
    Keywords: Mercury antinionide iodide, Hg5Sb2I6 ; Preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Kristallstruktur von Hg5Sb2I6Das Antimonid-Iodid von Quecksilber, Hg5Sb2I6, früher irrtümlich als Hg3Sb2I4 formuliert, wurde in Standardampullen synthetisiert. Einkristalle wurden mittels Transport über die Gasphase erhalten. Hg5Sb2I6: Raumgruppe Pc21n, Gitterparameter: a = 8,108(1), b = 10,702(1), c = 21,295(1) Å. Die Struktur (Einkristall) ist aus [HgSbI3]-Tetraedern und [HgSbI2]-Dreiecken aufgebaut. Alle Antimonatome sind paarweise zu Sb24--Hanteln verbunden. Die Struktur wird mit anderen Strukturen, die Sb24--Hanteln enthalten, verglichen.
    Notes: Mercury antimonide iodide, Hg5Sb2I6, previously and erroneously reported as Hg3Sb2I4 was synthesized using standard ampoule technique. A gas-phase transport reaction was applied for preparation of single crystals. Hg5Sb2I6 crystallizes in the space group Pc21n (No. 33) with unit cell dimensions: a = 8.108(1), b = 10.702(1), c = 21.295(1) Å. Crystal structure solved using single crystal X-ray data is built of [HgSbI3] tetrahedra and [HgSbI2] triangles. All antimony atoms are joined into Sb24- dumbbells. The structure is compared with ones containing similar Sb24- dumbbells.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200232
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    Synthesis, structures and luminescence of two new Europium(II) Silicate-Chlorides, Eu2SiO3Cl2 and Eu5SiO4Cl6 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 451-456 
    Details
    ISSN: 0044-2313
    Keywords: Silicates ; crystal structure ; europium ; luminescence ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Strukturen und Lumineszenz von zwei neuen Europium(II)-silicat-chloriden, Eu2SiO3Cl2 und Eu5SiO4Cl6Eu2SiO3Cl2 und Eu5SiO4Cl6 wurden durch Erhitzen von EuCl2 mit EuSiO3 bzw. Eu2SiO4 gewonnen, Sr2SiO3Cl2:Eu2+ aus einem Gemenge von SrCO3, Eu2O3, SrCl2 · 6H2O und SiO2 unter reduzierenden Bedingungen. Die Kristallstrukturen von Eu2SiO3Cl2 [a = 1118,7(5), c = 952,6(1) pm, tetragonal, I4/m, Z = 8, R = 3,3, Rw = 3,0%] und Eu5SiO4Cl6 [a = 900,4(1), b = 1401,7(2), c = 1112,3(2) pm, β = 103,51(1)°, monoklin, C2/c, Z = 4, R = 3,6, Rw = 2,6%] wurden aus Einkristall-Vierkreisdiffraktometer-Daten bestimmt und mit verwandten Verbindungen verglichen. Die Lumineszenzeigenschaften wurden bei 300 K und bei 4,2 K untersucht; sämtliche Verbindungen zeigen eine intensive blaugrüne Photolumineszenz. Sr2SiO3Cl2:Eu2+ zeigt Thermolumineszenz.
    Notes: Eu2SiO3Cl2 and Eu5SiO4Cl6 were prepared by reaction of EuCl2 with EuSiO3 and Eu2SiO4, respectively, Sr2SiO3Cl2: Eu2+ from mixtures of SrCO3, Eu2O3, SrCl2 · 6H2O and SiO2 under reducing conditions. The crystal structures of Eu2SiO3Cl2 [a = 1118.7(5), c = 952.6(1) pm, tetragonal, I4/m, Z = 8, R = 3.3, Rw = 3.0%] and Eu5SiO4Cl6 [a = 900.4(1), b = 1401.7(2), c = 1112.3(2) pm, β = 103.51(1)°, monoclinic, C2/c, Z = 4, R = 3.6, Rw = 2.6%] were determined from four-circle diffractometer data and compared with related compounds. The luminescence properties were investigated at 300 K and at 4.2 K; all compounds show intense bluish-green photoluminescence. Sr2SiO3Cl2:Eu2+ shows thermoluminescence.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200308
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  • 126
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    Die Chloride Na3xM2-xCl6 (M = La—Sm) und NaM2Cl6 (M = Nd, Sm): Derivate des UCl3-Typs. Synthese, Kristallstruktur und Röntgenabsorptionsspektroskopie (XANES) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 444-450 
    Details
    ISSN: 0044-2313
    Keywords: Chlorides ; lanthanides ; synthesis ; crystal structure ; X-ray absorption spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Chlorides Na3xM2-xCl6 (M = La—Sm) and NaM2Cl6 (M = Nd, Sm): Derivatives of the UCl3-Type of Structure. Synthesis, Crystal Structure and X-Ray Absorption Spectroscopy (XANES)Single crystals of the derivatives of the UCl3-type structure Na3xM2-xCl6 (M = La/x = 0.364(4); Ce/0.349(5); Pr/0.318(8); Nd/0.305(5); Sm/0.246(4)) and NaSm2Cl6 were grown by different methods generally under reducing conditions. They are addition [Na(Sm2)Cl6] and addition/substitution variants [Na2x(NaxM2-x)Cl6] of the UCl3 structure type [□(U2)Cl6]. X-Ray Absorption Spectroscopy (XANES) at the LIII edge characterizes NaSm2Cl6 and NaNd2Cl6 as mixed-valence compounds with valences of +2 and +3 in statistical distribution (approximately 1:1) for Sm and Nd, respectively.
    Notes: Einkristalle der Derivate des UCl3-Typs Na3xM2-xCl6 (M = La/x = 0,364(4); Ce/0,349(5); Pr/0,318(8); Nd/0,305(5); Sm/0,246(4)) sowie von NaSm2Cl6 wurden auf unterschiedlichen Wegen, im allgemeinen unter reduzierenden Bedingungen erhalten. Sie sind Additions- [Na(Sm2)Cl6] bzw. Additions- / Substitutionsvarianten [Na2x(NaxM2-x)Cl6] des UCl3-Strukturtyps [□(U2)Cl6]. Röntgenabsorptionsspektren (XANES) an der Lm-Kante charakterisieren NaSm2Cl6 und NaNd2Cl6 als gemischtvalente Verbindungen mit Valenzen von +2 und +3 in statistischer Verteilung (etwa 1:1) für Sm bzw. Nd.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200307
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  • 127
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    Synthese und Struktur eines Caesium-tetraimidophosphat-diamids, Cs5[P(NH)4](NH2)2 = Cs3[P(NH)4] · 2 CsNH2Professor Heinz Dieter Lutz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 531-534 
    Details
    ISSN: 0044-2313
    Keywords: Cesium tetraimidophosphate-diamide ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of a Cesium-tetraimidophosphate-diamide, Cs5[P(NH)4](NH2)2 = Cs3[P(NH)4] · 2 CsNH2Well crystallized Cesium-tetraimidophosphate-diamide is obtained by the reaction of CsNH2 with P3N5 in autoclaves at 673 K within three days. X-ray single crystal investigations led to the following dataCcca, Z = 4, a = 8.192(5) Å, b = 20.472(5) Å,c = 8.252(3) ÅZ(F2o) ≥3σ(F2o) = 916, Z(Var.) = 32, R/Rw=1 = 0.017/0.021The compound contains the hitherto unknown anion [P(NH)4]3-.
    Notes: Gut kristallisiertes Caesium-tetraimidophosphat-diamid entsteht bei der Umsetzung von CsNH2 mit P3N5 in Autoklaven bei 673 K innerhalb von drei Tagen. Röntgenographische Untersuchungen an Einkristallen der Verbindung ergaben:Ccca, Z = 4, a = 8,192(5) Å, b = 20,472(5) Å,c = 8,252(3) ÅZ(F2o) ≥ 3σ(F2o) = 916, Z(Var.) = 32, R/Rw=1 = 0,017/0,021Die Verbindung enthält das bis dahin unbekannte Anion [P(NH)4]3-.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200324
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  • 128
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    Preparation and crystal structure of potassium manganese cyclodecaphosphate octadecahydrate: K2Mn4P10O30 · 18 H2O (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 545-550 
    Details
    ISSN: 0044-2313
    Keywords: Dipotassium tetramanganese cyclodecaphosphate octadecahydrate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur von Kaliummangancyclodecaphosphat-octadecahydrat: K2Mn4P10O30 · 18 H2ODie Titelverbindung, ein neues Cyclodecaphosphat, wurde durch Fällung aus wäßriger K10P10O30-Lösung hergestellt. Das in Wasser wenig lösliche Salz kristalliert monoklin in der Raumgruppe P21/a mit den Gitterkonstanten a = 14,546(10), b = 15,211(10), c = 9,860(6) Å, β = 105,12(4)°.Die Kristallstruktur wurde unter Verwendung von 6501 unabhängigen Reflexen gelöst, der R-Wert beträgt 0,044.Die zentrosymmetrischen Ringanionen sind relativ weit voneinander entfernt und in einer pseudotetragonalen Weise angeordnet, so daß parallel zur c-Achse große, die Wassermoleküle enthaltende Kanäle gebildet werden.
    Notes: The title compound, a new cyclodecaphosphate, was prepared by precipitation from an aqueous solution of K10P10O30. The sparingly soluble salt crystallizes monoclinic in the space group P21/a, with Z = 2, and the unit-cell dimensions a = 14.546(10), b = 15.211(10), c = 9.860(6) Å, β = 105.12(4)°.The crystal structure was solved using 6501 unique reflections with a final R-value of 0.044.The centrosymmetrical ring anions rather distant from each other and arranged in a pseudo-tetragonal way create, parallel to the c direction, large channels containing the water molecules.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200327
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  • 129
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    (O,O′)-Diorganodithiophosphatophenyltellur(II)- und Tris[(O,O′)-diorganodithiophosphato]phenyltellur(IV)-Verbindungen; Kristallstruktur von Tris[(O,O′)-diphenyldithiophosphato]phenyltellur(IV) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1397-1402 
    Details
    ISSN: 0044-2313
    Keywords: Tris[(O,O′)-diorganodithiophosphato]phenyltellurium(IV) compounds (O,O′)-Diorganodithiophosphatophenyltellurium(II) compounds ; reductive elimination ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (O,O′)-Diorganodithiophosphatophenyltellurium(II)- and Tris[(O,O′)-diorganodithiophosphato]phenyltellurium(IV) Compounds; Crystal Structure of Tris[(O,O′)-diphenyldithiophosphato]phenyltellur(IV)The title compounds are available by reaction of trichlorophenyltellurium(IV) respectively iodophenyltellurium(II) with the sodium or ammonium salts of (O,O′)-diorganodithiophosphorus acids in various solvents. The resulting tellurium(IV) compounds have a pronounced tendency towards reductive elimination of bis[(O,O′)-diorganothiophosphoryl]disulfanes [S2P(OR)2]2 in solution. In contrast, the tellurium(II) compounds are stable, although they are disintegrated to diphenylditellane and [S2P(OR)2]2 on prolonged standing in chlorinated hydrocarbons.Crystals of tris[(O,O′)-diphenyldithiophosphato]phenyltellurium(IV) are monoclinic (space group P21/c) with the cell constants: a = 1 039.2(1), b = 1 037.9(3), c = 4 205.0(1) pm, β = 95.273(1)°, V = 4 516.42(9)X106 pm3, Z = 4. The compound appears to be monomeric in the solid state forming a distorted pentagonal bipyramid. The stereochemical influence of the lone pair of electrons causes the axial (i. e. C1—Te—S4) angle to be 156.6(1)° rather than the theoretical 180°.
    Notes: Die Titelverbindungen sind durch Reaktion von Trichlorophenyltellur(IV) bzw. Iodophenyltellur(II) mit Natrium- oder Ammoniumsalzen von (O,O′)-Diorganodithiophosphorsäuren in verschiedenen Lösungsmitteln zugänglich. Die dabei erhaltenen Tellur(IV)-Verbindungen zeigen in Lösung eine ausgeprägte Tendenz zur reduktiven Eliminierung der Bis[(O,O′)-diorganothiophosphoryl]disulfane [S2P(OR)2]2. Die Tellur(II)-Verbindungen sind dagegen stabil, zersetzen sich aber bei längerem Stehenlassen in chlorierten Kohlenwasserstoffen in Diphenylditellan und [S2P(OR)2]2.Die Kristalle von Tris[(O,O′)-diphenyldithiophosphato]phenyltellur(IV) sind monoklin (Raumgruppe P21/c) mit den Zellkonstanten a = 1 039,2(1), b = 1 037,9(3), c = 4 205,0(1) pm, β = 95,273(1)°, V = 4 516,42(9)X106 pm3, Z = 4. Die Verbindung liegt im Kristall monomer in Form einer verzerrt pentagonalen Bipyramide vor. Das stereochemisch aktive freie Elektronenpaar bedingt einen von den theoretischen 180° abweichenden axialen (d. h. C1—Te—S4) Winkel von 156,6(1)°.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200812
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  • 130
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    Synthese und Kristallstruktur von LiAl[(P2O6)2] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1409-1412 
    Details
    ISSN: 0044-2313
    Keywords: Polyphosphate ; lithium aluminium polyphosphate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure Determination of LiAl[(P2O6)2]Single crystals of previously unknown LiAl[(P2O6)2] have been obtained by reaction of Li2CO3, Al2O3 and H3PO4 (1:1:16) at 350°C. The title compound crystallizes in Pbcn (a = 1 244.54(1), b = 823.40(1), c = 892.46(1) pm; Z = 4). The least-squares refinement (with anisotropic temperature factors) was performed using 766 observed reflections yielding R = 0.029 and R(w) = 0.075. Four anion chains are running parallel to the shortest axis in the unit cell, the period of identity amounting to four. Aluminium is surrounded by an almost regular octahedron, lithium by a distorted tetrahedron of oxygen.
    Notes: Durch Umsetzung von Li2CO3, Al2O3 und H3PO4 im molaren Verhältnis 1:1:16 bei 350°C bildet sich vorher unbekanntes LiAl[(P2O6)2] einkristallin. LiAl[(P2O6)2] kristallisiert orthorhombisch in Pbcn mit a = 1 244,54(1), b = 823,40(1), c = 892,46(1) pm; Z = 4. Die Verfeinerung (mit anisotropen Temperaturfaktoren) erfolgte mit 766 beobachteten Reflexen bis zu R = 0,029 und R(w) = 0,075. Vier Phosphatketten verlaufen in der Elementarzelle mit einer Periodizität von vier parallel zu b. Aluminium ist oktaedrisch, Lithium verzerrt tetraedrisch von Sauerstoff umgeben.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200814
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  • 131
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    Synthese und Strukturbestimmung von (i-Pr)2NB(t-BuP)3 und (i-Pr)2NB(t-BuP)4Professor Ernst-Otto Fischer zum 75. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 8-15 
    Details
    ISSN: 0044-2313
    Keywords: P3B and P4B ring systems ; NMR data ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Analysis of (i-Pr)2NB(t-BuP)3 and (i-Pr)2NB(t-BuP)4The diphosphide K(t-Bu)P-(t-BuP)2-P(t-Bu)K obtained by the cleavage reaction of the 3-membered ring system (i-Pr)2BN(t-BuP)2 with potassium reacts with t-BuPCl2 at -78°C under ring expansion to form the P3B ring system (i-Pr)2NB(t-BuP)3 - 1,2,3-tri-t-butyl-tri-phospha-4-diisopropyl-aminoboretane (1). - The 5-membered P4B ring system (i-Pr)2NB(t-BuP)4 - 1,2,3,4-tetra-t-butyl-tetraphospha-5-diisopropylaminoborolidine, (2) - is formed from K(t-Bu)P—(t-BuP)2—P(t-Bu)K and (i-Pr)2NBCl2 analogous to the above reaction. 1 and 2 could be obtained in a pure form and characterized NMR spectroscopically and by X-ray structure analysis. 1 shows at 200 K two conformation isomers; for 2 31P-10,11B-isotopic shifts could be identified.
    Notes: Das bei der Spaltung des Dreiringes (i-Pr)2BN(t-BuP)2 mit Kalium gebildete Diphosphid K(t-Bu)P—BN(i-Pr)2—P(t-Bu)K reagiert bei -78°C mit t-BuPCl2 unter Ringerweiterung zu (i-Pr)2NB(t-BuP)3-1,2,3-Tri-t-butyl-triphospha-diisopropyl-aminoboretan, (1) - mit einem P3B-Ringgerüst. In analoger Weise entsteht bei der Reaktion zwischen K(t-Bu)P—(t-BuP) - (t-BuP)2—P(t-Bu)K und (i-Pr)2NBCl2 das P4B-Ringsystem (i-Pr)2NB(t-BuP)4 - 1,2,3,4-Tetra-t-butyl-tetraphospha-5-diiso-propylaminoborolidin, (2) -, 1 und 2 konnten in reiner Form isoliert, NMR-spektroskopisch und durch Röntgenstrukturanalysen charakterisiert werden. 1 zeigt bei 200 K zwei Konformationsisomere; bei 2 konnten 31P-10,11B-Isotopieverschiebungen nachgewiesen werden.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200104
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  • 132
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    Struktur einer kristallinen Hochtemperaturmodifikation des Calciumultraphosphats, CaP4O11, und die kristallographische Orientierungsbeziehung zur Raumtemperaturphase (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 766-770 
    Details
    ISSN: 0044-2313
    Keywords: CaP4O11 ; crystal structure ; orientation relation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure of a High Temperature Modification of Calciumultraphosphate, CaP4O11, and its Crystallographic Orientation Relation with Respect to the Room Temperature PhaseThe title compound was obtained by heating a mixture of CaCO3, P4O10 in excess and H3PO4 in excess as well to 500°C and annealing for 10 days. The Calciumultraphosphate, CaP4O11, transforms at 85°C in a hot nitrogen gas stream into a second modification with orthorhombic space group (Aba2), the structure of which was determined: a = 12.683 Å, b = 12.090 Å, c = 12.627 Å, Z = 8, layer structure, R = 0.034. The crystallographic orientation relation between the two phases of CaP4O11 was determined.
    Notes: Die Titelverbindung wurde durch Erhitzen von CaCO3 mit einem Überschuß an P4O10 und H3PO4 auf 500°C und anschließendes Tempern (10 Tage) erhalten. Das gebildete CaP4O11 wandelt sich im heißen N2-Strom bei 85°C in eine zweite CaP4O11-Modifikation um, deren Struktur bestimmt wurde: a = 12,683 Å, b = 12,090 Å, c = 12,627 Å, orthorhombische Raumgruppe Aba2, Z = 8, Schichtstruktur, R = 0,034. Die kristallographische Orientierungsbeziehung zwischen den beiden Phasen des CaP4O11 wurde ermittelt.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200431
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    Zur Kenntnis des Natrium-tetrahydroxoaluminat-chlorids Na2[Al(OH)4]Cl (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 771-776 
    Details
    ISSN: 0044-2313
    Keywords: Tetrahydroxoaluminate chloride, Na2[Al(OH)4]Cl ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Sodium Tetrahydroxoaluminate Chloride Na2[Al(OH)4]ClThe hitherto unknown compound Na2[Al(OH)4]Cl was prepared by crystallisation from a NaCl containing sodium aluminate solution. According to the X-ray single crystal investigation (tetragonal, space group P4/nmm, a = 7.541 Å, c = 5.059 Å, Z = 2) the compound represents the first example of a crystalline hydroxoaluminate with monomeric [Al(OH)4]- anions. Cl- shows a quadratic anti prismatic coordination to 4 Na+ and over hydrogen bonds to 4 O2- while Na+ is octahedrally coordinated by 4 O2- and 2 Cl- (axial). The results of the crystal structure analysis are confirmed by 27Al and 23Na MAS NMR investigations. Na2[Al(OH)4]Cl decomposes at about 200°C without intermediates under formation of β-NaAlO2 and NaCl.
    Notes: Die bisher unbekannte Verbindung Na2[Al(OH)4]Cl wurde durch Kristallisation aus mit NaCl versetzter Natriumaluminatlösung erhalten. Entsprechend der Röntgenstrukturanalyse an einem Einkristall (tetragonal, Raumgruppe P4/nmm, a = 7,541 Å, c = 5,059 Å, Z = 2) liegt mit dieser Verbindung erstmals ein Beispiel für ein kristallines Hydroxoaluminat mit monomeren [Al(OH)4]--Anionen vor. Cl- ist quadratisch antiprismatisch mit 4 Na+ sowie über Wasserstoffbrückenbindungen mit 4 O2- koordiniert, während Na+ oktaedrisch von 4 O2- und 2 Cl- (axial) umgeben ist. Die Ergebnisse der Kristallstrukturanalyse werden durch 27Al- und 23Na-MAS-NMR-Messungen bestätigt. Na2[Al(OH)4]Cl zersetzt sich ohne Zwischenprodukte bei 200°C zu β-NaAlO2 und NaCl.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200432
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    Synthese und Kristallstruktur von Cu4[PhN3C6H4N3(H)Ph]4(μ2-O)2, einem vierkernigen Kupfer(II)-Komplex mit 1-Phenyltriazenido-2-phenyltriazenobenzol als Ligand (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 107-111 
    Details
    ISSN: 0044-2313
    Keywords: Tetrameric copper(II) complex ; μ2-oxo ligand ; 1-phenyltriazenido-2-phenyltriazeno benzene ligand ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Cu4[PhN3C6H4N3(H)Ph]4(μ2-O)2, a Tetranuclear Copper(II) Complex with 1-Phenyltriazenido-2-phenyltriazeno-benzene as LigandCu4[PhN3C6H4N3(H)Ph]4(μ-O)2 (1) results from the reaction of an aqueous solution of [Cu(NH3)4]2+ with 1,2-bis(phenyltriazeno)benzene in ether. 1 crystallizes in the orthorhombic space group Pba2 with the lattice parameters a = 1661.5(5), b = 1914.7(7), c = 1269.2(5) pm; Z = 2. In the tetrameric complex with the symmetry C2 the Cu2+ cations form a tetrahedron (Cu—Cu: 298.3(1)-337.1(1) pm). The μ2-oxo ligands occupy the twofold axis and bridge two opposite edges of the Cu4 tetrahedron (Cu—O: 190.0(3) and 192.5(4) pm). The 1-phenyltriazenido-2-phenyltriazeno benzene anions bridge two Cu2+ ions chelating one metal ion and coordinating monodentate the neighbouring one (Cu—N: 191.0(5)-204.1(4) pm).
    Notes: Cu4[PhN3C6H4N3(H)Ph]4(μ-O)2 (1) entsteht bei der Umsetzung einer wäßrigen Lösung von [Cu(NH3)4]2+ mit 1,2-Bis(phenyltriazeno)benzol in Ether. 1 kristallisiert orthorhombisch in der Raumgruppe Pba2 mit den Gitterkonstanten a = 1661,5(5); b = 1914,7(7); c = 1269,2(5) pm; Z = 2. Im tetrameren Komplex mit der Symmetrie C2 bilden die Cu2+-Ionen ein Tetraeder (Cu—Cu: 298,3(1)-337,1(1) pm). Die μ2-Oxoliganden liegen auf der C2-Achse und überbrücken zwei gegenüberliegende Tetraederkanten (Cu—O: 190,0(3) und 192,5(4) pm). Die 1-Phenyltriazenido-2-phenyltriazeno-benzol-Anionen verbrücken benachbarte Cu2+-Ionen, die sie einerseits chelatisierend und andererseits einzähnig koordinieren (Cu—N: 191,0(5)-204,1(4) pm).
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200117
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    Hydrate schwacher und starker Basen. IX. Zur Wasserstoffbrückenbindung in CsNa2(OD)3 · 6D2O: Neutronenbeugung an einem Einkristall bei 120 KProfessor Heinz Dieter Lutz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 809-813 
    Details
    ISSN: 0044-2313
    Keywords: Cesium disodium trihydroxide hexahydrate ; deuterated material ; neutron diffraction ; hydrogen bonding ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrates of Weak and Strong Bases. IX. Hydrogen Bonding in CsNa2(OD)3 · 6D2O: A Single-Crystal Neutron-Diffraction Study at 120 KThe title compound is the first hydrate of a ternary alkali hydroxide reported. Its structure is related to the hexagonal perovskites and at the same time shaped by a complex system of hydrogen bonds. In a previous X-ray structure analysis at room temperature of the isotypic undeuterated material, these had been characterized only insufficiently. Therefore a complete structure determination has now been performed on a perdeuterated single crystal using low-temperature neutron-diffraction data (Pca21, Z = 4; a = 13.86, b = 6.070, c = 12.41 Å at 120 K; 1 655 observed independent reflections, R = 0.027).
    Notes: Die Titelverbindung ist das erste beschriebene Hydrat eines ternären Alkalihydroxids. Ihre Struktur ist verwandt mit der der hexagonalen Perowskite und zugleich durch ein komplexes System von Wasserstoffbrücken geprägt. Dieses war in einer vorangegangenen Röntgenstrukturanalyse bei Raumtemperatur an der isotypen nicht deuterierten Substanz nur unzureichend charakterisiert worden. Daher wurde nun eine vollständige Strukturbestimmung an einem perdeuterierten Einkristall mit Tieftemperatur-Neutronenbeugungsdaten durchgeführt (Pca21, Z = 4; a = 13,86, b = 6,070, c = 12,41 Å bei 120 K; 1 655 beobachtete unabhängige Reflexe, R = 0,027).
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200509
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  • 136
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    New Fluoromanganate(III) Hydrates: Mn3F8 · 12H2O and AgMnF4 · 4H2O (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 833-838 
    Details
    ISSN: 0044-2313
    Keywords: Fluoromanganate(III) hydrates, Mn3F8 · 12H2O, AgMnF4 · 4 H2O ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Neue Fluoromanganat(III)-Hydrate: Mn3F8 · 12H2O and AgMnF4 · 4H2ODie Fluoridhydrate Mn3F8 · 12H2O und AgMnF4 · 4 H2O wurden in Form von Einkristallen hergestellt und durch Röntgenbeugungsmethoden charakterisiert. Mn3F8 · 12H2O kristallisiert in Raumgruppe P1 (a = 623.0(3), b = 896.7(4), c = 931.8(4) pm, α = 110.07(2)°, β = 103.18(2)°, γ = 107.54(2)°, Z = 1); AgMnF4 · 4 H2O kristallisiert in Raumgruppe P21/m (a = 700.9(2), b = 726.1(1), c = 749.4(3) pm, β = 107.17(3)°, Z = 2). Beide Strukturen enthalten Jahn-Teller-verzerrte [Mn(H2O)2F4]-Anionen und zeigen ein komplexes Wasserstoffbrücken-Netzwerk zwischen Anionen und Kationen, nämlich [Mn(H2O)6]2+ in der ersteren und einem polymeren [Ag(H2O)2]--Kation in der zweiten Verbindung.
    Notes: Single crystals of fluoride hydrates Mn3F8 · 12 H2O and AgMnF4 · 4 H2O have been prepared and characterized by X-ray methods. Mn3F8 · 12 H2O crystallizes in the space group P1 (a = 623.0(3), b = 896.7(4), c = 931.8(4) pm, α = 110.07(2)°, β = 103.18(2)°, γ = 107.54(2)°, Z = 1); AgMnF4 · 4 H2O crystallizes in the space group P21/m (a = 700.9(2), b = 726.1(1), c = 749.4(3) pm, β = 107.17(3)°, Z = 2). Both structures contain Jahn-Teller-distorted [Mn(H2O)2F4]- anions as well as crystal water molecules and exhibit a complex hydrogen bond network between anions and cations, i. e. [Mn(H2O)6]2+ for the first and a polymeric [Ag(H2O)2]- cation for the second compound.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200514
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  • 137
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    Synthese und Struktur von [(Ph3C6H2)Te]2, [(Ph3C6H2)Te(AuPPh3)2]PF6 und [(Ph3C6H2)TeAuI2]2Professor Ekkehard Lindner zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1678-1685 
    Details
    ISSN: 0044-2313
    Keywords: Ditelluride ; [(2,4,6-Ph3C6H2)Te]2 ; Bis(triphenylphosphanegold(I))tellurolate ; [(2,4,6-Ph3C6H2)Te(AuPPh3)2]PF6 ; Diiodinegold(III) tellurolate ; [(2,4,6-Ph3C6H2)TeAuI2]2 ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of [(Ph3C6H2)Te]2, [(Ph3C6H2)Te(AuPPh3)2]PF6 and [(Ph3C6H2)TeAuI2]2[(2,4,6-Ph3C6H2)Te]2 reacts with Ph3PAu+ to yield [2,4,6-Ph3C6H2TeAuPPh32]PF6 which can be oxidized by I2 to form the gold(III) complex [(2,4,6-Ph3C6H2)TeAuI2]2. [(2,4,6-Ph3C6H2)Te]2 crystallizes in the monoclinic space group P21/c with a = 810.6(2); b = 2026.5(5); c = 2260.6(7) pm; β = 99.23(3)° and Z = 4. In the crystal structure the ditelluride exhibits a dihedral angle C11—Te1—Te2—C21 of 66.1(2)°. The distance Te1—Te2 is 269.45(6) pm. In the cation of the triclinic complex [(2,4,6-Ph3C6H2)Te(AuPPh3)2]PF6 (space group P1; a = 1197.4(3); b = 1457.2(4); c = 1680.0(6) pm; α = 84.69(3)°; β = 85.11(3)°; γ = 75.54(3)°; Z = 2) a pyramidal skeleton RTeAu2 with distances Te—Au = 259.2(1) and 257.8(2) pm and Au—Au = 295.3(1) pm is present. [(2,4,6-Ph3C6H2)TeAuI2]2 crystallizes in the triclinic space group P1 with a = 1086.3(3); b = 1462.9(6); c = 1654.2(2) pm; α = 85.25(2)°; β = 87.44(1)°; γ = 80.90(3)°; Z = 2. In the centrosymmetrical dinuclear complex [(2,4,6-Ph3C6H2)TeAuI2]2 the Au atoms exhibit a square-planar coordination by two iodine atoms and two tellurolate ligands. The tellurolate ligands form symmetrical bridges with distances Te—Au = 260.0 pm. The distances Au—I are in the range of 260.3(1) and 263.7(1) pm.
    Notes: [(2,4,6-Ph3C6H2)Te]2 reagiert mit Ph3PAu+ unter Bildung von [2,4,6-Ph3C6H2)Te(AuPPh3)2]+, das von I2 zu der Gold(III)-Verbindung [(2,4,6-Ph3C6H2)TeAuI2]2 oxidiert werden kann. [(2,4,6-Ph3C6H2)Te]2 kristallisiert monoklin in der Raumgruppe P21/c mit a = 810,6(2); b = 2026,5(5); c = 2260,6(7) pm; β = 99,23(3)° und Z = 4. In der Kristallstruktur bildet das Ditellurid einen Diederwinkel C11—Te1—Te2—C21 von 66,1(2)°. Der Abstand Te1—Te2 beträgt 269,45(6) pm. Im Kation der triklinen Verbindung [(2,4,6-Ph3C6H2)Te(AuPPh3)2]PF6 (Raumgruppe P1; a = 1197,4(3); b = 1457,2(4); c = 1680,0(6) pm; α = 84,69(3)°; β = 85,11(3)°; γ = 75,54(3)°; Z = (2) liegt ein pyramidales RTeAu2-Gerüst mit Abständen Te—Au = 259,2(1) und 257,8(2) pm und Au—Au = 295,3(1) pm vor. [(2,4,6-Ph3C6H2)TeAuI2]2 kristallisiert in der triklinen Raumgruppe P1 mit a = 1086,3(3); b = 1462,9(6); c = 1654,2(2) pm; α = 85,25(2)°; β = 87,44(1)°; γ = 80,90(3)°; Z = 2. Im zentrosymmetrischen Zweikernkomplex [(2,4,6-Ph3C6H2)TeAuI2]2 sind die Au-Atome quadratisch planar von zwei Iod-und zwei Tellurolatoliganden koordiniert. Die Tellurolatoliganden bilden symmetrische Brücken mit Au—Te-Abständen von 260,0 pm. Die Au—I-Abstände liegen zwischen 260,3(1) und 263,7(1) pm.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201003
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  • 138
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    TlCu(OH)CO3  -  Ein neues basisches Thallium-Kupfer-Carbonat (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1707-1713 
    Details
    ISSN: 0044-2313
    Keywords: Thallium-μ-carbonato-μ-hydroxo-copper(II) ; synthesis ; crystal structure ; thermal decomposition ; IR-spectroscopy ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: TlCu(OH)CO3  -  a New Basic Thallium Copper CarbonateTlCu(OH)CO3 was prepared from carbonate solutions. Its crystal structure was determined (hexagonal, P63/m (Nr. 176), a = 1084.9(1), b = 611.8(1) pm, VEZ = 623.6(1) X 106 pm3, Z = 6, R = 0.036, Rw = 0.020). Structural features are Cu—O chains bridged by carbonate groups and tunnels parallel [0 0 1]. The thermal behaviour of the new carbonat was examined with TG/DTA- and Simon-Guinier-techniques. The decomposition occurs in two steps to the products Tl2O and CuO. Magnetic measurements show Curie-paramagnetism with θCurie = 2.7 K. A ferromagnetic arrangement of the Cu2+-moments was detected below 4.8 K. An IR-spectrometric characterisation in comparision with other copper-carbonato complexes will be discussed.
    Notes: TlCu(OH)CO3 wurde aus wäßrigen Carbonatlösungen dargestellt. Es kristallisiert hexagonal, in der RG P63/m (Nr. 176), mit a = 1084,(1), b = 611,8(1) pm, VEZ = 623,6(1) · 106 pm3, Z = 6, R = 0,036, Rw = 0,020. Struktur-bestimmende Merkmale sind über Carbonatgruppen verbrückte Cu—O-Ketten und parallel [0 0 1] verlaufende kanalartige Hohlräume. Das thermische Verhalten wurde mittels TG/DTA-Untersuchungen und Simon-Guinier-Aufnahmen untersucht. Die Zersetzung erfolgt in zwei Schritten zu Tl2O und CuO als Endprodukte. Magnetische Messungen ergeben einen reinen Curie-Paramagnetismus mit θCurie = 2,7 K. Unterhalb 4,8 K wird eine ferromagnetische Ordnung der Cu2+ -Momente festgestellt. Das IR-Spektrum wird im Vergleich mit Spektren anderer Kupfer(II)-carbonato-Komplexe diskutiert.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946201008
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  • 139
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    Ba[CoN]: Ein niedervalentes Nitridocobaltat mit gewinkelten Ketten ∞1[CoN2/22-] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1781-1785 
    Details
    ISSN: 0044-2313
    Keywords: Nitridocobaltate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ba[CoN]: A Low-Valency Nitridocobaltate with Angled Chains ∞1[CoN2/22-]Ba[CoN] is prepared by reaction of barium and cobalt (molar ratio Ba : Co = 1 : 2.5) in tantalum crucibles at 870°C with flowing nitrogen (1 atm) within a period of 96 h. After cooling down to room temperature (24°C/h) black single crystals of the ternary phase with a platy habit are obtained (orthorhombic, Pnma; a = 959.9(2) pm, b = 2 351.0(3) pm, c = 547.6(2) pm; Z = 20). The crystal structure of Ba[CoN] contains angled (planar) chains ∞1[CoN2/22-] which run along the [010]-direction (N—Co—N[°]: 178.5(5), 179.6(6), 180.0; Co—N—Co[°]: 82.9(6), 84.2(5), 177.1(8); Co—N[pm]: 174.6(12), 177.2(12), 181.9(13), 184.3(13), 187.1(12)). Nitrogen is in an octahedral coordination (N Ba4Co2) and is arranged in a distorted cubic close packing. Barium occupies one half of the tetrahedral holes (Ba—N[pm]: 274.8(16) - 308.2(12)). The cis-positions of the Co-atoms at the nitrogen coordination-octahedra cause short Co—Co contacts within the chains ∞1[CoN2/22-]. Through this, Co2-units (Co—Co[pm]: 247.8(4); bridged by nitrogen) and linear Co3-groups (Co—Co [pm]: 245.5(2); Co—Co—Co[°]: 180.0; bridged by nitrogen) alternate along the chains.The crystal structure of Ba[CoN] is closely related to the Ba[NiN] type structure.
    Notes: Ba[CoN] wird durch Umsetzung von Barium und Cobalt im molaren Verhältnis Ba: Co = 1 : 2,5 bei 870°C im Tantaltiegel mit strömendem Stickstoff (1 atm) dargestellt. Die Reaktionszeit beträgt 96 h. Nach Abkühlen auf Raumtemperatur (24°C/h) liegt die ternäre Phase in Form schwarzer Einkristalle mit plattigem Habitus vor (orthorhombisch, Pnma; a = 959,9(2) pm, b = 2 351,0(3) pm, c = 547,6(2) pm; Z = 20). Die Kristallstruktur von Ba[CoN] enthält gewinkelte (ebene) Ketten ∞1[CoN2/22-], die entlang [010] verlaufen (N—Co—N[°]: 178,5(5), 179,6(6), 180,0; Co—N—Co[°]: 82,9(6), 84,2(5), 177,1(8); Co—N[pm]: 174,6(12), 177,2(12) 181,9(13), 184,3(13), 187,1(12)). Stickstoff ist oktaedrisch koordiniert (N Ba4Co2) und bildet das Motiv einer verzerrt kubisch dichtesten Packung. Barium besetzt eine Hälfte der Tetraederlücken (Ba—N[pm]: 274,8(16) - 308,2(12)). Die cis-Positionierung der Co-Atome an den Stickstoff-Koordinationsoktaedern bedingt kurze Co—Co-Abstände innerhalb der Ketten ∞1[CoN2/22-], so daß von Stickstoff überbrückte Co2-Einheiten (Co—Co[pm]: 247,8(4)) und gestreckte, von Stickstoff überbrückte Co3-Gruppen (Co—Co[pm]: 245,5(2); Co—Co—Co[°]: 180,0) in Kettenrichtung alternierend aufeinanderfolgen.Die Kristallstruktur von Ba[CoN] zeigt enge Verwandtschaft zum Ba[NiN]-Typ.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946201020
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  • 140
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    Oxo- und Thiotantal(V)-Verbindungen: Synthese von TaOX3 und TaSX3 (X = OR, SR) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1812-1817 
    Details
    ISSN: 0044-2313
    Keywords: Chloro, oxo and thiotantalum(V) compounds ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Oxo- and Thiotantalum(V) Compounds: Synthesis of TaOX3 and TaSX3 (X = OR, SR)TaO(OR)3 [R = tC4H9, Mes* (2)], TaO(SR)3 [R = tC4H9, p-Tolyl], TaS(OR)3 [R = tC4H9, Mes* (6)] and TaS(SR)3 [R = tC4H9, p-Tolyl] have been prepared by reaction of TaOCl3 and TaSCl3 with LiOR or LiSR. The reaction of TaCl5 with an excess of LiOMes* yields the chlorotantalum(V)compounds TaCl3(OMes*)2 and TaCl2(OMes*)3 (10). The synthesis of TaCl2(nC4H9)(OMes*)2 (11), Ta(Sp-Tolyl)5 and TaCl2(OEt)3 · C5H5N are also described. 2, 6, 10 and 11 decompose in benzolic solution or by heating under vacuum splitting off 2,4,6-tri-tert-butyl-phenol, n-butane respectively, and forming cyclometallated tantalum(V) complexes with the bidentate ligand OC6H2tBu2CMe2CH2. TaCl2(OEt)3 was investigated by X-ray diffraction analysis; the crystal structure has been found to be a binuclear tantalum complex with two bridging ethoxo ligands.
    Notes: TaO(OR)3 [R = tC4H9, Mes* (2)], TaO(SR)3 [R = tC4H9, p-Tolyl], TaS(OR)3 [R = tC4H9, Mes* (6)] und TaS(SR)3[ R = tC4H9, p-Tolyl] werden dargestellt durch Reaktion von TaOCl3 und TaSCl3 mit LiOR oder LiSR. Die Umsetzung von TaCl5 mit überschüssigem LiOMes* führt zu den Chlorotantal(V)-Verbindungen TaCl3(OMes*)2 und TaCl2(OMes*)3 (10). Darüber hinaus wird die Synthese von TaCl2(nC4H9)(OMes*)2 (11), Ta(Sp-Tolyl)5 und TaCl2(OEt)3 · C5H5N beschrieben. 2, 6, 10 und 11 zersetzen sich in benzolischer Lösung oder beim Erhitzen i. Vak. unter Abspaltung von 2,4,6-Tri-tert-butyl-phenol bzw. n-Butan und Bildung von cyclometallierten Tantal(V)-Verbindungen mit dem zweizähnigen Liganden OC6H2tBu2CMe2CH2. Die Kristallstruktur von TaCl2(OEt)3 wurde bestimmt; im zweikernigen Komplex sind die Tantalatome über zwei Ethoxo-Liganden verbrückt.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201025
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    Synthese und Struktur der Phosphor-verbrückten Übergangsmetallkomplexe [Fe2(CO)6(PR)6] (R = tBu, iPr), [Fe2(CO)4(PiPr)6], [Fe2(CO)3Cl2(PtBu)5], [Co4(CO)10(PiPr)3], [Ni5(CO)10(PiPr)6] und [Ir4(C8H12)4Cl2(PPh)4] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1821-1831 
    Details
    ISSN: 0044-2313
    Keywords: Cyclotriphosphanes ; transition metal carbonyl complexes of Fe, Co, Ir, and Ni ; phosphorus-bridged ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of the Phosphorus-bridged Transition Metal Complexes [Fe2(CO)6(PR)6] (R = tBu, iPr), [Fe2(CO)4(PiPr)6], [Fe2(CO)3Cl2(PtBu)5], [Co4(CO)10(PiPr)3], [Ni5(CO)10(PiPr)6], and [Ir4(C8H12)4Cl2(PPh)4](PtBu)3 and (PiPr)3 react with [Fe2(CO)9] to form the dinuclear complexes [Fe2(CO)6(PR)6] (R = tBu: 1; iPr: 2). 2 is also formed besides [Fe2(CO)4(PiPr)6] (3) in the reaction of [Fe(CO)5] with (PiPr)3. When PiPr(PtBu)2 and PiPrCl2 are allowed to react with [Fe2(CO)9] it is possible to isolate [Fe2(CO)3Cl2(PtBu)5] (4). The reactions of (PiPr)3 with [Co2(CO)8] and [Ni(CO)4] lead to the tetra- and pentanuclear clusters [Co4(CO)10(PiPr)3] (5), [Ni4(CO)10(PiPr)6] [2] and [Ni5(CO)10(PiPr)6] (6). Finally the reaction of [Ir(C8H12)Cl]2 with K2(PPh)4 leads to the complex [Ir4(C8H12)4Cl2(PPh)4] (7). The structures of 1-7 were obtained by X-ray single crystal structure analysis (1: space group P21/c (Nr. 14), Z = 8, a = 1 758.8(16) pm, b = 3 625.6(18) pm, c = 1 202.7(7) pm, β = 90.07(3)°; 2: space group P1 (Nr. 2), Z = 1, a = 880.0(2) pm, b = 932.3(3) pm, c = 1 073.7(2) pm, α = 79.07(2)°, β = 86.93(2)°, γ = 72.23(2)°; 3: space group Pbca (Nr. 61), Z = 8, a = 952.6(8) pm, b = 1 787.6(12) pm, c = 3 697.2(30) pm; 4: space group P21/n (Nr. 14), Z = 4, a = 968.0(4) pm, b = 3 362.5(15) pm, c = 1 051.6(3) pm, β = 109.71(2)°; 5: space group P21/n (Nr. 14), Z = 4, a = 1 040.7(5) pm, b = 1 686.0(5) pm, c = 1 567.7(9) pm, β = 93.88(4)°; 6: space group Pbca (Nr. 61), Z = 8, a = 1 904.1(8) pm, b = 1 959.9(8) pm, c = 2 309.7(9) pm. 7: space group P1 (Nr. 2), Z = 2, a = 1 374.4(7) pm, b = 1 476.0(8) pm, c = 1 653.2(9) pm, α = 83.87(4)°, β = 88.76(4)°, γ = 88.28(4)°).
    Notes: Die Cyclotriphosphane (PtBu)3 und (PiPr)3 reagieren mit [Fe2(CO)9] unter Bildung der Zweikernkomplexe [Fe2(CO)6(PR)6] (R = tBu: 1; iPr: 2). 2 entsteht auch bei der Reaktion von [Fe(CO)5] mit (PiPr)3 neben dem Komplex [Fe2(CO)4(PiPr)6] (3). Aus der Reaktion von PiPr(PtBu)2 und PiPrCl2 mit [Fe2(CO)9] kann weiterhin [Fe2(CO)3Cl2(PtBu)5] (4) isoliert werden. Die Umsetzungen von (PiPr)3 mit [Co2(CO)8] und [Ni(CO)4] führen zu den vier- und fünfkernigen Clustern [Co4(CO)10(PiPr)3] (5), [Ni4(CO)10(PiPr)6] [2] und [Ni5(CO)10(PiPr)6] (6). Weiterhin kann aus der Reaktion von [Ir(C8H12)Cl]2 mit K2(PPh)4 der Komplex [Ir4(C8H12)4Cl2(PPh)4] (7) erhalten werden. Die Strukturen von 1-7 konnten durch Einkristall-Röntgenstrukturanalyse aufgeklärt werden (1: Raumgruppe P21/c (Nr. 14), Z = 8, a = 1 758,8(16) pm, b = 3 625,6(18) pm, c = 1 202,7(7) pm, β = 90,07(3)°; 2: Raumgruppe P1 (Nr. 2), Z = 1, a = 880,0(2) pm, b = 932,3(3) pm, c = 1 073,7(2) pm, α = 79,07(2)°, β = 86,93(2)°, γ = 72,23(2)°; 3: Raumgruppe Pbca (Nr. 61), Z = 8, a = 952,6(8) pm, b = 1 787,6(12) pm, c = 3 697,2(30) pm; 4: Raumgruppe P21/n (Nr. 14), Z = 4, a = 968,0(4) pm, b = 3 362,5(15) pm, c = 1 051,6(3) pm, β = 109,71(2)°; 5: Raumgruppe P21/n (Nr. 14), Z = 4, a = 1 040,7(5) pm, b = 1 686,0(5) pm, c = 1 567,7(9) pm, β = 93,88(4)°; 6: Raumgruppe Pbca (Nr. 61), Z = 8, a = 1 904,1(8) pm, b = 1 959,9(8) pm, c = 2 309,7(9) pm. 7: Raumgruppe P1 (Nr. 2), Z = 2, a = 1 374,4(7) pm, b = 1 476,0(8) pm, c = 1 653,2(9) pm, α = 83,87(4)°, β = 88,76(4)°, γ = 88,28(4)°).
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201027
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    Darstellung und Kristallstruktur von CsBO2Professor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1867-1871 
    Details
    ISSN: 0044-2313
    Keywords: Cesium metaborate, CsBO2 ; crystal structure ; calculation of ECoN, MEFIR, MAPLE, CHARDI ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of CsBO2Colourless single crystals of CsBO2 have been prepared from intimate mixtures of CsO0.57 and B2O3 (Cs:B = 3.2:1.0; 600°C, 38 d). The structure determination from fourcircle diffractometer data (MoKα-, 443 Io (h k l), R = 3.1%, Rw = 2.0%) confirms the isotypy with NaBO2 and KBO2: space group R 3 c; a = 1 363.7(2) pm, c = 836.5(2) pm; Z = 18. A characteristic structure unit is the planar cyclic anion [B3O6]3-.Effective Coordination Numbers (ECoN), Mean Fictive Ionic Radii (MEFIR), the Madelung Part of Lattice Energy (MAPLE) and the Charge Distribution (CHARDI) are calculated and discussed.
    Notes: CsBO2 wurde durch Tempern inniger Gemenge von CsO0,57 und B2O3 (Cs:B = 3,2:1,0; 600°C, 38 d) in Form von farblosen plättchenförmigen Einkristallen erhalten. Die Strukturaufklärung (Vierkreisdiffraktometer, MoKα-, 443 Io (h k l), R = 3,1%, Rw = 2,0%) belegt die Isotypie mit NaBO2 und KBO2: Raumgruppe R 3 c; a = 1 363,7(2) pm, c = 836,5(2) pm; Z = 18. Charakteristische Strukturelemente sind planare, cyclische Anionen [B3O6]3.Effektive Koordinationszahlen (ECoN), Mittlere Fiktive Ionenradien (MEFIR), der Madelunganteil der Gitterenergie (MAPLE) und die Ladungsverteilung (CHARDI) werden berechnet und diskutiert.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201106
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    Na2B2Se7, K2B2S7 und K2B2Se7: Drei Perchalkogenoborate mit neuem polymeren AnionengerüstProfessor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1898-1904 
    Details
    ISSN: 0044-2313
    Keywords: Perchalcogenoborates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na2B2Se7, K2B2S7, and K2B2Se7: Three Perchalcogenoborates with a Novel Polymeric Anion NetworkNa2B2Se7 (I 2/a; a = 11.863(4) Å, b = 6.703(2) Å, c = 13.811(6) Å, β = 109.41(2)°; Z = 4), K2B2S7 (I 2/a; a = 11.660(2) Å, β = 6.827(1) Å, c = 12.992(3) Å, β = 106.78(3)°; Z = 4), and K2B2Se7 (I 2/a; a = 12.092(4) Å, b = 7.054(2) Å, c = 13.991(5) Å, β = 107.79(3)°; Z = 4) were prepared by reaction of stoichiometric amounts of sodium selenide (potassium sulfide) with boron and sulfur or of potassium selenide and boron diselenide, respectively, at 600°C with subsequent annealing. The crystal structures consist of polymeric anion chains of composition ([B2S7]2-)n or ([B2Se7]2-)n formed by spirocyclically connected five-membered B2S3 (B2Se3) rings and six-membered B2S4 (B2Se4) rings. The nine-coordinate alkaline metal cations are situated in between.
    Notes: Na2B2Se7 (I 2/a; a = 11,863(4) Å, b = 6,703(2) Å, c = 13,811(6) Å, β = 109,41(2)°; Z = 4); K2B2S7 (I 2/a; a = 11,660(2) Å, β = 6,827(1) Å, c = 12,992(3) Å, β = 106,78(3)°; Z = 4) und K2B2Se7 (I 2/a; a = 12,092(4) Å, b = 7,054(2) Å, c = 13,991(5) Å, β = 107,79(3)°; Z = 4) wurden durch Reaktion stöchiometrischer Mengen des Metallsulfids (-selenids) mit Bor und Schwefel (bzw. Bordiselenid) bei 600°C mit anschließendem Tempern dargestellt. Die Kristallstrukturen bestehen aus kettenförmigen ([B2S7]2-)n- bzw. ([B2Se7]2-)n-Polyanionen aus spirocyclisch verknüpften B2S3 (B2Se3)-Fünfringen und B2S4(B2Se4)-Sechsringen, zwischen denen sich die neunfach koordinierten Alkalimetallkationen befinden.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201110
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    Ein neues Kaliumhydrogensulfat, K(H3O)(HSO4)2  -  Synthese und StrukturProfessor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1921-1924 
    Details
    ISSN: 0044-2313
    Keywords: Potassium hydrogen sulfate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Potassium Hydrogensulfate, K(H3O)(HSO4)2  -  Synthesis and StructureSingle crystals of the new compound K(H3O)(SO4)2 are synthesized from the system potassium sulfate/sulfuric acid. The up to day not described compound crystallizes in the monoclinic space group P21/c with the unit cell parameters a = 7.203(1) b = 13.585(2) and c = 8.434(1) Å, β = 105.54(1)°, V = 795.1 Å3, Z = 4 and Dx = 2.107 g · cm-3.There are two crystallographically different tetrahedral SO3(OH) anions. The first kind S1 tetrahedra forms dimers, whereas the second kind S2 forms infinite chains bonded via hydrogen bridges. The S1 dimers are linked to the S2 chains via oxonium ions (hydrogen bonds).Potassium is coordinated by 8 oxygen atoms which belong to four different SO3(OH) tetrahedra. These potassium oxygen polyhedra are connected by common edges forming chains running parallel z.
    Notes: Im System Kaliumsulfat/Schwefelsäure ist ein neues, bisher nicht beschriebenes saures Sulfat der Zusammensetzung K(H3O)(HSO4)2 synthetisiert worden. Die Verbindung kristallisiert in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 7,203(1), b = 13,585(2) und c = 8,434(1) Å, β = 105,54(1)°, V = 795,1 Å3, Z = 4 und Dx = 2,107 g · cm-3.Es liegen zwei kristallographisch verschiedene SO3(OH)-Tetraeder vor. Die eine Tetraedersorte (S1) bildet Dimere aus, während die Tetraeder der Sorte S2 über Wasserstoffbrücken verbundene Ketten bilden. Die Dimeren der S1-Tetraeder sind mit den unendlichen Ketten der S2-Tetraeder über Oxoniumionen (Wasserstoffbrücken) verbrückt.Kalium ist von 8 Sauerstoffatomen, die vier verschiedenen SO3(OH) Tetraedern angehören, koordiniert. Die Kalium-Sauerstoff-Polyeder sind über gemeinsame Kanten miteinander verknüpft und bilden Ketten parallel der z-Achse.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201114
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    Darstellung, Kristallstruktur und elektronenmikroskopische Untersuchung von UNb6O16 - einem neuen niobreichen Oxid im System U/Nb/O (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1056-1065 
    Details
    ISSN: 0044-2313
    Keywords: UNb6O16 ; chemical transport ; crystal structure ; HRTEM ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Crystal Structure and Electron Microscopic Investigation of UNb6O16 - a New Niobium-rich Phase in the System U/Nb/OPowdery UNb6O16 was produced by heating (1 000°C or 1 100°C; evacuated silica tube) mixed powders of UO2, NbO2 and Nb2O5 (1:2:2). Single-crystals of UNb6O16 were obtained by chemical transport in a small temperature gradient (1 000°C → 990°C; transport agent NH4Cl). The lattice constants are a = 22 339(4) Å; b = 3.7750(6) Å; c = 7.249(3) Å; β = 97.61(3)° and Z = 2. The structure determination (space group C2) let to R = 0.026 (Rw = 0.026). Eight oxygen atoms surround U4+ like a trans-bis-capped octahedron, Nb4+ and Nb5+ are coordinated distorted octahedraly. The structure was checked and the occupation of the positions O8 and O9 was clarified with the program MAPLE4 [3]. A through focus series of high resolution transmission electron microscopic images was obtained which is in acceptable agreement with images calculated on the basis of the multi-slice method.
    Notes: Die Darstellung von pulverförmigem UNb6O16 gelingt durch Festkörperreaktion (1 000°C oder 1 100°C; evakuierte Quarzglasampulle) aus UO2, NbO2 und Nb2O5 (Gemenge 1:2:2). Schwarze Einkristalle sind durch chemischen Transport in einem geringen Temperaturgefälle (1 000°C→990°C; Transportmittel NH4Cl) zugänglich. UNb6O16 hat die Gitterkonstanten a = 22,339(4) Å; b = 3,7750(6) Å; c = 7,249(3) Å; β = 97,61(3)°; Z = 2. Die Strukturverfeinerung anhand von Einkristalldaten (RG C2) konvergierte bei R = 0,026 (Rw = 0,026). Die Metall-Sauerstoff-Koordinationspolyeder um Uran und Niob sind stark verzerrt. U4+ kann als dodekaedrisch bzw. trans-bis-bekappt oktaedrisch (CN = 8), Nb4+ und Nb5+ als oktaedrisch (CN = 6) koordiniert angesehen werden. Mit dem Programm MAPLE4 [3] konnte die Struktur überprüft, sowie die Halbbesetzung der Punktlagen O8 und O9 geklärt werden. Eine Defokusserie hochaufgelöster elektronenmikroskopischer Durchstrahlungsaufnahmen wurde mit rechnerischen Kontrastsimulationen verglichen.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200619
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    Fluorierung von Cyanurchlorid und Tieftemperatur-Kristallstruktur von [(ClCN)3F]+ [AsF6]- (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1132-1136 
    Details
    ISSN: 0044-2313
    Keywords: Cyanuric chloride ; FPDE values ; crystal structure ; chlorotrifluoro methane ; oxidative fluorinators ; ab initio computations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fluorination of Cyanuric Chloride and Low-Temperature Crystal Structure of [(ClCN)3F]+[AsF6]-The low-temperature fluorination of cyanuric chloride, (ClCN)3, with F2/AsF5 in SO2F2 solution yielded the salt [(ClCN)3F]+ [AsF6]- (1) essentially in quantitative yield. Compound 1 was identified by a low-temperature single crystal X-ray structure determination: R 3c, trigonal, a = b = 10.4246(23) Å, c = 15.1850(24) Å, V = 1429.1(4) Å 3, Z = 6, RF = 0.056, Rw = 0.076 (for significant reflections), RF = 0.088, Rw = 0.079 (for all reflections). Fluorination of neat (ClCN)3 with [NF4]+ [Sb2F11]- yielded NF3, CClF3, SbF3, N2 and traces of CF4. A qualitative scale for the oxidizing strength of the oxidative fluorinators NF4+ and (XCN)3F+ (X = H, F, Cl) has been computed ab initio.
    Notes: Durch Tieftemperaturfluorierung von Cyanurchlorid, (ClCN)3, mit F2/AsF5 in SO2F2-Lösung wurde [(ClCN)3F]+ [AsF6]- (1) in nahezu quantitativer Ausbeute dargestellt, aus SO2 bei Raumtemperatur umkristallisert und durch eine Tieftemperatur-Röntgenstrukturanalyse (-170°C) identifiziert: R 3c, trigonal, a = b = 10,4246(23) Å, c = 5,1850(24) Å, V = 1 429,1(4) Å3, Z = 6, RF = 0,056, Rw = 0,076 (für wesentliche Reflexionen), RF = 0,088, Rw = 0,079 (für alle Reflexe). Die Fluorierung von festem (ClCN)3 mit [NF4]+ [Sb2F11]- im Molverhältnis 1:2 lieferte NF3, CClF3, SbF3, N2 und Spuren an CF4. Eine qualitative Reihenfolge bezüglich der FPDE-Werte von NF4+ und (XCN)3F+ (X = H, F, Cl) wurde ab initio berechnet.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200630
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    Neue Komplexe der Lanthanoiden mit zweizähnigen Liganden. Die Strukturen von [(C17H17N2)GdBr2(thf)2] und [(C17H17N2)3Ln] (L = Sm, Gd) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 814-818 
    Details
    ISSN: 0044-2313
    Keywords: GdIII and SmIII octahedra complexes ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Complexes of the Lanthanoides with Bidentate Ligands. The Crystal Structures of [(C17H17N2)GdBr2(thf)2] and [(C17H17N2)3Ln] (L = Sm, Gd)Reaction of [(AIP)Li] with GdBr3 leads to a new mononuclear complex [(AIP)GdBr2(thf)2] 1. In contrast to this with SmI2 the compound [(AIP)3Sm] 2 is build up. Such complexes are also formed with Gd(OR*)3 (R* = OtBu2C6H3) and [(AIP)Li] in a 1:3 ratio, [(AIP)3Gd] 3. The structures of 1-3 were characterized by X-ray single crystal structure analysis (1: space group Pna21 (No. 33), Z = 4, a = 1 972.7(9) pm, b = 984.7(5) pm, c = 1 425.0(8) pm, α = β = γ = 90°; 2 · 2 THF: space group C2/c (No. 15), Z = 8, a = 3 644.4(9) pm, b = 1 437.5(5) pm, c = 2 334.4(7) pm, β = 1 21.07(6)°; 3: space group P2(1)/c (No. 14), Z = 4, a = 1 872.9(1) pm, b = 1 064.6(1) pm, c = 2 282.4(2) pm, β = 103.75(8)°).
    Notes: GdBr3 reagiert mit [(AIP)Li] zu dem einkernigen Komplex [(AIP)GdBr2(thf)2] 1. Mit SmI2 bildet sich dagegen überraschenderweise die Komplexverbindung [(AIP)3Sm] 2. Komplexe dieser Art bilden sich auch bei der Umsetzung von Gd(OR*)3 (R* = OtBu2C6H3) mit [(AIP)Li] im Verhältnis 1:3, [(AIP)3Gd] 3. Der Aufbau von 1-3 konnte durch Kristallstrukturanalyse geklärt werden (1: Raumgruppe Pna21 (Nr. 33), Z = 4, a = 1 972,7(9) pm, b = 984,7(5) pm, c = 1 425,0(8) pm, α = β = γ = 90°; 2 · 2 THF: Raumgruppe C2/c (Nr. 15), Z = 8, a = 3 644,4(9) pm, b = 1 437,5(5) pm, c = 2 334,4(7) pm, β = 1 21,07(6)°; 3: Raumgruppe P2(1)/c (Nr. 14), Z = 4, a = 1 872,9(1) pm, b = 1 064,6(1) pm, c = 2 282,4(2) pm, β = 103,75(8)°).
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200510
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    Trigonal-bipyramidale Cluster mit interstitiellen C2-Hanteln in den Chloriden K[M5(C2)]Cl10 (M = La, Ce, Pr) und Rb[M5(C2)]Cl10 (M = Pr, Nd)Professor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1872-1878 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanide clusters ; interstitial C2-units ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trigonal-Bipyramidal Clusters with Interstitial C2-Units in the Chlorides K[M5(C2)]Cl10 (M = La, Ce, Pr) and Rb[M5(C2)]Cl10 (M = Pr, Nd)The chlorides K[M5(C2)]Cl10 (M = La, Ce, Pr) and Rb[M5(C2)]Cl10 (M = Pr, Nd) are obtained via metallothermic reduction of the trichlorides MCl3 with potassium and rubidium, respectively, in the presence of metal M and carbon in sealed niobium containers at temperatures between 700 and 900°C. They contain trigonal bipyramids, interstitially stabilized by a C2 unit, [M5(C2)], and crystallize with the hexagonal (K[Pr5(C2)]Cl10, Rb[M5(C2)]Cl10 with M = Pr, Nd) or monoclinic (K[M5(C2)]Cl10 with M = La, Ce) crystal system. The trigonal bipyramids are surrounded by nine inner Cl- ligands (capping the nine edges) and by 12 (hexagonal) or 13 (monoclinic) outer ligands and are connected via all of the 21 and 22 ligands, respectively. Special features are Cla-a-a (hexagonal) and Cla-a-a-a (monoclinic) bridges.
    Notes: Die Chloride K[M5(C2)]Cl10 (M = La, Ce, Pr) und Rb[M5(C2)]Cl10 (M = Pr, Nd) erhält man durch metallothermische Reduktion der entsprechenden Trichloride MCl3 mit Kalium bzw. Rubidium in Gegenwart von Metall M und Kohlenstoff in verschweißten Niobampullen bei Temperaturen zwischen 700 und 900°C. Sie enthalten durch C2-Hanteln stabilisierte trigonale Bipyramiden [M5(C2)] und kristallisieren im hexagonalen (K[Pr5(C2)]Cl10, Rb[M5(C2)]Cl10 mit M = Pr, Nd) bzw. im monoklinen Kristallsystem (K[M5(C2)]Cl10 mit M = La, Ce). Die trigonalen Bipyramiden werden von neun inneren Cl- (über den neun Kanten) und von 12 (hexagonal) bzw. 13 (monoklin) äußeren Liganden koordiniert und über sämtliche Liganden miteinander verknüpft, wobei als Besonderheiten Cla-a-a- (hexagonal) bzw. Cla-a-a-a-Brücken (monoklin) auftreten.
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    URL: http://dx.doi.org/10.1002/zaac.19946201107
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    Synthese und Kristallstruktur von Cu2PtIIPt3IVS8Professor Heinrich Oppermann zum 60. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1909-1914 
    Details
    ISSN: 0044-2313
    Keywords: Cu2Pt+IIPt3+IVS8; Copperthioplatinate(II,IV) ; mixed valent compounds ; crystal structure ; Rietveld refinement ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Cu2PtIIPt3IVS8(NH4)2PtCl6 and Cu(CH3COO)2 were reacted at 380 K in a constant flow of H2S in the molar ratio of 2:1. Subsequent annealing of the product in sealed quartz glass ampoules in the presence of CuS as a buffer for the sulfur activity (temperature range 770 to 870 K) yields Cu2Pt4S8 as a polycrystalline, greyish black powder. Cu2Pt4S8 crystallizes in the space group P2/n (No. 13) with the cell parameters a = 10.6478(2), b = 6.9350(1), c = 6.7411(1) Å, β = 91.942(1), Z = 2. The structure determination and refinement were performed by the means of x-ray powder diffraction data of this first copperthioplatinate. There are no isotypic compounds known, so far. According to the characteristic coordination of the metals by sulfur, the oxidation states are Cu+I, Pt+II and Pt+IV, the compound may be formulated as Cu2Pt+IIPt3+IVS8. Cu2Pt4S8 exhibits diamagnetic and semiconducting properties.
    Notes: Die Umsetzung von (NH4)2PtCl6 und Cu(CH3COO)2 im molaren Verhältnis von 2:1 bei 380 K im H2S Strom, gefolgt von Tempern des Produktes in abgeschmolzenen Quarzglasampullen zwischen 770 und 870 K, in Gegenwart von CuS als Puffer für die Schwefelaktivität, ergibt Cu2Pt4S8 als polykristallines, grau-schwarzes Pulver. Cu2Pt4S8 kristallisiert in der Raumgruppe P2/n (Nr. 13) mit den Gitterkonstanten a = 10,6478(2), b = 6,9350(2), c = 6,7411(1) Å, β = 91,942(1), Z = 2. Die Strukturaufklärung und -verfeinerung erfolgten unter Verwendung von Röntgenpulverdaten dieses ersten Kupferthioplatinats. Isotype Verbindungen sind nicht bekannt. Nach der jeweils charakteristischen Umgebung durch Schwefel liegen Cu+I, Pt+II und Pt+IV gemäß Cu2Pt+IIPt3+IVS8 vor. Cu2Pt4S8 ist diamagnetisch und halbleitend.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946201112
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    Synthese und Kristallstruktur der molekularen Clusterverbindung W6Br14Professor Wilhelm Preetz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1312-1320 
    Details
    ISSN: 0044-2313
    Keywords: Tungsten bromide cluster compound, W6Br14 ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of the Molecular Cluster Compound W6Br14Brownish-black crystals of W6Br14 are formed in the direct synthesis from W6Br12 and Br2 (400 K). The compound crystallizes cubically with neutral cluster molecules ([W6Br8i]Br6a): a = 13.458 Å; Pn3 (Nr. 201); d̄(W—W) = 2.653 Å; d̄(W—Bri) = 2.616 Å; d̄(W—Bra) = 2.569 Å. The W atoms are 0.03 Å outside of the Br8i cube faces. The molecules are arranged according to a cF point configuration, but each is rotated -23° about a threefold axis in order to avoid short inter cluster distances Bra—Bra. Nevertheless, via 12 short intermolecular distances per cluster of about d(Bri … Bra) = 3.487 Å the clusters are interconnected by forming two independent and interpenetrating 3D nets (Cu2O type). Although local distortion of the M6X8i cluster does not occur, as is expected for this system with 22 electrons per M6 octahedron, it is assumed that the Jahn-Teller theorem is fulfilled collectively via the low-symmetry nets of intermolecular interactions.
    Notes: W6Br14 wird bei der direkten Synthese aus W6Br12 und Br2 in Form braum-schwarzer Kristalle erhalten (400 K). Die Verbindung kristallisiert kubisch mit neutralen Clustermolekülen ([W6Br8i]Br6a): a = 13.458 Å; Pn3 (Nr. 201); d̄(W—W) = 2.653 Å; d̄(W—Bri) = 2.616 Å; d̄(W—Bra) = 2.569 Å. Die W-Atome liegen um 0.03 Å außerhalb der Br8i-Würfelflächen. Die Moleküle sind entsprechend einer cF-Konfiguration verteilt und dabei um jeweils eine der 3zähligen Achsen gedreht (-23°; Vermeidung kurzer inter-Clusterabstände Bra—Bra). Es resultieren aber pro Cluster 12 sehr kurze intermolekulare Abstände d(Bri … Bra) = 3.487 Å, über welche die Cluster zu zwei unabhängigen, sich durchdringenden 3D-Netzen miteinander verbunden sind (Cu2O-Typ). Die bei einem M6X8i-Cluster mit 22 Elektronen pro M6-Oktaeder erwartete lokale Verzerrung tritt nicht auf. Es wird angenommen, daß das Jahn-Teller-Theorem kollektiv über die niedersymmetrischen Netze intermolekularer Wechselwirkungen erfüllt wird.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19946200728
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    Crystal structure and in vitro antitumour activity of dibutylbis(5-chloro-2-hydroxybenzoato)tin(IV) (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 8 (1994), S. 19-23 
    Details
    ISSN: 0268-2605
    Keywords: Diorganotin ; carboxylate ; crystal structure ; antitumour ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The crystal structure of the title compound, [nBu2Sn(5-Cl-2-OH-C6H3CO2)2], shows that in the monomeric species the six-coordinate Sn atom exists in a skew trapezoidal bipyramidal geometry in which the four O donor atoms, derived from two asymmetrically chelating carboxylate ligands, define the basal plane and the n-butyl substituents lie over the weaker Sn—O interactions defining a C—Sn—C angle of 147.6(2)°. An unusual feature of the structure is the presence of both intra- and inter-molecular hydrogen bonding contacts which serve to stabilize the structure. The in vitro antitumour activity of this compound against mammary and colon carcinoma cell lines is also reported.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/aoc.590080105
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  • 152
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    Crystal structure and fungitoxicity of aquatributyltin N-phthaloylglycinateAtomic coordinates for this structure have been deposited with the Cambridge Crystallographic Data Centre. The coordinates can be obtained from the Cambridge Crystallographic Data Centre, University Chemical Laboratory, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, UK. (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 8 (1994), S. 37-42 
    Details
    ISSN: 0268-2605
    Keywords: Triorganotin ; carboxylate ; crystal structure ; fungitoxicity ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The [nBu3Sn(N-phthaloylglycinate)(OH2)] compound has been prepared and characterized. The crystal structure reveals the tin atom, in each of the two molecules comprising the asymmetric unit, to exist in a distorted trigonal bipyramidal geometry in which the trigonal plane is defined by the three organic substituents and the axial sites are occupied by an oxygen atom derived from a monodentate carboxylate ligand and a coordinated water molecule. The [nBu3Sn(N-phthaloylglycinate)(OH2)] compound and three other triorganotin derivatives of N-phthaloyl-protected amino acids display marked toxicity against several economically important plant pathogenic fungi.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/aoc.590080108
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  • 153
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    Synthesis and characterization of diorganotin(IV) derivatives of 2-mercaptopyridine and crystal structure of diphenyl pyridine-2-thiolatochlorotin(IV) (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 8 (1994), S. 397-407 
    Details
    ISSN: 0268-2605
    Keywords: Organotin ; 2-mercaptopyridine ; pyridine-2-thiolato complexes ; Mössbauer ; IR ; NMR ; crystal structure ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Diorganotin(IV) derivatives of 2-mercaptopyridine (HSPy), R2Sn(SPy)2, R2SnCl(SPy) (R = Me, iPr, nBu, tBu, Cy, Ph) and Cy2SnBr(SPy), were obtained from R2SnX2 (X = Cl, Br) and NaSPy.Ph2SnCl(SPy) crystals, as determined by singlecrystal X-ray diffraction, are monoclinic in the space group P21/n. Tin forms with the bidentate SPy ligand a four-membered chelate ring with a short NSnS bite angle of 64.8(1)° leading to a heavily distorted trigonal-bipyramidal environment about tin. Apical Cl-Sn-N angle = 156.1(1)° equatorial C-Sn-C angle = 121.9(2)°. From 119Sn Mössbauer and IR data, analogous structures are inferred for the other solid compounds R2SnX(SPy), and distorted octahedral molecular structures for the solid compounds R2Sn(SPy)2 with R in the trans position, and sulfur atoms and nitrogen-donor atoms each in cis positions. According to IR and 1H, 13C and 119Sn NMR data, the solid-state molecular structures are retained in chloroform solution.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/aoc.590080414
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  • 154
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    Synthesis, spectroscopic characterization and fungicidal activity of triphenyltin derivatives of N,N-dimethylglycine: Crystal structure of [dimethyl(carboxylatomethyl)ammonium]-chlorotriphenylstannateAtomic coordinates for this structure have been deposited with the Cambridge Crystallographic Data Centre. The coordinates can be obtained from the Cambridge Crystallographic Data Centre, University Chemical Laboratory, University of Camhridgc. Lenslield Road. Cambridge CB2 1 EW. UK. (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 8 (1994), S. 33-36 
    Details
    ISSN: 0268-2605
    Keywords: Organotin ; fungicidal ; crystal structure ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new triorganotin complexes formulated as Me2HNCH2COO · Ph3SnX, X = Cl, NCS were prepared and spectroscopically characterized, and their fungicidal properties against Ceratocystis ulmi were determined. An X-ray structure for [dimethyl(carboxylatomethyl)ammonium] chlorotriphenylstannate is also reported.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/aoc.590080107
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  • 155
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    The structure of Mo4Cl8(PEt3)4: How unrecognized disorder previously reduced the quality of the refinement (1991)
    Springer
    Journal of cluster science 2 (1991), S. 121-129 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum tetranuclear cluster ; rectangular ; triethylphosphine ligand ; preparation ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The preparation and structure of the title compound were reported several years ago by McCarly and co-workers ((1978).J. Am. Chem. Soc. 100, 7900). Curiously, it was reported that refinement of the structure converged at exceptionally high figures of merit (R=0.126;R w =0.158), but no reason was given. In view of a recent observation in this laboratory (Chen and Cotton (1991).J. Am. Chem. Soc. 113, 5857) that a similar type of compound, [Re4Cl8(μ-O)2(μ-OMe)2]2− exhibited a subtle but elegant disorder, we reexamined the crystal structure of the title compound. It is found to have 92% of the Mo4 rectangles in one orientation (the only one previously included in the refinement) and 8% in an orientation perpendicular to the main one. In both orientations the ligand positions are approximately the same. The figures of merit are nowR=0.041;R w =0.064. The three structure parameters previously reported are now only slightly different: Mo-Mo=2.210(1) vs. 2.211(3) Å; Mo-Mo'=2.897(1) vs. 2.901(2) Å; angle Mo-Clb-Mo=74.2[8]° vs. 74.4(2)°. We report here the complete structure.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702953
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    The characterization of high-tech materials: Perspectives, challenges, trends (1991)
    Springer
    Microchimica acta 104 (1991), S. 177-214 
    Details
    ISSN: 1436-5073
    Keywords: atomic structure ; crystal structure ; microstructure ; constructions ; topochemistry ; graphite ; glassy carbon ; pyrolytic carbon ; microelectronics ; carriers of information ; refractory metal alloys ; life time ; recrystallization ; fatigue ; photon probe techniques ; electron probe techniques ; ion probe techniques ; electrical field probes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract From the Stone Age on, developmental periods of mankind carry the names of materials. Materials determine the applicability of key technologies and these are in turn of major significance for the economic success and the social development in modern society. Today's high-tech materials are the consequence of an improved understanding of the structure and composition of matter and of the interplay of microstructure and minor and trace constituents. We can distinguish four basic dimensional structural categories of materials: (a) the atomic structure level; (b) the crystal, glassy or amorphous structural level; (c) the microstructural level; (d) the level of constructions. As an example, these structural levels are described in some detail for graphite, a material used extensively throughout Analytical Chemistry. Decisive differences at the microstructural level result in graphitic materials with very varying properties: polycrystalline electrographite, glassy carbon, and pyrolytic graphite. Examples for the use of these materials in ETAAS are discussed. Structural features together with topochemical and trace chemical characteristics are studied today by a wide variety of analytical instrumentation and methods of modern materials analysis which can be grouped into four categories of techniques: (a) photon probe techniques; (b) electron probe techniques; (c) ion probe techniques; (d) electrical field probes. The most important of those techniques are discussed shortly with respect to their main characteristics as lateral and depth resolution, detection sensitivity, additional bonding or structural information, depth profiling possibilities etc. The constructions are the ultimate level of a materials structure. Structures of microelectronic components reach dimensionally into the domain of microstructure whereas constructions in heavy industry are of meter-ton dimensions. Progress in the use of materials as carriers of information is visualized by a morphological comparison of the sound tracks of conventional records with the information imprinted in optical discs. It is important to conceive materials as dynamic systems with limited lifetime. Fatigue and recrystallization are prominent relevant phenomena which must be studied by microstructural and topochemical methods. Dispersion strengthened microalloys like TZM, HT-molybdenum and NS-tungsten are discussed as examples how materials can be improved with respect to their extended use under extreme conditions. Again, a thorough structural and topochemical characterization was the basis of a successful respective materials development although a multitude of relevant topochemical questions still remain to be solved. Lifetime investigations are an essential tool of materials development as well as quality control. Relevant investigations for various tube materials for ETAAS are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01245508
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  • 157
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    Conformational analysis of fluorinated copolymers of tetrafluoroethylene (1991)
    Springer
    Colloid & polymer science 269 (1991), S. 477-482 
    Details
    ISSN: 1435-1536
    Keywords: Polytetrafluoroethylene ; copolymers ; conformation ; conformational disorder ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract Conformational analysis of fluorinated copolymers of tetrafluoroethylene (TFE) is performed by taking into account only intramolecular effects (isolated-chain model). In particular, variations of the chain conformation, which are induced by incorporating different side groups, such as −Cl, −CF3, −OCF3, −OCF2CF3, and −OCF(CF3)2, are investigated and discussed with respect to qualitative correlations between conformation, crystal structure, and supramolecular morphology.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00655885
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    Atomistic calculations of crystal structures of polyisobutylene (1991)
    Springer
    Colloid & polymer science 269 (1991), S. 449-454 
    Details
    ISSN: 1435-1536
    Keywords: Polyisobutylene ; atomistic calculations ; conformational analysis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract Semiempirical atomistic calculations are performed to investigate the crystalline structure of stretched poly(1,1-dimethylethylene), or polyisobutylene. The packing analysis was done without any lattice symmetry assumptions. The results are in good agreement with the x-ray analysis and favor Tanaka's model II. The calculations show several other crystalline structures with the chains in an all-gauche conformation. They have a somewhat higher density and may play a role in a hypothetical high-pressure phase of polyisobutylene.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00655881
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  • 159
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    Structural studies of 2,2-Diphenyl-1-picrylhydrazine: A clathrate forming compound (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 203-217 
    Details
    ISSN: 1573-1111
    Keywords: Diarylpicrylhydrazine ; clathrate ; single crystal ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 2,2-Diphenyl-1-picrylhydrazine was crystallized from both tetrahydrofuran and chloroform. The crystal structures of samples from both preparations were determined by X-ray diffraction at low temperatures. Both crystals are clathrates with solvent molecules included as guest species in a host framework formed by the diphenylpicrylhydrazine molecules. The structures are rhombohedral, space groupR3. For the crystal from tetrahydrofuran, at 228 K,a = 25.820(4),c = 15.096(2) Å,Z = 18,R = 0.084 andwR = 0.133. For the crystal from chloroform, at 115 K,a = 25.453(12),c = 15.083(3) Å,Z = 18,R = 0.117 andwR = 0.153. Each unit cell contains three cavities which have approximate cylindrical shape with diameter 7.8 Å and height 6.0 Å, and 3 point symmetry. The integrity of the host framework is maintained only through van der Waals forces rather than through intermolecular hydrogen bonding as is found in many other known organic cathrates. The conformation of the trinitroanilino group of the hydrazine molecule is similar to that in the related trinitroanilinocarbazole molecule. The N-N bond approximates a single bond, and both hydrazine N atoms aresp 2 hybridized.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01066204
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  • 160
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    Channel inclusion of potassium and tetrachloroplatinate ions in a complex formed between 1,3-diamino-2-propanone and K2PtCl4 in an acidic medium (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 225-232 
    Details
    ISSN: 1573-1111
    Keywords: Diaminopropanone ; potassium tetrachloroplatinate ; channel inclusion ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystalline complex dipotassium 1,3-diammonio-2-propanone tetrachloroplatinate trihydrate, formulated as K2[(NH3CH2C)2O][PtCl4]2 · 3H2O, has been prepared while synthesizing complexes analogous tocis-dichlorodiamine Pt(II). Its structure is orthorhombic, space groupPnma,M r = 896.1,F(000) = 1640,a = 8.428(4),b = 20.360(10),c = 12.141(7)A,V = 2083.3Å3,Z = 4,D x = 2.860 g cm−3, μ(MoK x) = 196 cm−1, finalR = 0.083 for 1379 unique reflections. The structure consists of a very extended hydrogen bonded network which involves half of the PtCl4 2− ions, the organic molecules and the water molecules of hydration, leaving large oval channels which accommodate potassium cations and tetrachloroplatinate anions. Within the channel the potassium and tetrachloroplatinate ions pack in columns extending along the a axis. The dense packing is rather reminiscent of that found in the neat salt where each potassium ion is surrounded by six chlorine atoms which describe a polyhedron of a distorted trigonal prism with K+ —C1 distances ranging between 3.163–3.187 Å. There is some indirect evidence for the formation of 1,3-diammonio-2-propanone dications which counterbalance the charges of half of the PtCl4 2− ions by protonation of each of the amino nitrogens. The carbonyl oxygens, however, are involved only in a very weak O-C-O interactions along thea axis.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01066206
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  • 161
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    Molecular encapsulation of transition metal complexes in cyclodextrins. Part 2. Synthesis and crystal structures of 2:1 adducts between α-cyclodextrin and metallocenium hexafluorophosphates [η5-C5H5)2M]PF6(M = Fe, Co, Rh) (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 255-265 
    Details
    ISSN: 1573-1111
    Keywords: Cyclodextrin inclusion compound ; metallocene ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title metallocenium salts form crystalline 2:1 host:guest inclusion compounds withα-cyclodextrin, [(η5-C5H5)2M]PF6 · 2α-CD · 8H2O (1, M = Fe;2, M = Co;3, M = Rh). The X-ray crystal structures of1 and3, and the lattice constants, crystal system and space group of2 have been determined. Crystal data: triclinic, space groupP1 (No. 1),Z = 1;1,a = 13.865 (2) Å,b = 13.839 (2) Å,c = 15.520 (2) Å,α = 91.43 (2)°,β = 85.81 (2)°,γ = 120.22 (2)°, andR F = 0.089 for 4257 observed MoK α reflections [I 〉 3δ(I)];2,a = 13.810 (2) Å,b = 13.872 (2) Å,c = 15.560 (2) Å,α = 93.99 (2)°,β = 87.06 (2)°,γ = 120.04 (2)°;3,a = 13.756 (1) Å,b = 13.863 (1) Å,c = 15.561 (2) Å,α =94.39 (1)°,β = 86.92 (1)°,γ = 119.89 (1)°, andR F = 0.061 for 11142 observed MoK α reflections [I 〉 3δ(I)]. In the crystals of1 and3, two α-cyclodextrin molecules are arranged head-to-head to form a dimer by means of intermolecular hydrogen bonding across the secondary hydroxyl faces of adjacent α-CD monomers. The dimers are stacked along the crystallographicc axis to form a channel-type structure. The metallocenium cation is encapsulated within the cavity of the dimer, while the PF 6 − anion is located outside the cavity, being centered between the primary hydroxyl faces of adjacent dimers. Eight water molecules of hydration per asymmetric unit reside in the spaces between the α-CD columns. In view of the almost identical crystal data for2 a similar structure can be assumed for the cobaltocenium adduct.
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    URL: http://dx.doi.org/10.1007/BF01066209
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    The crystal structures of α, ω-diaminoalkanecadmium(II) tetracyanonickelate(II)-Aromatic molecule inclusion compounds. V. Toluidine clathrates of the hosts built of the diamines, 1,4-diaminobutane, 1.5-diaminonentane, and 1,8-diaminooctane (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 11 (1991), S. 137-152 
    Details
    ISSN: 1573-1111
    Keywords: cadium ; crystal structure ; Hofmann-diam-type ; 1,4-diaminobutane ; 1,5-diaminopentane ; 1,6-diaminohexane ; 1,8-diaminooctane ; tetracyanonickelate ; toluidine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structures have been analyzed for the threeo-toluidine clathrates,catena-[catena-μ-(1,4-diaminobutane)cadmium(II) tetra-μ-cyanonickelate(II)]-o-toluidine(2/3),4-o,catena-[catena-μ-(1,5-diaminopentane)cadmium(II) tetra-μ-cyanonickelate(II)]-o-toluidine(3/4),5-o, andcatena-[catena-μ-(1,8-diaminooctane)cadium(II) tetra-μ-cyanonickelate(II)]-o-toluidine(1/1),8-o, for am-toluidine onecatena-[catena-μ-(1,5-diaminopentane)cadmium(II) tetra-μ-cyano-nickelate(II)]-m-toluidine(1/1),5-m, and for ap-toluidine onecatena-[catena-μ-(1,8-diaminooctane)cadium(II) tetra-μ-cyanonickelate(II)]-p-toluidine(1/1),8-p. 4-o crystallizes in the triclinic space groupPī,a/Å = 9.806(3),b/Å = 14.388(3),c/Å = 7.725(2), α/° = 89.71(2), β/° = 89.96(2), γ/° = 98.12(2),V/Å3 = 1078.8(5),Z = 2, 3750 reflections,R = 0.056;5-o: tetragonalP4lmmm, (a = b)/Å = 7.485(7),c/Å = 10.06(3),V/Å3 = 563(2),Z = 1, 573 reflections,R = 0.19;8-o: monoclinicP2/m,a/Å = 11.513(4),b/Å = 7.626(1),c/Å = 7.101(1), β/° = 109.63(3),V/Å3 = 587.2(2),Z = 1, 1682 reflections,R = 0.058;5-m: orthorhombicPbam,a/Å = 12.254(6),b/Å = 20.62(1),c/Å = 7.804(1),V/Å3 = 1972(1),Z = 4, 2240 reflections,R = 0.059; and8-p: triclinic,Pī,a/Å = 11.52(1),b/Å = 7.632(3),c/Å = 7.039(4), α/° = 88.93(4), β/° = 109.71(5), γ/° = 82.81(9),V/Å3 = 576.9(6),Z = 1, 2598 reflections,R = 0.042. Their structures are substantially similar to the already-known structure ofcatena-[catena-μ-(1,6-diaminohexane)cadmium(II) tetra-μ-cyanonickelate(II)]-o-toluidine(1/1): the guest toluidine molecules are accommodated in the cavities formed betweencatena-[cadmium(II) tetra-μ-cyanonickelate(II)] layers bridged by the ambidentate α,ω-diaminoalkane ligands at the cadmium(II) atoms. The carbon chain length of the α,ω-diaminoalkane influences the number of cavities per formula unit and the deformation of the metal complex layers.
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    URL: http://dx.doi.org/10.1007/BF01153297
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    Crystal and molecular structures ofp-(1,1,3,3-tetramethylbutyl)calix[5]arene and its 1 : 1 complex with toluene (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 11 (1991), S. 171-183 
    Details
    ISSN: 1573-1111
    Keywords: Calixarene ; inclusion compounds ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A cyclic pentamer was obtained fromp-(1,1,3,3-tetramethylbutyl) phenol. It crystallizes from a mixture of acetone and toluene at room temperature giving a 1 : 1 complex with toluene (compound A), whereas at 50°C the empty form (compound B) is obtained. Crystals of A are orthorhombic, space groupPna21,a = 20.083(2),b = 12.936(6),c = 28,423(1) Å,Z = 4, finalR value = 0.067. The empty form, B, is monoclinicP21/c,a = 18.695(2),b = 11.673(5),c = 35.100(4) Å, β = 114.33(1),Z = 4, finalR value = 0.135. The macrocycle is in the cone conformation for both compounds; the toluene molecule lies in the cone as often found for calix[4]arenes.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01153300
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    Novel cage-like cavity accommodating a pair of guest molecules in the structure ofcatena-[dl-1,2-diaminopropanecadmium(II) tetra-μ-cyanocadmate(II)]-(1,2-dichloroethane)(1/1) (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 11 (1991), S. 397-403 
    Details
    ISSN: 1573-1111
    Keywords: Cadmium cyanide ; cadmium tetracyanocadmate ; crystal structure ; dichloroethane ; metal complex host ; propylenediamine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title clathrate Cd(dl-pn)Cd(CN)4·CH2CICH2CI (pn=dl-1,2-diaminopropane=dl-propy-lenediamine) crystallizes in the monoclinic space groupP2 ,a = 8.278(2),b = 14.904(2),c = 14.477(1) Å,β = 91.24(1)°,V = 1785.7(1) Å3,Z = 4,R = 0.068 for 4993 independent reflections. A novel three-dimensional host is built of the alternate array of the pn-chelated octahedral Cd and the tetrahedral Cd(CN)4 linked at every N atom to the former Cd to provide a cage-like cavity for a pair of 1,2-dichloroethane guest molecules.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01041417
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    Analysis of the steric strain in the polypeptide backbone of protein molecules (1991)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 11 (1991), S. 223-229 
    Details
    ISSN: 0887-3585
    Keywords: protein structure ; crystal structure ; dihedral angles ; cis peptides ; protein active sites ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The extent to which local strain is present in the polypeptide backbone of folded protein molecules has been examined. The occurrence of steric strain associated with nonproline cis peptide bonds and energetically unfavorable main chain dihedral angles can be identified reliably from the well ordered parts of high resolution, refined crystal structures. The analysis reveals that there are relatively few sterically strained features. Those that do occur are located overwhelmingly in regions concerned with function. We attribute this to the greater precision necessary for ligand binding and catalysis, compared with the requirements of satisfactory folding.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340110307
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    X-Ray Structure and Crystal Lattice Interactions of the Taxol Side-Chain Methyl Ester (1991)
    Springer
    Pharmaceutical research 8 (1991), S. 908-912 
    Details
    ISSN: 1573-904X
    Keywords: taxol side chain ; crystal structure ; crystal lattice interactions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A colorless, parallelepiped crystal of methyl (2R,3S)-N-benzoyl-3-phenylisoserinate belonging to the space group P2l with a = 5.414(4), b = 7.813(1), c = 17.802(7) Å, β = 90.87(4)°, Z = 2, V = 752.9 Å3, D calc = 1.32 g cm−3, and µcalc = 1.02 cm−1 was selected and the structure solved using direct methods. Refinement led to a final R = 0.079 for 819 [F o ≥ 5σ(Fo)] reflections. Intermolecular hydrogen-bonding interactions are prevalent in the crystal lattice of this compound.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1015863814901
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    Crystal and molecular structure ofN,N′,N″-tritosyl-5,8,14,17,23,26-hexamethyl-2,11,20-triaza[3.3.3]-paracyclophane 1 : 1 dichloromethane clathrate (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 11 (1991), S. 41-48 
    Details
    ISSN: 1573-1111
    Keywords: N-tosyl azamacrocycles ; crystal structure ; clathrate formation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structure of the title compound, C51H57N3O6S3·CH2Cl2 has been determined by single crystal X-ray analysis and refined to anR-value of 0.069 for 1032 reflections. The crystal is trigonal, space groupR3, witha = 21.255(7),c = 11.317(4), andZ = 3. One molecule of dichloromethane used as solvent is enclathrated in the crystal lattice.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01073682
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  • 168
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    Air stable liquid clathrates: Solid state structure and hydrocarbon solubility of organic cation triiodide salts (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 11 (1991), S. 103-114 
    Details
    ISSN: 1573-1111
    Keywords: Liquid clathrate ; triiodide ; NMR ; crystal structure ; molten salts
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A series of air and water stable organic cation triiodide salts have been prepared and characterized. Almost all of the salts isolated sustain liquid clathrate phases in the presence of benzene or toluene, the compositions of which were determined via1H NMR spectroscopy. Two of the salts were also characterized via X-ray crystallography in order to determine the nature of any solid state interionic interactions (1-ethylpyridinium triiodide, monoclinic,P21/c,a = 9.6031(7),b = 15.129(3),c = 8.8160(16) Å, β = 104.192(11)°,Z = 4,R = 0.041 for 2463 independent observed reflections; 1,2,4-trimethylpyridinium triiodide, orthorhombic,Pbcm,a = 9.434(4), 20.176(4), 7.411(4) Å,Z = 4,R = 0.045 for 966 observed reflections).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01153294
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  • 169
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    Thermoanalytical investigation of the guest-release process in aromatic-guest clathrates of three-dimensional metal complex hosts (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 29-37 
    Details
    ISSN: 1573-1111
    Keywords: activation energy ; benzene ; cadmium complex ; crystal structure ; ethylenediamine ; guest-release process ; propylenediamine ; pyrrole ; tetracyanocadmate ; tetracyanomercurate ; tetracyanonickelate ; thermal analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The guest-release process was investigated in terms of the activation energy evaluated by thermogravimetry for the en-Td-type clathratescatena-μ-[catena-μ-(ethylenediamine)cadmium(II) tetra-μ-cyanocadmate(II) or -mercurate(II)]-benzene(1/2), -benzene-d 6(1/2), and -pyrrole(1/2), the Hofmannen-type clathratescatena-[catena-μ-(ethylenediamine)cadmium(II) tetra-μ-cyanonickelate(Il)]-benzene (1/2) and -pyrrole(1/2), the Hofmann-pn-type clathratecatena-[catena-μ-(dl- orl-propylenediamine (cadmium(II) tetra-μ-cyanonickelate(II)]-pyrrole(2/3), and the pn-Td-type clathratescatena-[catena-μ-(dl-propylenediamine) or -(l-propylenediamine)cadmium(II) tetra-μ-cyanocadmate(II)]-benzene(2/3). Values of the activation energy are correlated with the structural change in the metal complex host accompanied by the release of the guest molecules. The crystal structure ofcatena-[ethylenediaminecadmium tetra-μ-cyanonickelate(II)], the residual host of the Hofmann-en-type, has been analyzed to elucidate the correlation.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01041637
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  • 170
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    Stabilization of H2O ⁗ BF3 by hydrogen bonding to 18-crown-6 (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 153-158 
    Details
    ISSN: 1573-1111
    Keywords: Hydrogen bonding ; 18-crown-6 ; boron trifluoride ; water ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The decomposition of H2O ⁗ BF3 in both the solid and solution states is rapid at room temperature, but 18-crown-6 ⁗ H2O ⁗ BF3,1, is stable to its melting point, 72°C.1 crystallizes in the monoclinic space groupC2/c witha = 27.273(9),b = 8.432(5),c = 22.936(9) Å, β = 128.33(4)°, andD c = 1.27 g cm−3 forZ = 8. Least-squares refinement based on 1409 observed reflections led to a finalR = 0.083. The BF3 is covalently bonded to the oxygen atom of the water molecule which in turn is hydrogen bonded to the 18-crown-6.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01041648
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  • 171
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    Molecular structures of complexes of rare-earth metals with benzo-12-crown-4 (1991)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 10 (1991), S. 191-202 
    Details
    ISSN: 1573-1111
    Keywords: Crown ethers ; rare-earth metals ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An X-ray diffraction study of the complexes [Nd(N03)3(Bl2C4)] (I), [La(NO3)3(Bl2C4)(H2O)]·MeCN (II), and [Er(NO3)3(H2O)3]·2(Bl2C4)·MeCN (III), (B12C4 = benzo-12-crown-4) has been carried out. Crystals ofI are monoclinic,a = 8.050(2),b = 29.92(1),c = 7.741(2) Å,β = 102.71(2)°, space groupP21/c,Z = 4,R = 0.047 for 4718 reflections. Crystals of II are triclinic,a = 8.211(2),b = 10.613(3),c = 12.837(4)Å,a = 94.46(3),β = 108.19(2), γ = 89.98(3)°, space groupPT,Z = 2,R = 0.037 for 5611 reflections. Crystals ofIII are monoclinic,a = 9.847(3),b = 17.201(4),c = 21.664(5)Å,β = 100.85(2)°, space groupP21/n,Z = 4,R = 0.040 for 8328 reflections. The chemical structures of the complexes have been elucidated. The correlation between the radius of a particular lanthanide-ion and its coordination number (10 inI, 11 inII and 9 inIII) and consequently its influence on the composition of the complex is discussed. The possibilities of conformational changes in the B12C4 molecule depending on the type and size of the coordinated moiety (ions Nd(III) and La(III) inI andII and the H2O molecule inIII) are considered.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01066203
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  • 172
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    Chirality of isomers of aldosterone formed in dilute alkali (1991)
    New York, NY [u.a.] : Wiley-Blackwell
    Chirality 3 (1991), S. 71-75 
    Details
    ISSN: 0899-0042
    Keywords: crystal structure ; aldosterone conformation ; correction of assigned configuration ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the presence of dilute alkali at room temperature aldosterone undergoes rearrangement to form 11β,18:18,21-diepoxy-20,21-dihydroxy-4-pregnen-3-one (V). X-Ray crystallographic analysis demonstrates that isomers of both 18R, 20S, 21S and 18R, 20S, 21R configuration are formed rather than the 18R, 20R, 21R isomer postulated on the basis of examination of 1H-NMR spectra. The spectra appears to be consistent with the major component of the mixture. The 20S configuration observed is in agreement with the chirality assigned to the degradation product obtained when the same alkaline solution of aldosterone is subjected to reflux. The crystals of (V) are monoclinic P21, Z = 4 with a = 20.891(2), b = 6.3848(5), c = 16.067(2)Å, β = 122.09°(1) with two molecules in the asymmetric unit. Molecule A has the 20S,21S configuration and the molecules in the second site are a mixture of the 20S, 21S and 20S, 21R configuration in the ratio of 3:2.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chir.530030112
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  • 173
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    [t-Bu2P]3P7 und (t-Bu2Sb)3P7 sowie Untersuchungen zur Bildung von Heptaphosphanen(3) mit PMe2-, PF2- und P(CF3)2-GruppenFrau Professor Marianne Baudler zum 70. Geburtstage am 27. April 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 594 (1991), S. 36-46 
    Details
    ISSN: 0044-2313
    Keywords: Tris(di-tert-butylphospha)heptaphosphanortricyclane, (t-Bu2P)3P7 ; Tris(di-tert-butylstiba)heptaphosphanortricyclane, (t-Bu2Sb)3P7 ; syntheses ; crystal structure ; 31{1H} n.m.r. data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [t-Bu2P]3P7 and (t-Bu2Sb)3P7, as well as Investigations on the Formation of Heptaphosphanes (3) Containing PMe2, PF2, and P(CF3)2 GroupsTris(di-tert-butylphospha)heptaphosphanortricyclane (t-Bu2P)3P7 1 obtained by reacting Li3P7 · 3 DME with t-Bu2PF forms yellow crystals. (t-Bu2Sb)3P7 2 produced similarly from t-Bu2SbCl and Li3P7 · 3 DME didn't form crystals; it decomposes in a solution of toluene above -10°C. Both compounds were identified by their 31P{1H} NMR spectra, and 1 also by elemental analysis and single crystal structure determination (space group) P21/a, a = 1 712.0(9) pm, b = 1 105.1(7) pm, c = 1 854.0(10) pm, β = 94.96(4)°, Z = 4 formula units in the elementary cell).Attempts to synthesize (Me2P)3P7 3, (F2P)3P7 4 and [(F3C)2P]3P7 5 failed as dialkylchlorophosphanes as Me2PCl e. g. with Li3P7 · 3 DME react under Li/Cl exchange, dialkylfluorophosphanes (except t-Bu2PF) disproportionate, and neither PF3 nor (F3C)2PBr with Li3P7 · 3 DME give the desired products 4 or 5, resp.
    Notes: Tris(di-tert-butyl-phospha)-heptaphosphanortricyclan (t-Bu2P)3P7 1 entsteht durch Umsetzung von Li3P7 · 3 DME mit t-Bu2PF und bildet gelbe Kristalle. Das analog aus t-Bu2SbCl und Li3P7 · 3 DME gebildete (t-Bu2Sb)3P7 2 wurde nicht kristallin erhalten. Es zersetzt sich in Lösung (Toluol) oberhalb -10°C. Der Nachweis von 2 erfolgt über das 31P{1H}-NMR-Spektrum, der von 1 anhand des 31P{1H}-NMR-Spektrums, der Analyse und der Kristallstrukturbestimmung. 1 kristallisiert in der Raumgruppe P21/a mit Z = 4 Formeleinheiten; a = 1 712,0(9) pm, b = 1 105,1(7) pm, c = 1 854,0(10) pm, β = 94,96(4)°.Untersuchungen zur Bildung von (Me2P)3P7 3, (F2P)3P7 4, [(F3C)2P]3P7 5 führten nicht zum Ziel, weil Dialkylchlorphosphane wie Me2PCl (zur Bildung von 3) mit Li3P7 · 3 DME unter Li/Cl-Austausch reagieren, Dialkylfluorphosphane (ausgenommen t-Bu2PF) disproportionieren und PF3 sowie (F3C)2PBr mit Li3P7 · 3 DME nicht zu den Verbindungen 4 und 5 führen.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915940105
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    Ternäre intermetallische Phasen des Lithiums mit Elementen der 4. Neben- und 5. Hauptgruppe mit statistischer Metallverteilung im „Kationen“-TeilgitterProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 33-39 
    Details
    ISSN: 0044-2313
    Keywords: Intermetallic phases (ternary) ; lithium ; 4A metals ; 5B elements ; preparation ; crystal structure ; X-ray ; neutron scattering ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Intermetallic Phases of Lithium, Transition Metals of the 4th Group and Elements of the 5th Maingroup with Statistical Metal Distribution in the „Cation“-SubstructureThe results of X-ray investigations and neutron diffraction on new and in some cases already known [1, 2] ternary intermetallic phases of Lithium with transition metals of the 4th group (b) and those of the 5th main group (X = P, As, Sb, Bi) will be reported. They crystallize in a partly „filled“ antifluorite type structure with a statistical Li/B-distribution in the tetrahedral sites. The structures are obviously stabilized by small amounts of enclosed d-elements.
    Notes: Es wird über Röntgenstrukturuntersuchungen und Neutronenbeugung an neuen und einigen schon bekannten [1, 2] ternären intermetallischen Phasen des Lithiums mit Elementen der 4. Nebengruppe (B) und Elementen der 5. Hauptgruppe (X = P, As, Sb, Bi) berichtet. Sie kristallisieren in einer teilweise „aufgefüllten“ Antifluorit-Struktur mit statistischer Li/B-Besetzung der Tetraederlücken, die offenbar durch den Einbau von geringen Mengen der Übergangsmetalle stabilisiert wird.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915970106
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  • 175
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    Synthese, Struktur und Eigenschaften der neuen Bromoselenate(II) [Se3Br8]2-, [Se4Br14]2- und [Se5Br12]2- Kristallstrukturen von [Cu(i-PropCN)4]2[Se3Br8], [EtPh3P]2[Se4Br14] und [n-Prop4N]2[Se5Br12]Professor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 115-132 
    Details
    ISSN: 0044-2313
    Keywords: Selenium ; bromoselenates(II) ; preparation ; crystal structure ; FIR spectra ; Raman spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Properties of the Novel Bromoselenates(II) [Se3Br8]2-, [Se4Br14]2-, and [Se5Br12]2-. Crystal Structures of [Cu(i-PropCN)4]2[Se3Br8], [EtPh3P]2[Se4Br14], and [n-Prop4N]2[Se5Br12]Using the symproportionation of elemental selenium and selenium tetrabromide in polar aprotic solvents a new class of tri-, tetra-, and pentanuclear bromoselenates(II) was obtained. In 2-methylpropionitrile solution the novel ion [Se3Br8]2- was stabilized and isolated as its black solvated copper salt. The crystals of [Cu(i-PropCN)4]2[Se3Br8] are monoclinic (C 2/c, a = 20.753(6), b = 13.344(4), c = 19.149(6) Å, β = 90.09(3)° at 140K, Z = 4) and contain trigonal star-shaped ions [Se3Br8]2- consisting of three edge-sharing square planar SeBr4 units. The mean terminal and μ3-bridging Se—Br bond lengths are 2.408 Å, respectively. [EtPh3P]2[Se4Br14] was obtained from dichloromethane solutions as dark red square-shaped crystals. The X-ray structure analysis (space group P 21/n, a = 11.400(3), b = 11.815(3), c = 20.720(A) Å, β = 92.50(3)° at 140 K, Z = 2) shows the crystals to contain tetranuclear ions [Se4Br14]2- that are built of two parallel planar [Se2Br6] units connected via two linear μBr-bridges. In the interesting delocalized electronic system a formal oxidation number of +1 has to be assigned to the bridging bromine. The mean terminal Se—Br bond length is 2.411 Å, the bridging bond lengths are 2.764 Å in the planar Se2Br6 units 2.594 Å in the linear Se—Br—Se bridges. Dark red [n-Prop4N]2[Se5Br12] was also isolated from CH2Cl2 solutions. It crystallizes in the tetragonal space group P 42/mnm (a = 14.798(3), c = 11.69(2) Å at 140 K, Z = 2) and its structure shows the novel pentanuclear ion [se5Br12]2-, consisting of a central square planar SeBr4 unit with two of its trans-edges being shared with additional pairs of square planar SeBr4, units. The anion can be described as two star-like Se3Br8 fragments with one sharing Se. The mean terminal and μ3-bridging Se—Br bond lengths are 2.343 Å and 2.956 Å, respectively. The vibrational spectra of the novel anions are reported and discussed.
    Notes: Durch Symproportionierung von elementarem Selen und Selentetrabromid in polaren protischen Lösungsmitteln wurde eine neue Klasse tri-, tetra- und pentanuklearer Bromoselenate(II) dargestellt. In 2-Methylpropionitril als Lösungsmittel wurde das strukturell neuartige Ion [Se3Br8]2- stabilisiert und als schwarzes solvatisiertes Kupfersalz isoliert. Kristalle von [Cu(i-PropCN)4]2[Se3Br8] sind monoklin (C2/c, a = 20,753(6), b = 13,344(4), c = 19,149(6) Å, β = 90,09(3)° bei 140K, Z = 4) und enthalten trigonale sternförmige Ionen [Se3Br8]2-, die aus drei kantenverknüpften quadratisch-planaren SeBr4-Einheiten bestehen. Die mittleren endständigen und μ3-verbrückenden Se—Br-Bindungslängen betragen 2,408 Å und 2,911 Å. [EtPh3P]2[Se4Br14] wurde aus Lösungen in Dichlormethan in Form dunkelroter Kristalle erhalten. Wie die Röntgenstrukturanalyse zeigt (Raumgruppe P21/n, a = 11,400(3), b = 11,815(3), c = 20,720(7) Å, β = 92,50(3)° bei 140K, Z = 2), enthalten sie vierkernige Ionen [Se4Br14]2-, die aus zwei parallel angeordneten, über lineare μBr-Brücken verknüpften Se2Br6-Einheiten aufgebaut sind. In diesem bemerkenswerten delokalisierten Elektronensystem muβ für das verbrückende Brom die formale Oxidationszahl + 1 angenommen werden. Die mittlere Se—Brterm-Bindungslängen sind 2,411 Å, die Brückenbindungslängen 2,764 Å in den planaren Se2Br6-Einheiten sowie 2,594 Å in den linearen Se—Br—Se-Brücken. Dunkelrotes [n-Prop4N]2[Se5Br12] konnte ebenfalls aus Lösungen in CH2Cl2 dargestellt werden. Es kristallisiert tetragonal (Raumgruppe P42/mnm, a = 14,798(3), c = 11,169(2) Å bei 140K, Z = 2). Seine Struktur enthält neuartige molekulare Ionen [Se5Br12]2-, die aus einer zentralen quadratisch-planaren SeBr4-Einheit bestehen, die über zwei trans-Kanten mit jeweils zwei weiteren quadratisch-planaren SeBr4-Einheiten verknüpft ist. Das Anion kann als über ein Selenatom verknüpfte Anordnung zweier sternförmiger Se3Br8-Fragmente beschrieben werden. Die mittleren endständigen und μ3-verbrückenden Se—Br-Abstände sind 2,343 Å und 2,956 Å. Über schwingungsspektroskopische Untersuchungen der neuen Anionen wird berichtet.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915970115
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    Kristallstruktur von gelbem K3OBrProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 197-200 
    Details
    ISSN: 0044-2313
    Keywords: Tripotassium bromide oxide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Yellow K3OBrK3OBr was prepared for the first time and investigated by X-ray methods. The yellow compound crystallizes with cubic symmetry, space group Pm3m, a = 521.3(1) pm, Z = 1 and shows like colourless Na3OCl anti-perovskite structure.
    Notes: K3OBr wurde erstmal dargestellt und an Einkristallen untersucht. Die gelbe Verbindung kristallisiert kubisch, Raumgruppe Pm3m, a = 521,3(1) pm, Z = 1 und weist wie farbloses Na3OCl anti-Perowskitstruktur auf.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915970122
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  • 177
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    Tetraphenylphosphonium-Heptathiacyclo-thioarsenat(III), PPh4[SAsS7]Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 211-215 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium heptathiacyclo thioarsenate(III) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetraphenylphosphonium Heptathiacyclo Thioarsenate(III), PPh4[SAsS7]From PPh4[As2SCl5] und K2S5 the title compound was obtained in acetonitrile among other products. According to an X-ray crystal structure analysis, it crystallizes in the orthorhombic space group Pna21 with a = 1 826.1(3), b = 1 312.0(2), c = 1 215.9(2) pm, Z = 4. The structure consists of PPh4+ and [SAsS7]- ions, AsS7 rings in the crown conformation as in S8 being present.
    Notes: Aus PPh4[As2SCl5] und K2S5 wurde in Acetonitril unter anderem die Titelverbindung erhalten. Nach der Röntgenstrukturanalyse mit 1474 beobachteten Reflexen (R = 7,1%, wR = 2,7%) kristallisiert sie rhombisch in der Raumgruppe Pna21; a = 1 826,1(3), b = 1 312,0(2), c = 1 215,9(2) pm, Z = 4. Die Struktur besteht aus PPh4+-und [SasS7]-Ionen, wobei AsS7-Ringe in der Kronenform wie beim S8 vorliegen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915950120
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  • 178
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    Die Kristallstruktur von 2CaCl2 · 11HgCl2 · 16H2O, eines kubischen, quecksilberreichen Chloromercurats mit ikosaedrischen Hg6Cl13- und Hg5Cl13-BaugruppenProfessor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 193-202 
    Details
    ISSN: 0044-2313
    Keywords: Bis(octaaquocalcium)-tridecachlorohexamercurate-tridecachloropentamercurate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of 2CaCl2 · 11HgCl2 · 16H2O, a Cubic Mercury-rich Chloromercurate with Icosahedral Hg6Cl13 and Hg5Cl13 GroupsThe mercury-rich chloromercurate 2CaCl2 · 11HgCl2 · 16H2O has been obtained by crystallization from concentrated aqueous solutions of CaCl2 and HgCl2 at room temperature. In the cubic crystal structure (a = 18.170(3) Å, space group F23, Z = 4) a three-dimensional framework is formed by Hg6Cl13- and Hg5Cl133- anions with large cavities, in which the dodecahedral Ca(H2O)82+ cations are accomodated. 96 out of 104 Cl atoms in the cell form a lattice complex cP2[12i] with 8 Cl12 icosahedra, which are centered by Cl atoms. In four of these Hg atoms are situated on 6 edges thus forming Cl(HgCl2)6- anions, while the remaining four icosahedra hold 3 Hg atoms on edges and two on faces. Here the central Cl- anions are coordinated by 3 HgCl2 and 2 HgCl3 groups. The Hg5Cl13 and Ca(H2O)8 polyhedra are crystallographically disordered.
    Notes: Das quecksilberreiche Chloromercurat 2CaCl2 · 11HgCl2 · 16H2O ist durch Kristallisation aus konzentrierten wäßrigen Lösungen von CaCl2 und HgCl2 bei Raumtemperatur zu erhalten. In der kubischen Kristallstruktur (a = 18,170(3) Å, Raumgr. F23, Z = 4) bilden Hg6Cl13-- und Hg5Cl133--Anionen ein Gerüst mit großen Hohlräumen, in denen sich Ca(H2O)82+-Kationen mit dodekaedrischer Konformation befinden. Von den 104 Cl-Atomen in der Zelle bilden 96 einen Bauverband cP2[12i] mit acht Cl12-Ikosaedern, die jeweils durch ein Cl-Atom zentriert sind. Bei vier der Ikosaeder befinden sich 6 Hg-Atome auf Kanten, so daß Cl(HgCl2)6--Anionen resultieren. Bei den Hg5Cl133--Anionen besetzen jeweils 3 Hg-Atome Kanten und 2 Hg-Atome Flächen der Ikosaeder, so daß die zentralen Cl--Anionen von 3 HgCl2- und 2 HgCl3-Gruppen koordiniert sind. Die Hg5Cl13- und Ca(H2O)8-Baugruppen sind kristallographisch fehlgeordnet.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915950118
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  • 179
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    K4BeP2, K4BeAs2 und K4BeSb2-Verbindungen mit linearen [BeX2]4-. Anionen (X = P, As, Sb)Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 217-223 
    Details
    ISSN: 0044-2313
    Keywords: Tetrapotassium biphosphidoberyllate, -biarsenidoberyllate, -biantimonidoberyllate ; crystal structure ; vibrational spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: K4BeP2, K4BeAs2, and K4BeSb2 Compounds with Linear [BeX2]4- Anions (X = P, As, Sb)The title compounds are synthesized from the elements. K4BeP2 and K4BeAs2 are isostructural and crystallize trigonal rhombohedrally in the space group R3m (No. 166) with Z = 3. The partial structure of the potassium atoms corresponds to a closest packing of rotational ellipsoides, which envelope an elongated K14-polyhedron (combination of rhombohedron and hexagonal prism). The polyhedrons are filled with linear [BeX2]4- anions, which are the analoga to BeCl2 molecules. The bond lengths are: d(Be—P) = 198.2 pm and d(Be—As) = 206.0 pm. IR spectra confirm the presence of [Sb—Be—Sb]4- anionic groups in K4BeSb2, which crystallizes in the hexagonal system with Z = 2. The vibrational spectra of the compounds are measured. The assignment of the observed frequencies is based on the D∞h symmetry of an isolated [X—Be—X]4- unit.
    Notes: Die Titelverbindungen wurden aus den Elementen dargestellt. K4BeP2 und K4BeAs2 sind isotyp und kristallisieren trigonal-rhomboedrisch in der Raumgruppe R3m (Nr. 166) mit Z = 3. Die Teilstruktur der Kaliumatome entspricht einer dichtesten Packung von Rotationsellipsoiden, welche ein gestrecktes K14-Polyeder (Kombination von Rhomboeder und hexagonalem Prisma) einhüllen. Die Polyeder sind durch lineare [BeX2]4--Anionen aufgefüllt, Analoga des BeCl2-Moleküls. Die Bindungslängen sind d(Be—P) = 198,2 qm und d(Be—As) = 206,0 pm. IR-Spektren belegen die Existenz von [Sb—Be—Sb]4--Anionen auch in K4BeSb2, welches im hexagonalen System mit Z = 2 kristallisiert. Die Schwingungsspektren der Verbindungen wurden gemessen. Die Zuordnung der beobachteten Frequenzen basiert auf der D∞h-Symmetrie einer isolierten [X—Be—X]4--Einheit.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915950121
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  • 180
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    Synthese und Struktur der Platin(O)-Verbindungen [(dipb)Pt]2(COD) und (dipb)3Pt2 sowie des clusters Hg6[Pt(dipb)]4 (dipb = (i-Pr)2P(CH2)4P(i-Pr)2)Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 595 (1991), S. 239-250 
    Details
    ISSN: 0044-2313
    Keywords: Platinum(0) compounds ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of the Platinum(0) Compounds [(dipb)Pt]2(COD) and (dipb)3Pt2 and of the Cluster Hg6[Pt(dipb)]4 (dipb = (i-Pr)2P(CH2)4P(i-Pr)2)The reduction of (dipb)PtCl2 with Na/Hg yields (dipb)Pt as an intermediate which reacts with the amalgam to form the cluster Hg6[Pt(dipb)]4 (3) or decomposes to (dipb)3Pt2 (2) and Pt. In the presence of COD [(dipb)Pt]2(COD) (1) is obtained. 1 crystallizes monoclinicly in the space group P21/c with a = 1596.1(4), b = 996.5(2), c = 1550.4(3) pm, β = 113.65(2)°, Z = 2. In the dinuclear complex two (dipb)Pt units are bridged by a 1,2-η2-5,6-η2 bonded COD ligand. Whereby the C = C double bonds are lengthened to 145 pm. 2 forms triclinic crystals with the space group P1 and a = 1002.0(2), b = 1635.9(3), c = 868.2(2) pm, α = 94.70(2)°, β = 94.45(2)°, σ = 87.95(1)°, Z = 1. In 2 two (dipb)Pt moieties are connected by a μ-dipb ligand in a centrosymmetrical arrangement. 3 is monoclinic with the space group C2/c and a = 1273.8(3), b = 4869.2(6), c = 1660.2(3) pm, β = 95.16(2)°, Z = 4. The clusters Hg6[Pt(dipb)]4 have the symmetry C2. Central unit is a Hg6 octahedron of which four faces are occupied by Pt(dipb) groups. The bonding in the cluster is discussed on the basis of eight Pt—Hg two center bonds of 267.6 pm and two Pt—Hg—Pt three center bonds with Pt—Hg = 288.0 pm.
    Notes: Bei der Reduktion von (dipb)PtCl2 mit Na/Hg entsteht intermediär (dipb)Pt, das mit dem Amalgam den Cluster Hg6[Pt(dipb)]4 (3) bildet oder sich zu (dipb)3Pt2 (2) und Pt zersetzt. Bei Anwesenheit von COD entsteht [(dipb)Pt]2(COD) (1). 1 kristallisiert monoklin in der Raumgruppe P21/c mit a = 1596,1(4), b = 996,5(2), c = 1550,4(3) pm, β = 113,65(2)°, Z = 2. Im zentrosymmetrischen Zweikernkomplex sind zwei (dipb)Pt-Einheiten über das 1,2-η2-5,6-η2-gebundene COD verbrückt. Die C = C-Doppelbindungen werden dabei auf 145 pm aufgeweitet. 2 bildet trikline Kristalle mit der Raumgruppe P1 und a = 1002,0(2), b = 1635,9(3), c = 868,2(2) pm, α = 94,70(2)°, β = 94,45(2)°, σ = 87,95(1)°, Z = 1. In 2 überbrückt ein μ-dipb-Ligand zwei (dipb)Pt-Gruppen in zentrosymmetrischer Anordnung. Monoklines 3 mit der Raumgruppe C2/c und a = 1273,8(3), b = 4869,2(6), c = 1660,2(3) pm, β = 95,16(2)°, Z = 4 ist aus Hg6[Pt(dipb)]4-Clustern mit der Symmetrie C2 aufgebaut. Zentrale Einheit des Clusters ist ein Hg6-Oktaeder, bei dem vier Flächen von (dipb)Pt-Gruppen besetzt sind. Die Bindungsverhältnisse werden auf der Grundlage von acht Pt—Hg-Zweizentrenbindungen mit Pt—Hg = 267,6 pm und zwei Pt—Hg—Pt-Dreizentrenbindungen mit Pt—Hg = 288,0 pm diskutiert.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915950123
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    Synthese und Kristallstruktur von Quecksilber(II)-N,N′-bis(trimethylsilyl)benzamidinat, Hg[Ph—C(NSiMe3)2]2 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 47-53 
    Details
    ISSN: 0044-2313
    Keywords: Mercury-N,N′-bis(trimethylsilyl)benzamidinate ; synthesis ; i.r. spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Mercury(II)-N,N′-bis(trimethylsilyl)benzamidinate, Hg[Ph—C(NSiMe3)2]2The title compound has been synthesized by the reaction of N,N,N′-tris(trimethylsilyl)benzamidine with mercury(I)-acetate in boiling acetonitrile because of redox disproportionation, forming white crystal needles, which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P1; Z = 2; 6846 observed unique reflections; R = 0.048. Lattice dimensions at -90 ° C: a = 1091.9, b = 1212.8, c = 1433.5 pm; α = 106.89°, β = 109.25°, γ = 90.62°. The compound forms a nearly centro-symmetric molecule structure with sp-hybridized Hg atom (r Hg—N = 207 pm).
    Notes: Die Titelverbindung entsteht bei der Reaktion von N,N,N′-tris(trimethylsilyl)-benzamidin mit Quecksilber(I)-acetat in siedendem Acetonitril durch Redox-Disproportionierung in Form weißer Kristallnadeln, die durch das IR-Spektrum und durch eine röntgenographische Kristallstrukturanalyse charakterisiert werden. Raumgruppe P1, Z = 2, 6 846 beobachtete unabhängige Reflexe; R = 4, 8%. Gitterabmessungen bei -90 °C: a = 1091,9; b = 1212,8; c = 1433,5 pm; α = 106,89α β = 109,25°; γ = 90,62°. Die Verbindung bildet eine nahezu zentrosymmetrische Molekülstruktur mit sp-hybridisiertem Hg-Atom (r Hg—N = 207 pm).
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960107
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  • 182
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    Die Antimonid-Triantimonidometallate(III) Cs6K3Sb[AlSb3] und Cs6K3Sb[GaSb3]Professor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 201-208 
    Details
    ISSN: 0044-2313
    Keywords: Antimonide triantimonidometallates(III) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Antimonide Triantimonidometallates(III) Cs6K3Sb[AlSb3] and Cs6K3Sb[GaSb3]The novel compounds Cs6K3Sb[AlSb3] and Cs6K3Sb[GaSb3] are formed from stoichiometric mixtures of Cs, AlSb (GaSb) and KSb in sealed niobium ampoules at 950 K. The hexagonal structures are especially characterized by one-dimensional rod packings 1∞[Cs6K3Sb] which are formed from columns of condensed (Cs6K6/2) icosahedra. The icosahedra are centered by Sb3-- anions. The trigonal planar anions [AlSb3]6-- and [GaSb3]6-- are embedded between the icosahedra columns, and they are coordinated by alkali metal atoms. The FIR spectra were assigned to the vibrations of the [MSb3]6-- anions, with respect to the 6m2-D3h symmetry.(P63/mmc, No. 194; a = 1101.7 and 1097.2 pm; c = 1158.9 and 1150.1 pm; Z = 2; Single crystal data: 574 and 546 reflections; R = 0.073 and 0.029. Distances:d(Al—Sb) = 265.4 pm; d(Ga—Sb) = 265.1 pm; d(Sb—Cs) = 401.6-423.0 pm; d(Sb—K) = 358.6-367.3 pm).
    Notes: Die neuen Verbindungen Cs6K3Sb[AlSb3] und Cs6K3Sb[GaSb3] entstehen aus stöchiometrischen Gemischen von Cs, AlSb (GaSb) und KSb in verschweißten Niob-Ampullen bei 950 K. Besonderes Merkmal der hexagonalen Strukturen sind eindimensionale Stabpackungen 1∞[Cs6K3Sb], gebildet aus Säulen kondensierter (Cs6K6/2)-Ikosaeder. Die Ikosaeder sind von Sb3---Anionen zentriert. Zwischen den Ikosaedersäulen sind die trigonal-planaren Anionen [AlSb3]6-- bzw. [GaSb3]6-- eingebettet. Sie werden durch die Alkalimetallatome koordiniert. Die FIR-Spektren können den Schwingungen der Anionen [MSb3]6-- mit der Symmetrie 6m2-D3h zugeordnet werden.(P63/mmc, Nr. 194; a = 1101,7 bzw. 1097,2 pm; c = 1158,9 bzw. 1150,1 pm; Z = 2; Einkristalldaten: 574 bzw. 546 Reflexe; R = 0,073 bzw. 0,029. Abstände: d(Al—Sb) = 265,4 pm; d(Ga—Sb) = 265,1 pm; d(Sb—Cs) = 401,6-423,0 pm; d(Sb—K) = 358,6-367,3 pm).
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915970123
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  • 183
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    Zur Kenntnis von (Ba0,5Sr0,5)Cu2V2O8 und Ba(CuMg)V2O8 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 149-154 
    Details
    ISSN: 0044-2313
    Keywords: Alkaline earth ; copper ; vanadium ; oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On (Ba0,5Sr0,5)Cu2V2O8 and Ba(CuMg)V2O8Single Crystals of (A): (Ba0.5Sr0.5)Cu2V2O8 and (B) Ba(CuMg)V2O8 were prepared by solid state reactions below the melting points of the starting mixtures. Both compounds were examined by X-ray technique. They crystallize in the space groups (A): 142d [No. 122]; a = 12.65; c = 8.18 Å; Z = 8; and (B): 141/acd [No. 142]; a = 12.50; c = 8.33 Å; Z = 8. In (A) are Ba2+ plus Sr2+ and in (B) are Cu2+ plus Mg2+ in statistical distribution. The square pyramidal Cu2+ coordination in (A) is changed to an octahedron in (B), by replacing Cu2+ by Mg2+.
    Notes: Einkristalle von (A): (Ba0,5Sr0,5)Cu2V2O8 und (B): Ba(CuMg)V2O8 wurden durch Feststoffreaktionen dicht unterhalb des Schmelzpunktes der jeweiligen Reaktionsgemenge erhalten. Zellparameter und Atompositionen wurden röntgenographisch bestimmt. Die Verbindungen kristallisieren in den Raumgruppen (A): 142d, [Nr. 122] mit a = 12,65; c = 8,18 Å; Z = 8; (B): 141/acd; [Nr. 142] mit a = 12,50; c = 8,33 Å; Z = 8. In (A) sind Ba2+ und Sr2+, in (B) Cu2+ und Mg2+ statistisch verteilt. Die tetragonal pyramidale Koordination von Cu2+ in (A) ändert sich durch den Einbau von. Mg2+ in (B) in eine gestreckt oktaedrische.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916020116
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  • 184
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    Zinc and cadmium adducts of 2,2′-Bis(pyrazol-1-yl) propane,(L—L), a sterically hindering ligand. Crystal structure of (L—L)Zn[OC(=O)CF3]2(H2O) (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 169-177 
    Details
    ISSN: 0044-2313
    Keywords: Zinc ; Cadmium ; 2,2′-bis(pyrazol-1-yl)propane ; adduct complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zink- und Cadmium-Addukte des 2,2′-Bis(pyrazol-1-yl)propan, (L—L), einem sterisch anspruchsvollen Liganden. Kristallstruktur des (L—L)Zn[OC(=O)CF3]2(H2O)1:1 Addukte zwischen dem Titelliganden und MX2 (M = Zn oder Cd; X = Cl, Br, I oder C2F3O2) bzw. den ionischen Verbindungen [(L—L)5Zn2(H2O)2](ClO4) 4 und [(L—L)2 Cd(H2O)2](ClO4)2 wurden dargestellt. Diese sind stabil im festen Zustand und in Aceton-Lösung, nicht jedoch in Dimethylsulfoxid-Lösung. In der Struktur des (L—L)Zn(H2O)[O—C(=O)CF3]2 liegt, auf Grund einer durch die Methylgruppen verursachten sterischen Behinderung, eine verzerrte trigonale Bipyramide vor, in der zwei Sauerstoffatome (vom Wasser und Trifluoroacetat) und ein Stickstoffatom in der äquatorialen Ebene liegen. Die axialen Zn—X-Bindungen (X = N = 2,125(3) Å; X = O = 2,085(4) Å) sind länger als die äquatorialen.
    Notes: 1:1 adducts between the title ligand and MX2 (M = Zn or Cd; X = Cl, Br, I or trifluoroacetate) as well as ionic compounds [(L—L)5Zn2(H2O)2](ClO4) 4 and [(L—L)2Cd(H2O)2](ClO4) 2 are stable in the solid state and in acetone solution, but not in dimethylsulphoxide. In (L—L)Zn(H2O)[O—C(=O)CF3]2 two oxygen atoms (belonging to water and to one O—C(=O)CF3) at 2.039(4) and 2.008(4) Å from Zn, and one nitrogen atom (Zn—N 2.067(3) Å) from the chelating L—L define the basal plane of a trigonal bipyramid, which is distorted owing to the steric requirements of the bridgehead methyls of L—L; the axial Zn—X bonds (X = N 2.125(3) Å; X = O 2.085(4) Å), are longer than the equatorial Zn—X bonds.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916020118
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    Preparation and crystal structure of Nb6.74 Ta5.26S4 - a new compound in the ternary system Ta—Nb—SDedicated to Professor Hans-Georg von Schnering on his 60th Birthday (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 353-362 
    Details
    ISSN: 0044-2313
    Keywords: Niobium tantalum sulfide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur von Nb6,74Ta5,26S4 - einer neuen Verbindung im ternären System Ta—Nb—SNb6,74Ta5,26S4 ist mittels Hochtemperaturtechnik dargestellt worden. Die Kristallstruktur wurde aus Einkristall-Röntgenbeugungsdaten bestimmt (R/Rw = 0,0588/0,0655). Die Verbindung kristallisiert orthorhombisch, Raumgruppe Pnma mit a = 959,11 (26), b = 336,37 (10) und c = 3282,51 (74) pm, Z = 4. Die Struktur entspricht eher der von Nb-reichen als der von Ta-reichen Sulfiden. Die Metall-Koordinationen sind bekappte, verzerrte kubische Prismen und pentagonale Prismen während die Schwefelkoordinationen bekappte trigonale Prismen sind.
    Notes: Nb6.74Ta5.26S4 has been prepared by high temperature techniques. The crystal structure has been determined from single crystal X-ray diffraction data (R/Rw = 0.0588/0.0655). The compound crystallizes in the orthorhombic space group Pnma with unit cell dimensions a = 959.11 (26) pm, b = 336.37 (10) pm, and c = 3282.51 (74) pm. The orthorhombic cell contains four formula units. Its structure is similar to that of Nb-rich sulfides, rather than to that of Ta-rich sulfides. The metal coordinations are capped distorted cubic prisms and pentagonal prisms while the coordinations of sulfur are capped trigonal prisms.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915980132
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    Hydrate schwacher und starker Basen. V. Die Kristallstrukturen von KOH · 2H2O (Substruktur) und KOH · 4H2OProfessor Wilhelm Kuchen zum 65. Geburtstage am 27. Mai 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 601 (1991), S. 73-82 
    Details
    ISSN: 0044-2313
    Keywords: Potassium hydroxide dihydrate ; tetrahydrate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrates of Weak and Strong Bases. V. Crystal Structures of KOH · 2H2O (Substructure) and KOH · 4H2OIn the context of studies on formation and structure of base hydrates the crystal structures of KOH · 2H2O and KOH · 4H2O have been determined. For both structures, Mokα diffractometer data were used, obtained at -150°C, which allowed also the complete set of H atoms to be localized and refined. The dihydrate, melting incongruently at 33°C, crystallizes with a superstructure. The substructure, which is reported here, is tetragonal with space group I41/amd and Z = 8 formula units per unit cell of dimensions a = 7.154 and c = 13.415 Å. With 462 independent observed reflections an R value of 0.026 was obtained. K(H2O)8+ cubes via common faces form rods and these in a tetragonal four-layer packing pattern are further linked into a three-dimensional framework. The OH-ions, hydrogen-bonded by the H2O molecules, are located with a twofold disorder in additional cubes of this frame-work, not occupied by K+ ions. The tetrahydrate, melting congruently at -33.7°C, is monoclinic with space group P21/c and Z = 4. The unit cell dimensions are a = 6.951, b = 11.530, c = 7.080 Å and β = 99.19°. With 2198 independent observed reflections the final R value is 0.025. Trigonal K(H2O)6+ prisms across common edges form layers, which are linked with each other via OH- ions and only loosely cation-bonded H2O molecules.
    Notes: Im Rahmen von Untersuchungen zu Bildung und Struktur von Basehydraten wurden die Kristallstrukturen von KOH · 2H2O und KOH · 4H2O bestimmt. Benutzt wurden hierzu bei -150°C mit Mokα-Strahlung erhaltene Diffraktometerdaten, mit denen auch sämtliche H-Atome lokalisiert und verfeinert werden konnten. Das bei 33°C inkongruent schmelzende Dihydrat kristallisiert mit einer Überstruktur. Die Substruktur, über die hier berichtet wird, ist tetragonal mit der Raumgruppe 141/amd und Z = 8 Formeleinheiten pro Elementarzelle sowie den Gitterkonstanten a = 7,154 und c = 13,415 Å. Mit 462 unabhängigen beobachteten Reflexen wurde ein R-Wert von 0,026 erreicht. K(H2O)8+ -Würfel bilden über gemeinsame Flächen Stäbe und durch weitere Verknüpfung ein nach dem Muster einer tetragonalen Vierschichtpackung aufgebautes dreidimensionales Gerüst. Die OH- -Ionen befinden sich, durch Wasserstoffbrücken von den H2O-Molekülen gebunden, mit zweifacher Fehlordnung in weiteren, nicht mit K+ -Ionen besetzten Würfeln dieses Gerüsts. Das bei -33,7°C kongruent schmelzende Tetrahydrat ist monoklin mit der Raumgruppe P21/c und Z = 4. Die Gitterkonstanten betragen a = 6,951, b = 11,530, c = 7,080 Å und β = 99,19°. Mit 2198 unabhängigen beobachteten Reflexen liegt der abschließende R-Wert bei 0,025. Trigonale K(H2O)6+ -Prismen bilden über gemeinsame Kanten Schichten, die durch Wasserstoffbrücken über OH- -Ionen und nur locker an die Kationen gebundene H2O-Moleküle miteinander verbunden sind.
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    URL: http://dx.doi.org/10.1002/zaac.19916010109
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    Synthese und Kristallstrukturen der Alkali-Tetraiodoindate(III), Alnl4 (A = Li, K, Rb, Cs)Professor Klaus Brodersen zum 65. Geburtstage am 12. August 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 31-37 
    Details
    ISSN: 0044-2313
    Keywords: Alkali-iodoindates(III) ; indium ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of the Alkali-tetraiodoindates(III), AInI4 (A = Li, K, Rb, Cs)Single crystals of the yellow alkaliiodoindates(III), AInI4 (A = Li, K, Rb, Cs), are obtained from mixtures of the binary components by slow cooling of the melts. LiInI4 is isotypic with LiAlCl4: monoclinic, P21/c, Z = 4; a = 838.9(4); b = 751.2(3); c = 1526,7(8) pm; β = 92.67(4)°. KInI4 belongs to the ATIX4 type of structure (A = NH4, K, Rb; X = Br, I): cubic, F4 3c, Z = 24; a = 1990.8(1) pm. RbInI4 crystallizes with the β-GaBr2 type: trigonal, R3c, Z = 18; a = 2452.6(6); c = 978.6(4) pm. CsInI4 is isostructural with CsTII4: monoclinic, P21/c, Z = 4; a = 738.4(1); b = 1875.7(3); c = 853.6(2) pm; β = 105.75(2)°. In all structures almost regular tetrahedral polyhedra [InI4]- occur. The coordination numbers of the alkali cations cover the wide range from 6 (Li+) via 9 (Rb+) and 11 (Cs+) to 12 (K1+).
    Notes: Einkristalle der gelben Iodoindate(III) der Alkalimetalle, AInI4 (A = Li, K, Rb, Cs), erhält man aus Gemengen der binären Komponenten durch langsames Abkühlen der Schmelzen. LiInI4 ist isotyp mit LiAlCl4: monoklin, P21/c, Z = 4; a = 838,9(4); b = 751,2(3); c = 1526,7(8) pm; β = 92,67(4)°. KInI4 gehört zum ATIX4-Typ (A= NH4, K, Rb; X= Br, I): kubisch, F4 3c, Z = 24; a = 1990,8(1) pm. RbInI4 kristallisiert im β-Ga[GaBr4]-Typ: trigonal, R3c, Z = 18; a = 2452,6(6); c = 978,6(4) pm. CsInI4 ist isotyp mit CsTII4: monoklin, P21/c, Z = 4; a = 738,4(1); b = 1875,7(3); c = 853,6(2) pm; β = 105,75(2)°. Stets liegen annähernd tetraedrische Baugruppen [InI4]- vor. Die Koordinationszahlen der Alkali-Kationen überstreichen das Spektrum von 6 (Li+) über 9 Rb+, 11 (Cs+) bis 12 (K1+).
    Additional Material: 6 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19916020104
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  • 188
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    Synthese und Kristallstruktur von PbMo5O8; ein reduziertes Oxomolybdat mit Mo10O28-Oktaederdoppeln (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 602 (1991), S. 49-63 
    Details
    ISSN: 0044-2313
    Keywords: Oxomolybdates ; cluster ; crystal structure ; HRTEM ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of PbMo5O8; a reduced Oxomolybdate with Mo10O28 Double OctahedraThe crystal structure of the new phase PbMo5O8 contains oligometric Mo clusters which consist of two edge-sharing Mo6 octahedra connected according to Mo10O6iO4/2i-iO16/2i-a. The compound is isotypic with LaMo5O8. Isolated, divalent Pb atoms are located in the “channels” of the monoclinic structure (a = 999.3(2) pm, b = 924.7(1) pm, c = 753.6(2) pm, β = 109.39(2)°, P21/a. Compared to the compound In 11Mo40O62 the Mo—O distances (average 206 pm) and the Mo—Mo distances within the octahedral units (average 275 pm) are slightly decreased by 1 and 4 pm, respectively. The very short Mo—Mo distances (278 pm) between the cluster units which are not observed in In11Mo40O62 (320 pm) are due to excess electrons in these inter-cluster bonds which would otherwise occupy antibonding cluster states.
    Notes: Mit der neuen Phase PbMo5O8 wurde ein weiteres Beispiel für oligomere Mo-Cluster aus zwei kantenverknüpften Mo6-Oktaedern gefunden, die nach Mo10O6iO4/2i-iO16sol;2i-a verknüpft sind. Die Verbindung ist isotyp zu LaMo5O8. In den „Kanälen“ der monoklinen Struktur a = 999,3(2) pm, b = 924,7(1) pm, c = 753,6(2) pm, β = 109,39(2)°, P21/a) findet man isolierte, zweiwertige Pb-Atome. Gegenüber der Verbindung In11Mo40O62 sind die Mo—O-Abstände mit durchschnittlich 206 pm nur gering um 1 pm und die Mo—Mo-Abstände innerhalb der oktaedrischen Baueinheiten mit durchschnittlich 275 pm ebenfalls nur schwach um 4 pm verkürzt. Allerdings findet man mit 278 pm sehr kurze Mo—Mo-Abstände zwischen den Clustereinheiten, die so nicht bei In11Mo40O62 (320 pm) beobachtet werden können. An diesen inter-Cluster-Bindungen sind überschüssige Elektronen beteiligt, die andernfalls antibindende Clusterzustände besetzen würden.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916020106
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  • 189
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    Über die Kronenetherkomplexe [K(15-Krone-5)2]3[Sb3I12], [TeCl3(15-Krone-5)][TeCl5] und [TeCl3(15-Krone-5)]2[TeCl6] (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 55-61 
    Details
    ISSN: 0044-2313
    Keywords: Crown ether complexes ; tellurium ; antimony ; syntheses ; i.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crown Ether Complexes [K(15-Crown-5)2]3[Sb3I12], [TeCl3(15-Crown-5)][TeCl5], and [TeCl3(15-Crown-5)]2[TeCl6]Orange-coloured crystals of [K(15-crown-5)2]3[Sb3I12] are formed in the reaction of potassium iodide with antimony triiodide and 15-crown-5 in acetonitrile solution. An X-ray structure determination reveals severe disorder of the crown ether molecules, which coordinate to the potassium atoms in a sandwich array; so only the [Sb3I12]3- ion and the potassium positions were ascertained. The anion is a centrosymmetric trimer (symmetry C2h), which can be understood as central SbI63- ion, coordinated by two SbI3 molecules. (Space group C2/m), Z = 2, 3263 observed, independent reflections, R = 0.06, lattice dimensions at 20°C: a = 2541.1 pm, b = 1441.7 pm, c = 1588.4 pm, β = 113.33°.The tellurium complexes [TeCl3(15-crown-5)] [TeCl5] and [TeCl3(15-crown-5)]2[TeCl6] are prepared by reaction of TeCl4 with 15-crown-5 in acetonitrile solution, forming yellow-green crystals sensitive to moisture. They are characterized by their i.r. spectra.
    Notes: Orange Kristalle [K(15-Krone-5)2]3[Sb3I12] entstehen durch Einwirkung von Kaliumiodid auf Antimontriiodid bei Anwesenheit von 15-Krone-5 in Acetonitrillösung. Wegen Fehlordnung der die Kaliumionen sandwichartig koordinierenden Kronenethermoleküle konnten röntgenogrpahisch in der Struktur nur das [Sb3I12]3--Ion sicher aufgeklärt werden. Es bildet ein zentrosymmetrisches Trimer (Symmetrie C2h), das sich als zentrales SbI63--Ion mit zwei koordinierten SbI3-Molekülen auffassen läßt. Raumgruppe C2/m, Z = 2, 3263 unabhängige beobachtete Reflexe, R = 6,2%. Gitterabmessungen bei 20 °C: a = 2541,1; b = 1441,7; c = 1588,4 pm, β = 113,33°.Die Tellurokomplexe [TeCl3(15-Krone-5)] [TeCl5] und [TeCl3(15-Krone-5)]2[TeCl6] entstehen aus TeCl4 und 15-Krone-5 in Acetonitrillösung als gelbgrüne, feuchtigkeitsempfindliche Kristalle, die durch ihre IR-Spektren charakterisiert werden.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960108
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  • 190
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    Über ein Oxidchlorid des Calciums: Ca4OCl6 (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 89-92 
    Details
    ISSN: 0044-2313
    Keywords: Calcium oxychloride ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: An Oxychloride of Calcium: Ca4OCl6Ca4OCl6 (hexagonal, P63mc, Z = 2), a = 905.8(3), c = 686.3(4) pm, (R = 0.031) crystallizes as colourless needles from reducing melts (CaCl2, Ca) that contain small amounts of „oxygen“. It contains „isolated“ tetrahedral units [Ca4O] and is isotypic with e.g., Ba4OCl6, Yb4OCl6 and K6HgS4. Ca4OCl6 does not form in the dehydration process of, for example, CaCl2 · 6 H2O.
    Notes: Ca4OCl6 (hexagonal, P63mc, Z = 2, a = 905.8(3)); c = 686.3(4) pm, (R = 0,031) kristallisiert in Form farbloser Nadeln aus „reduzierenden Schmelzen“ (CaCl2, Ca), die wenig „Sauerstoff“ enthalten. Es enthält „isolierte“ tetraedrische [Ca4O]-Einheiten und ist isotyp mit z. B. Ba4OCl6, Yb4OCl6 oder K6HgS4. Ca4OCl6 entsteht nicht beim Entwässern von z. B. CaCl2 · 6 H2O.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960112
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  • 191
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    Untersuchungen über Polythiocuprate(I) [Cu(Sx)]-. 3. Kristallstruktur von [H3N—C2H4—NH3][Cu(S5)]2 · 4 H2O (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 111-119 
    Details
    ISSN: 0044-2313
    Keywords: Polythiocuprates(I) ; ethylenediammonium bis(pentathiocuprate(I)) tetrahydrate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Polythiocuprates(I) [Cu(Sx)]-. 3. Crystal Structure of [H3N—C2H4—NH3][Cu(S5)]2 · 4 H2OThe title compound crystallizes with Z = 2 in the monoclinic space group P21/c (Nr. 14) with cell dimensions a = 8.820(1) Å, b = 15.532(3) Å, c = 6.999(2) Å and β = 96.92(4)°. For 2368 independent reflections the structure was refined to R = 0.070 and Rw = 0.045.The structure contains endless [Cu(S5)]nn- anion-chains ∥c and is stabilized by hydrogen bonds N—H…S, N—H…O, O—H…S, and O—H…O. Each copper atom is tetrahedrally coordinated by four sulfur atoms from three different (S5)2- chains. There are CuS4 and Cu2S3 five-ring systems, which are linked together by common edges forming the one-dimensional chains.
    Notes: Die Titelverbindung kristallisiert monoklin in der Raumgruppe P21/c (Nr. 14) mit den Gitterdimensionen a = 8,820(1) Å, b = 15,532(3) Å, c = 6,999(2) Å, β = 96,92(4)° und zwei Formeleinheiten in der Elementarzelle. Unter Verwendung von 2368 symmetrieunabhängigen Reflexen konnte die Struktur bis auf Zuverlässigkeitsfaktoren von R = 0,070 und Rw = 0,045 verfeinert werden.Die Struktur ist aus polymeren [Cu(S5)]nn--Anionenketten ∥c aufgebaut und wird durch Wasserstoffbrückensysteme N—H…S, N—H…O, O—H…S und O—H…O stabilisiert. Jedes Cu-Atom ist tetraedrisch von 4 S-Atomen umgeben, die aus drei aus drei verschiedenen (S5)2--Ketten stammen. Dabei liegen über Kanten zu Ketten verknüpfte CuS4- und Cu2S3-Fünfringsysteme vor.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960116
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  • 192
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    Benzamidinium-Hexachlorostannat Synthese und Kristallstruktur (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 133-138 
    Details
    ISSN: 0044-2313
    Keywords: Benzamidinium hexachlorostannate ; synthesis ; crystal structure ; i.r. spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Benzamidinium Hexachlorostannate: Synthesis and Crystal Structure[Ph—C(NH2)2SnCl6] has been prepared by the reaction of hydrogen chloride with the amidinato complex [Ph—C(NSiMe3)2SnCl3] in CH2Cl2 solution, forming colourless crystals. which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P21/c, Z = 4, 3070 observed unique reflexions, R = 0.029. Lattice dimensions at -50°C: a = 892.5, b = 1076.7, c = 1175.6 pm, β = 109.3°. The compound consists of benzamidinium ions C6H5—C(NH2)2+ and anions SnCl62-, which are connected by a network of N—H…Cl hydrogen bridges.
    Notes: [Ph—C(NH2)2]2SnCl6 entsteht in Form farbloser Einkristalle durch Einwirkung von Chlorwasserstoff auf eine Lösung des Amidinatokomplexes [Ph—C(NSiMe3)2SnCl3] in Dichlormethan. Die Verbindung wird durch das IR-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, 3070 beobachtete unabhängige Reflexe, R = 2,9%. Gitterabmessungen bei -50°C: a = 892,5; b = 1076,7; c = 1175,6 pm; β = 109,3°. Die Verbindung besteht aus Benzamidinium-Kationen C6H5—C(NH2)2+ und SnCl62--Ionen, in denen ein Netz von N—H…Cl-Wasserstoffbrücken besteht.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960118
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  • 193
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    Über die Bildung und Kristallstruktur von Mg(HSO4)2 · H2O (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 167-171 
    Details
    ISSN: 0044-2313
    Keywords: Magnesium bis(hydrogensulfate) hydrate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Formation and Structure of Mg(HSO4)2 · H2OMg(HSO4)2 reacts with water under formation of its monohydrate, Mg(HSO4)2 · H2O. This reaction proceeds crystallographically oriented and is reversible. Mg(HSO4)2 · H2O crystallized monoclinic in the space group P21/n, with the unit cell parameters a = 8.623(2), b = 5.014(1), c = 15.428(3) Å, β = 101.32(2)°, V = 654 Å3, Z = 4. The crystal structure of Mg(HSO4)2 · H2O consists of two types of SO3OH-tetrahedra connected over three common oxygen atoms with three different MgO6-octahedra. This motif forms layers parallel to the xy-plane. The layers are arranged at a distance of c/2 and are linked via hydrogen bonds which start from the water of crystallization situated between the layers.
    Notes: Mg(HSO4)2 bildet durch Wasseraufnahme das Monohydrat Mg(HSO4)2 · H2O. Diese Reaktion verläft kristallographisch orientiert und ist reversibel. Mg(HSO4)2 · H2O kristallisiert in der monoklinen Raumgruppe P21/n mit den Gitterkonstanten a = 8,623(2), b = 5,014(1), c = 15,428(3) Å, β = 101,33(2)°, V = 654 Å3, Z = 4. Die Kristallstruktur des Mg(HSO4)2 · H2O ist charakterisiert durch 2 Sorten von SO3OH-Tetraedern, die jeweils über drei gemeinsame Sauerstoffatome mit drei verschiedenen MgO6-Oktaedern verknüpft sind. Dieses Strukturmotiv bildet Schichten parallel zur xy-Ebene. Die Schichten folgen im Abstand von c/2 aufeinander und werden über H-Brücken miteinander verknüpft, die vom Hydratwasser ausgehen, das zwischen den Schichten positioniert ist.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915960122
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  • 194
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    Li3Sr3Ni4N4: Ein Niedervalentes Nitridoniccolat mit ∞1[NiN]-KettenProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 61-67 
    Details
    ISSN: 0044-2313
    Keywords: Lithium strontium nitridoniccolate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li3Sr3Ni4N4: An Low-Valency Nitridoniccolate with ∞1[NiN]-ChainsIsometric black-reflecting crystals of Li3Sr3Ni4N4 (orthorhombic, Immm; a = 401.1(1) pm, b = 708.8(3) pm, c = 1663.0(8) pm; Z = 2) were obtained by wall-reaction of Li4SrN2 in closed nickel tubes (heating rate 50°C/h; reaction at 800°C for 20 h; cooling rate 10°C/h). The crystal structure contains ∞1[NiN]-chains (Ni—N: 177.3(1) pm and 177.8(1) pm) which run parallel to the [010] direction. Lithium and strontium are arranged in planes (010) perpendicular to the [NiN]-chains and interconnect the chains via the nitrogen atoms. Lithium is in a two-fold (linear; Li—N: 200.7(1) pm and 200.4(7) pm), strontium is in three-and four-fold (distorted trigonal-and square-planar) N-coordination (Sr—N: 264.5(5) pm, 268.0(7) pm and 277.6(6) pm, resp.). Nitrogen is in an octahedral surrounding by Ni, Li and Sr; the coordination-octahedra NNi2Sr4 and NNi2Li3Sr are condensed by sharing common edges and apices. The three-dimensional framework contains one-dimensional fragments of the (inverse) octahedral structures of the ReO3 and Rutile structure types.
    Notes: Isometrische, schwarz-glänzende Einkristalle von Li3Sr3Ni4N4 (orthorhombisch, Immm; a = 401,1(1) pm, b = 708,8(3) pm, c = 1663,0(8) pm; Z = 2) wurden in geschlossenen Nickelampullen durch Reaktion von Li4SrN2 mit dem Tiegelmaterial dargestellt (Aufheizraten 50°C/h; 20 h bei 800°C; Abkühlrate 10°C/h). Die Kristallstruktur enthält parallel [010] verlaufende ∞1[NiN]-Ketten (Ni—N: 177,3(1) pm und 177,8(1) pm). Lithium und Strontium sind in Ebenen (010) senkrecht zu den [NiN]-Ketten angeordnet und verknüpfen diese über die Stickstoffatome. Lithium ist zweifach (linear; Li—N: 200,7(1) pm und 200,4(7) pm), Strontium ist sowohl verzerrt trigonal-planar (Sr—N: 264,5(5) pm und 268,0(7) pm) als auch planar-quadratisch (Sr—N: 277,6(6) pm) von Stickstoff koordiniert. Stickstoff selbst ist oktaedrisch von Ni, Li und Sr umgeben; die Koordinationsoktaeder NNi2Sr4 und NNi2Li3Sr werden über gemeinsame Ecken und Kanten miteinander verknüpft. Der insgesamt dreidimensionale Strukturverband enthält eindimensionale (inverse) Fragmente der Oktaederstrukturen des ReO3- und Rutil-Typs.
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    URL: http://dx.doi.org/10.1002/zaac.19915970109
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    Ag18(SiO4)2(Si4O13), das erste Silbersilicat mit gemischten AnionenProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 79-86 
    Details
    ISSN: 0044-2313
    Keywords: Silver silicate ; mixed-anion silicate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ag18(SiO4)2(Si4O13), the First Mixed-Anion Silver(I) SilicateThe system Ag2O/SiO2 has been investigated at Ag : Si = 3 : 1 by solid state reactions. Ag6Si2O7(II) forms from the binary components applying elevated oxygen pressures (p(O2) = 0.2 GPa) at 560-580°C. By adding conc. NH3-solution to the same starting mixtures Ag6Si2O7(I) forms at 500-550°C. Hitherto unknown (Ag4SiO4)2 · Ag10Si4O13 is the product if the temperature is kept below 470°C. (Ag4SiO4)2 · Ag10Si4O13 transforms in an irreversible phase transition to Ag6Si2O7(I) at T = 495 ± 10°C. The crystal structure of (Ag4SiO4)2 · Ag10Si4O13 (C2/m; a = 1201.7(1), b = 1060.7(1), c = 607.4(1) pm, β = 106.7(1)°; 1927 independent reflections; R = 0.06; Rw = 0.05) is constituted from orthosilicate and catena-tetrasilicate anions. The catena-tetrasilicate anions exhibit 2/m point symmetry. The intense red colour indicates the existence of weak Ag—Ag bonding interactions (shortest Ag+—Ag+ separation: 282.1 pm).
    Notes: Das System Ag2O/SiO2 wurde bei dem Schnitt Ag : Si = 3 : 1 präparativ untersucht. Aus den binären Komponenten entsteht in einer Festkörperreaktion unter Sauerstoffdrucken 〉 0,2 GPa und im Temperaturbereich von 560-580°C Ag6Si2O7(II) als offensichtlich thermodynamisch stabile Phase. Bei Zusatz von konz. NH3 bildet sich zwischen 500 und 550°C Ag6Si2O7(I) und unterhalb 470°C (Ag4SiO4)2 · Ag10Si4O13. Diese neu erhaltene Verbindung wandelt sich bei 495 ± 10°C irreversibel in Ag6Si2O7(I) um. Die Kristallstruktur von (Ag4SiO4)2 · Ag10Si4O13 (C2/m; a = 1201,7(1), b = 1060,7(1), c = 607,4(1) pm, β = 106,7(1)°; Z = 2; 1927 unabhängige Reflexe; R = 0,06; RW = 0,05) enthält nebeneinander Orthosilicat- und catena- Tetrasilicatanionen. Letztere haben die Lagesymmetrie 2/m. Die intensiv rote Eigenfarbe wird auf schwache Ag—Ag-Wechselwirkungen (kürzester Ag—Ag-Abstand: 282, 1 pm) zurückgeführt.
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    URL: http://dx.doi.org/10.1002/zaac.19915970111
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    Rb[Re3Br10]  -  das erste ternäre Rhenium(III)-Halogenid mit KettenstrukturProfessor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 107-113 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium bromides ; cluster ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Rb[Re3Br10]  -  the First Ternary Rhenium(III) Halide with a Chain StructureRb[Re3Br10] crystallizes on evaporation of a hydrobromic acid solution of rhenium tribromide and rubidium bromide as dark red-brown single crystals. The crystal structure (monoclinic; C2/m; a = 1469.09(10); b = 1085.75(8); c = 1019.15(8) pm; β = 91.81(1)°; Vm = 245.1(2) cm3mol-1; Z = 4) is built up of chains along [010] of [Re3Br12] units that are connected via two edges. The anionic chains are held together by rubidium ions. Each cation is surrounded by eight bromide ions at distances between 332 and 368 pm with four additional bromide ions at 401 to 427 pm. This is the first example of a ternary rhenium halide with a chain structure. Only salts with isolated cluster anions [Re3X12-y(H2O)y](3-y)- (X = Cl, Br; y = 0-3) have been known so far.
    Notes: Aus bromwasserstoffsaurer Lösung von Rheniumtribromid und Rubidiumbromid kristallisieren beim Eindunsten dunkelrotbraune Einkristalle von Rb[Re3Br10] aus. Die Kristallstruktur (monoklin; C2/m; a = 1469,09(10); b = 1085,75 (8); c = 1019,15(8) pm; β = 91,81(1)°; Vm = 245,1(2) cm3mol-1; Z = 4) baut sich aus Ketten doppelt kantenverknüpfter [Re3Br12]-Baugruppen entlang [010] auf. Die anionischen Stränge kantenverknüpfter Cluster werden von Rubidiumionen zusammengehalten. Dabei ist jedes Kation von acht Bromid-Ionen in einem Abstand von 332-368 pm umgeben sowie von vier weiteren in einem Abstand zwischen 401 und 427 pm. Dies ist das erste Beispiel eines ternären Rhenium(III)-halogenids mit Kettenstruktur. Bislang waren nur Salze mit isolierten Clustern [Re3X12-y(H2O)y](3-y)- (X = Cl, Br; y = 0-3) bekannt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915970114
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    Das erste Gadoliniumcarbidfluorid: Gd2CF2Professor Hanskarl Müller-Buschbaum zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 145-150 
    Details
    ISSN: 0044-2313
    Keywords: Gadolinium carbide fluoride ; condensed clusters ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Gadolinium Carbide Fluoride: Gd2CF2Gd2CF2, the first gadolinium carbide fluoride is prepared by reaction of stoichiometric amounts of GdF3, Gd, and C at 1250°C in sealed Ta-capsules. It is isotypic with Gd2CBr2 (space group P3m1; a = 373.11(4) and c = 642.5(1) pm). The Gd atoms surround the C atoms octahedrally. Such Gd6C octahedra are condensed via edges to form octahedral sheets, which are separated by double slabs of F-- ions.
    Notes: Mit Gd2CF2 konnte erstmals ein Gadoliniumcarbidfluorid dargestellt werden. Man erhält Gd2CF2 durch Reaktion von stöchiometrischen Mengen GdF3, Gd und C bei 1250°C in verschweißten Ta-Ampullen. Es ist isotyp mit Gd2CBr2 (Raumgruppe P3m1; a = 373,11(4) und c = 642,5(1) pm). Die C-Atome sind von Gd-Atomen oktaedrisch umgeben. Diese Gd6C-Oktaeder sind zweidimensional zu Oktaederschichten kondensiert, die durch F---Doppelschichten voneinander getrennt sind.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915970117
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    Darstellung und Kristallstruktur von Kupfer(II)-monofluorophosphat-Dihydrat CuPO3F · 2H2OProfessor Helmut Köhler in memoriam (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 600 (1991), S. 231-238 
    Details
    ISSN: 0044-2313
    Keywords: Copper(II) monofluorophosphate dihydrate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Salts of Halogenophosphoric Acids. XVII. Preparation and Crystal Structure of Copper(II) Monofluorophosphate Dihydrate CuPO3F · 2H2OCopper(II) monofluorophosphate dihydrate, CuPO3F · 2H2O 1 was obtained by the reaction of aqueous NH4HPO3F and acid (NH4)2PO3F solutions, respectively, using acetone or ethanol as precipitating agents. The thermal dehydration of 1 gives the water-free copper monofluorophosphate CuPO3F (2). 1 crystallizes in the monoclinic space group P21/c with a = 761,44, b = 780,97, c = 921,02 pm, β = 112,94° and Z = 4.
    Notes: Bei der Reaktion von wäßrigen NH4HPO3F- bzw. sauren (NH4)2PO3F-Lösungen mit Kupfer(II)-Salzen wird unter Zusatz von Aceton bzw. Ethanol als Fällungsmittel Kupfer(II)-monofluorophosphat-Dihydrat CuPO3F · 2H2O 1 als kristalliner Niederschlag gebildet. Aus 1 läßt sich durch thermische Entwässerung wasserfreies Kupfer(II)-monofluorophosphat CuPO3F 2 herstellen.1 kristallisiert in der monoklinen Raumgruppe P21/c mit a = 761,44, b = 780,97, c = 921,02 pm, β = 112,94° und Z = 4.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916000132
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    PdSCl, ein molekulares Palladium(II)-disulfidchlorid mit achtkernigen Pd8(S2)4Cl8-Komplexen und vierfach überbrückenden DisulfidgruppenProfessor Hans Georg von Schnering zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 253-258 
    Details
    ISSN: 0044-2313
    Keywords: Palladium(II) disulfidechloride ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: PdSCl, a Molecular Palladium(II) Disulfidechloride with Octanuclear Pd8(S2)4Cl8 Groups and with Tetra Metal-coordinated bridging Disulfide GroupsBlack crystals of PdSCl have been obtained by reaction of Pd with S2Cl2 in closed quartz ampoules at 200°C. The compound is to be formulated as a Palladium(II)-disulfidechloride consisting of Pd8(S2)4Cl8 molecules with approximately D4h symmetry. In the octanuclear complexes Pd atoms form a cube, where bridging disulfide groups are found in front of 4 faces and μ2-bridging Cl atoms on 8 edges. In the monoclinic crystal structure (a = 8.763(2) Å; b = 9.082(2) Å; c = 13.662(4) Å; β = 91.748(23)°; V = 1086.8 Å3; Z = 16 PdSCl; Space gr. P21/n) the molecules form a cubic closed arrangement.
    Notes: Schwarze Kristalle von PdSCl wurden durch Umsetzung von Pd-Metall mit S2Cl2 in geschlossenen Ampullen bei 200°C erhalten. Die Verbindung ist ein Palladium(II)-disulfidchlorid, aufgebaut aus molekularen Pd8(S2)4Cl8-Gruppen mit annähernd D4h-Symmetrie. In den achtkernigen Komplexen bilden Pd-Atome einen Würfel mit S2-Gruppen vor vier Flächen und Cl-Atomen vor 8 Kanten. In der monoklinen Kristallstruktur (a = 8,763(2) Å; b = 9,082(2) Å; c = 13,662(4) Å; β = 91,748(23)°; V = 1086,8 Å3; Z = 16 PdSCl; Raumgr. P21/n) sind die Moleküle kubisch dichtest gepackt.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915980122
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    Untersuchungen über Zinn(IV)-alkoxide. I Kristall- und Molekülstruktur des Zinn(IV)-isopropanolat-Isopropanolsolvats, Sn(OiPr)4 · i-PrOHProfessor Hans-Georg von Schnering zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 259-268 
    Details
    ISSN: 0044-2313
    Keywords: Tin(IV)-isopropoxide-isopropanol solvate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigations into Tin(IV) Alkoxides. I. Crystal and Molecular Structure of Tin(IV)-isopropoxide-Isopropanol Solvate, Sn(OiPr)4 · i-PrOHThe isopropanol complex of tin(IV)-isopropoxide has been prepared by the reaction of tin tetrachloride with sodium isopropoxide. The compound forms colourless, moisture sensitive crystals, which in dry air easily release the coordinated solvent molecules. The crystal and molecular structure of Sn(OiPr)4 · i-PrOH has been determinated by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P21/c with a = 1174.2(5), b = 1428.5(3), c = 1234.1(3) pm, β = 95.37(1)° and Z = 4. The crystal structure consists of discrete, dimeric molecules in which the two tin atoms are bridged by two alkoxide groups. The octahedral coordination sphere of each tin atom is completed by one solvent molecule which, in addition, forms one hydrogen bridge to an alkoxide group of the neighboring tin atom.
    Notes: Der Isopropanolkomplex des Zinn(IV)-isopropanolats wurde durch Reaktion von Zinntetrachlorid mit Natriumisopropanolat in Isopropanol hergestellt. Die Verbindung bildet farblose, feuchtigkeitsempfindliche Kristalle, die an trockener Luft das koordinierte Lösungsmittelmolekül sehr leicht abgeben. Die Kristall- und Molekülstruktur von Sn(OiPr)4 · i-PrOH wurde durch Röntgenstrahlbeugung an einem Einkristall bestimmt. Die Verbindung kristallisiert in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 1174,2(5), b = 1428,5(3), c = 1234,1(3) pm, β = 95,37(1)° und Z = 4. Die Kristallstruktur besteht aus diskreten, dimeren Molekülen, in denen die beiden Zinnatome über zwei Alkoxidreste verbrückt werden. Die oktaedrische Koordinationssphäre an den Zinnatomen wird durch jeweils ein Lösungsmittel-Molekül vervollständigt, das zusätzlich eine Wasserstoffbrücke zu einem Alkoxidrest am benachbarten Zinnatom bildet.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915980123
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