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  • 1990-1994  (282)
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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
    Electronic Resource
    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.
    Type of Medium: Electronic Resource
    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.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/aoc.590080107
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  • 155
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    Reversible formation of an intramolecular agostic CH interaction in a dimanganese complex (1992)
    Springer
    Journal of cluster science 3 (1992), S. 103-108 
    Details
    ISSN: 1572-8862
    Keywords: Manganese ; agostic ; crystal structure ; CH activation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Agostic interactions of CH bonds with metal atoms are currently of great interest. UV irradiation of Mn2(CO)8 (PMe2Ph)2 in the presence of the HC≡COEt yielded the new compound Mn2(CO)6(PMe2Ph)2 [μ-C(OEt)=C(H)C=C(H)C=O(OEt)],1 that contains a strong agostic interaction of an olefinic CH bond to one of the managanese atoms, Mn...C=2.349(5), Mn...H=2.01(4). This interaction can be removed (reversibly) by CO addition (25°C/1000 psi) to1 to yield the new complex Mn2(CO)7(PMe2Ph)2[μ-C(OEt)=C(H)C=C(H)C=O(OEt)],2.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00814614
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  • 156
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    Further studies of M3(μ3-O)(μ-X)3(μ-O2CCH3)3L3 (M=Mo, W) type clusters with nine core electrons (1992)
    Springer
    Journal of cluster science 3 (1992), S. 123-144 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum ; tungsten ; crystal structure ; reduction ; acetate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Four new compounds having nine cluster electrons and cores of the types Mo3OCl3, Mo3OBr3, and W3OCl3 are reported. Compound (1) prepared by reduction of [Bu4N][Mo3OCl6(OAc)3] in THF with metallic zinc, was shown by X-ray crystallography to be Mo3OCl4(OAc)3 (THF)2 (1). It forms crystals in space groupP21 with unit cell dimensionsa=9.472(2) Å,b=13.546(4) Å,c=9.652(2) Å, β=101.70(2)°,V=1201(1) Å3,Z=2. The [Mo3(μ3-O)(μ-Cl)3]4+ core is surrounded by three μ-O2CCH3 anions, one Cl−, and two THF and has Mo-Mo distances of 2.620(1) Å, 2.613(1) Å, and 2.530(1) Å, with the shortest bond between the two Mo atoms to which the THF molecules are coordinated. Compounds [Bu4N]2 [Mo3OBr6(O2CCH3)3] · Me2CO, (2) and [Mo3OBr3(O2CCH3)3(PMe3)3]3 · BF4, (3) are the first two nine-electron Mo3 species with a [Mo3(μ3-O) Br3]4+ core. Both were obtained by zinc reduction of [Mo3OBr6(O2CCH3)3]− in the presence of (NBu4) Br (2) or PMe3 and NaBF4 (3), and each was characterized crystallographically. Compound (2) crystallized in space group Cc with unit cell dimensionsa=25.037(5) Å,b=12.827(2) Å,c=21.484(4) Å, β=122.96(1)0,V=5790(3) Å3,Z=4. While the anion has no crystallographically required symmetry, its virtual symmetry is C3v . The Mo-Mo distances are 2.619(2) Å, 2.610(3) Å, 2.644(2) Å, with a mean value of 2.624[14] Å. Compound (3) crystallized in space groupP21/c with unit cell dimensionsa=10.846(2) Å,b=25.033(5) Å,c=12.641(5) Å, β=94.74(2)0,V=3420(2) Å3,Z=4. The cation occupies a general position but has virtual C3v symmetry, with Mo-Mo distances of 2.601(2) Å, 2.610(2) Å, 2.627(2) Å, with a mean value of 2.613[14] Å. Thus the anionic and cationic Mo3 clusters in (2) and (3), respectively, have average Mo-Mo distances that are equal within experimental error. Compound (4), [NEt4]2 [W3OCl6(O2CCH3)3] is the first 9-electron compound of this type containing tungsten. It was prepared by reduction of [Et4N][W3OCl6(OAc)3] in benzene with Na/Hg. It crystallized in space groupP212121 with unit cell dimensionsa=11.076(2) Å,b=14.345(2) Å,c=21.026(3) Å,V=3574(1) Å3,Z=4. The anion resides on a general position but has virtual C3v symmetry, with W-W distances of 2.577(1) Å, 2.612(1) Å, 2.584(1) Å and a mean value of 2.591[15] Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702878
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  • 157
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    Synthesis, structural characterization and bonding properties of heterometallic-heterobridging cubane-type tetranuclear cluster compounds [CuMo3OS3]·I·(μ-OAc)[S2P(OC2H5)2]3·L (L=py, DMF) (1992)
    Springer
    Journal of cluster science 3 (1992), S. 179-199 
    Details
    ISSN: 1572-8862
    Keywords: Heterometallic-heterobridging cubane-type tetranuclear cluster ; preparation ; crystal structure ; molecular orbital calculation ; quasi-aromaticity ; copper ; molybdenum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract By the reaction of cluster [Mo3OS3](dtp)4(H2O) used as starting material with CuI using [3+1] mode, two novel heterometallic-heterobridging cubane-type tetranuclear cluster compounds [CuMo3OS3]·I·(μ-OAc)[S2P(OC2H5)2]3·L [(I)L=py, (II)L=DMF] [dtp=S2P(OC2H5)2; OAc=OOCCH3] containing [CuMo3OS3] core have been obtained. Compounds (I) and (II) have been characterized by IR, EPR, UV-VIS, electrochemistry and X-ray crystallography. By comparison of these two compounds with the analogous [CuMo3S4] series in the structure and molecular orbital calculation, the influence of mixed S/O bridging on the structure is discussed. It is demonstrated that the {Mo3S3} cluster ring in [Mo3OS3]4+ possesses a similar quasi-aromaticity to [Mo3S4]4+. Crystal data: for (I), space group= $$P\overline 1 $$ ,a=13.781(8)Å,b=14.523(6)Å,c=12.098(6)Å, α=98.37(4)°, β=109.41(5)°, γ=105.00(5)°,V=2133(2)Å3,Z=2,R=0.058; for (II), space group= $$P\overline 1 $$ ,a=13.215(4)Å,b=17.818(8)Å,c=9.873(4)Å, α=106.06(4)°, β=109.78(3)°, γ=82.00(3)°,V=2100(2)Å3,Z=2,R=0.045.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00702882
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  • 158
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    Packing analysis and the crystal chemistry of 2,5-dibenzylidenecyclopent-3-ene-1-one. Rationale for a non-topochemical solid-state reaction (1992)
    Springer
    Molecular engineering 2 (1992), S. 103-116 
    Details
    ISSN: 1572-8951
    Keywords: Non-topochemical reaction ; crystal structure ; lattice energy calculations ; thermal motion analysis ; disorder
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular and crystal structure of 2,5-dibenzylidenecyclopent-3-ene-1-one has been studied in detail to explain the formation of a non-topochemical pseudo-mirror-symmetric dimer upon photoirradiation. Packing energy calculations, analysis of the thermal motion, and lattice energy calculations are employed to analyse and understand the observed dimerization reaction, crystal structure, and crystal properties.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00999702
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  • 159
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    The crystal and molecular structures of 1,1′-divinyl-2,2′-biimidazolyl (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 1076-1079 
    Details
    ISSN: 1573-9171
    Keywords: X-ray crystallographic analysis ; 1,1′-divinyl-2,2′-biimidazolyl ; crystal structure ; molecular structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structures of 1,1′-divinyl-2,2′-biimidazolyl (L) were determined by x-ray crystallographic analysis. It was established that the molecule of L has crystallographic symmetry 2 and a cisoid conformation with an angle of rotation of 128° between the imidazole rings. The length of the C2-C2′ bond is increased to 1.485(11) Å compared with the length of the analogous bond in unsubstituted 2,2′-biimidazolyl (1.423 Å). Localization of the N=C multiple bond is observed [1.297(9) Å]. The other N-C bonds of the ring are almost equalized (1.374 Å) and are close to the standard values for bonds of the C sp 2-N type in imidazoles. The angle between the plane of the heterocycle and the plane passing through the atoms of the vinyl group amounts to 7°.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00866589
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  • 160
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    Photo- and thermochromic mannich bases. 1. Mannich bases from 3,5-di-tert-butyl-4-hydroxybenzaldehyde and 2-naphthols (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 1875-1883 
    Details
    ISSN: 1573-9171
    Keywords: synthesis ; crystal structure ; UV spectra ; 2,6-di-tert-butyl-4-[α-(2-hydroxy-1-naphthyl)methyl]phenol ; 2,6-di-tert-butyl-4-[α-morpholino-α-(2-hydroxy-6-bromo-1-naphthyl)methyl]phenol ; 2,6-di-tert-butyl-4-α-(2-hydroxy-1-naphthyl)-1,4-methylenequinone ; 2,6-di-tert-butyl-4-α-(2-acetyloxy-1-naphthyl)-1,4-methylenequinone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Mannich bases exhibiting photo- and thermochromic properties in solutions were synthesized from 3,5-di-tert-butyl-4-hydroxybenzaldehyde and 2-naphthols. An investigation of an acetyl derivative of methylenequinone, modeling a product of photo- and thermochromic transformations, proved that the color change of solutions of the Mannich bases is due to reversible dissociation into colored methylenequinones and morpholine. On the basis of data of x-ray diffraction analysis of one of the Mannich bases, characteristics of their molecular structure were determined, and reasons were stated for their effect on the dissociation mechanism.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863826
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  • 161
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    Synthesis and physicochemical investigation of LiMTif6 (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 1950-1956 
    Details
    ISSN: 1573-9171
    Keywords: hexafluorotitanates ; synthesis ; crystal structure ; 19F NMR ; IR spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Mixed alkali hexafluorotitanates of the composition LiMTiF6 are synthesized, which crystallize with the orthorhombic symmetry. The lattice parameters of these materials are determined. It is shown that substitution of the Li+ cation in Li2TiF6 by Na+, K+, Rb+, and Cs+ leads to various degrees of distortion of the hexafluoroion. It is determined (19F NMR data) that the change in the dynamic state of the octahedral [TiF6]2− ions is related to their transition from the hindered-rotational to the isotropic state.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863353
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  • 162
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    Macrocyclic amidophosphoryl polyethers: Biological activity, molecular structure, and structure of the complex with calcium thiocyanate (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 2211-2216 
    Details
    ISSN: 1573-9171
    Keywords: macrocyclic polyethers ; crystal structure ; biological activity ; IR spectra ; complex with calcium thiocyanate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The antihypoxic and anticonvulsant activity of eight new amidophosphoryl derivatives of crown ethers was investigated. It was found that some of them exhibit pronounced antihypoxic activity. The results of an x-ray structural and IR spectroscopic study of dibenzo-N-phenylphosphonyl-14-crown-5 (a=9.818,b=16.062,c=15.925 Å; γ=124.90°;V=2072 Å3;M=417.2;d=1.33 g/cm3 forZ=4, 1955 independent reflections [I〉3σ(I)] in a DAR-UM inCuK α radiation,P2 1/b space group,R=5.2%) and dibenzo-N-adamantylphosphonyl-14-crown-5 compounds (a=11.077,b=15.936,c=16.771 Å; γ=56.05°;V=2456 Å3;M=486.3;d=1.31 g/cm3 forZ=4, 2164 independent reflections [I〉3σ(I)] in a DAR-UM inCuK α radiation,P21/b space group,R=5.1%) are reported. Some details of the structure of the dibenzo-N-phenylphosphonyl-14-crown-5-complex with calcium thiocyanate and water are discussed; a polyhedron with a coordination number of six was found for the first time for calcium complexes with macrocyclic ligands. The combined examination of the results of the biological, x-ray structural, and IR spectroscopic study of macrocyclic, 14-member ligands suggested that the nature of the substituents at phosphorus affect the conformational state of the macrocycle, which remains unchanged in complexation in the investigated conditions.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01150749
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  • 163
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    Crystal and molecular structure of 1:1 molecular complexes of triphenyl-N-(4-methylpyridyl-2)phosphinimine and triphenyl-N-(3-methylpyridyl-2)phosphinimine with perchloric acid (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 495-499 
    Details
    ISSN: 1573-9171
    Keywords: crystal structure ; molecular complexes ; phosphinimines ; protonation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract X-ray diffraction analysis has been used to determine the crystal structures of the 1:1-composition products of protonation by perchloric acid of isomeric triphenyl-N-(4-methylpyridyl-2)phosphinimine (1) and triphenyl-N-(3-methylpyridyl-2)phosphinimine (2). The structures were refined toR=0.048 andR=0.052, respectively, using 2274 (1) and 2647 (2) reflections. The protonation centers are located at the sites of N atoms of the pyridine ring (1) and the phosphinimino group (2). The distribution of the bond lengths in the cations suggests that a significant contribution is made by a phosphonic structure with positive charges localized on the P atoms. N-H...O hydrogen bonds, with lengths of 2.890(4) and 3.020(3) Å, connect cations and anions in both structures.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863071
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  • 164
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    1,1,4,4-Tetranitrobutane-2,3-diol and its derivatives. 4. Study of the reaction of 1,1,4,4-tetranitrobutane-2,3-diol with N-(methoxymethyl)-2-fluoro-2,2-dinitroethylamine; synthesis and crystalline structure of 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 528-530 
    Details
    ISSN: 1573-9171
    Keywords: synthesis ; crystal structure ; 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A two-step synthesis has been proposed to obtain 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate, starting from 1,1,4,4-tetranitrobutane-2,3-diol and N-(methoxymethyl)-2-fluoro-2,2-dinitroethyl-amine, followed by nitration of the Mannich base formed. An x-ray-diffraction investigation of the dinitrate obtained was carried out.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00863077
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  • 165
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    X-ray structure of the organic conductor (ET)8[Hg2Br6·PhBr]2 (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 697-703 
    Details
    ISSN: 1573-9171
    Keywords: organic metals ; radical-cation salts ; bis(ethylenedithio)tetrathiafulvalene = ET ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The electrochemical oxidation of ET [bis(ethylenedithio)tetrathiafulvalene] in bromobenzene (electrolyte Bu 4 N[HgBr 3 ]) gave the radical-cation salt (ET) 8 [Hg 2 Br 6 ·PhBr] 2 (1), a new organic metal with a temperature range of 300–125 K. At 125 K a metal—dielectric transition is observed. Crystallographic data for (1):a=19.171(6),b=12.668(4),c=17.777(6) Å, α=118.03(3), β=89.45(2), γ=101.21(3)°, P $$\overline 1 $$ ,Z=1,d calc=2.30 g/cm 3 . The crystal structure of (1) is laminar. In the conducting organic layer the ET radical cations are linked into bands by shortened intermolecular S···S contacts of the “side-to-side” type. The anionic layer consists of centrosymmetric complexes [Hg 2 Br 6 ·C 6 H 5 Br] 2 4− . The Hg 1 and Hg 2 atoms are characterized by a trigonal configuration of the Hg-Br bond which is built up, on account of secondary Hg···Br interactions, into trigonal-bipyramidal for Hg 1 and trigonal-pyramidal (tetrahedral) for Hg 2 . Interaction between the anionic and cationic layers is effected through Br 6 ...S 8 contacts [3.491(7) Å)].
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01150895
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    Crystal structure of the organic metal (ET)2[Hg(SCN)2Cl] withT M-D=50 K (1992)
    Springer
    Russian chemical bulletin 41 (1992), S. 704-709 
    Details
    ISSN: 1573-9171
    Keywords: organic metals ; bis(ethylenedithio)tetrathiafulvalene (ET) ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The composition and structure of the radical-ion salt (ET) 2 [Hg(SCN) 2 Cl], a new organic metal withT M-D=50 K, were established in an x-ray structure investigation. Principal crystallographic data:a=36.69(1),b=8.302(8),c=11.732(8) Å, β=90.02(6)°, space groupCc, Z=4,d calc=2.08 g/cm 3 ,R=0.067. The crystal structure of the salt consists of an alternation of organic (cationic) and inorganic (anionic) layers along the axisa. The anionic layer consists of the polymeric chains in which the [Hg(SCN) 2 Cl]− ions are linked together along the axisc through secondary Hg···N bonds with lengths of 2.75(3) and 2.98(8) Å. On account of these interactions the trigonal configuration of the bonds of the Hg atom is built up to trigonal-bipyramidal. In the organic layer with a structure of the κ type the ET cations form dimers with an interplanar distance of 3.53 Å. ET cations belonging to neighboring dimers are linked together through shortened intermolecular S...S contacts with lengths of 3.40–3.50(2) Å.
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    URL: http://dx.doi.org/10.1007/BF01150896
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    Calixarenes as second-sphere ligands for transition metal ions. Synthesis and crystal structure of [(H2O)5 Ni(NC5H5)]2(Na)[calix[4]arene sulfonate] · 3.5 H2O and [(H2O)4Cu(NC5H5)2]-(H3O)3 [calix[4]arene sulfonate] · 10 H2O (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 37-46 
    Details
    ISSN: 1573-1111
    Keywords: Calix[4]arene ; crystal structure ; second-sphere coordination ; nickel(II) ; copper(II) ; pyridine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title compounds crystallize such that bilayers of calixarenes are separated by hydrophilic layers. In each case the transition metal has, in addition to a primary sphere of ligands, a second-sphere coordination by a calixarene. [(H2O)5Ni(NC5H5)]2(Na)[calix[4]arene sulfonate]·3.5 H2O,1, crystallizes in the triclinic space groupP $$\bar 1$$ witha = 12.487(4),b = 14.281(2),c = 15.055(5) Å, α = 85.66(2), β = 80.07(2), γ = 80.48(2)°, andD c = 1.64 g cm−3 forZ = 2. Refinement based on 2441 observed reflections led to a finalR value of 0.066. There are two different environments for the nickel-containing cations: one is positioned within the hydrophilic layer with the pyridine ligand intercalated into the hydrophobic calixarene bilayer and the other is also positioned within the hydrophilic layer, but the pyridine ligand is inserted into the hydrophobic cavity of the calix[4]arene. [(H2O)4Cu(NC5HS)2](H3O)3[calix[4]arene sulfonate]·10 H2O,2, crystallizes in the triclinic space groupP $$\bar 1$$ witha = 15.438(4),b = 15.727(6),c = 12.121(9) Å, α = 112.74(4), β = 102.02(4), γ = 85.34(4)°, andD c = 1.57 g cm−3 forZ = 2. Refinement based on 3925 observed reflections led to a finalR value of 0.107. The structure is similar to that of 1 except that the one copper-containing cation spans the hydrophilic layer and is intercalated into the bilayer of calixarenes on one side and positioned into the calixarene cavity on the other.
    Type of Medium: Electronic Resource
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    Isomerization processes in inclusion compounds: Xylenes in deoxycholic acid (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 55-64 
    Details
    ISSN: 1573-1111
    Keywords: Host-guest inclusion compound ; p-,m-,o-xylene ; deoxycholic acid ; symmetry factor ; energy transfer ; photophysical factor ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The isomerization processes induced by UV photons in inclusion compounds of the host-guest type are examined, with special attention to the photophysics of the energy transfer process between the host and the guest, as well as to the influence of the host molecular cavity symmetry and the guest molecular symmetry. In particular, the experimental study has been carried out on the isomerization processes ofp-,m-, ando-xylene inside the molecular cavities of deoxycholic acid. The results have been compared with those obtained by irradiating the xylenes in an inert solution of hexane. The main difference is the elimination of by-products when the photochemical process is carried out in the solid state inclusion compound; however, the high purity of the isomerization product corresponds to a decrease in its yield with respect to the reaction in solution, due to the energy transfer process from the host to the guest moiety.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01041366
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  • 169
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    Crystal structure analysis of Y2Cu2O5 (1992)
    Springer
    Journal of superconductivity 5 (1992), S. 33-38 
    Details
    ISSN: 1572-9605
    Keywords: Yttrium ; copper ; X-ray ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: Abstract Single crystals of Y2Cu2O5 were obtained in the flux growth process by controlled heating of a mixture of Y2O3, BaO, and CuO in a molar ratio of 1∶8∶20. These crystals were analyzed by a single-crystal X-ray diffraction analysis. The crystal contains polymeric chains of Cu2O5 interspersed by yttrium ions surrounded by octahedral arrangements of oxygen atoms. Crystal data: space group=Pna21,a=10.799(2) Å,b=3.4990(5) Å,c=12.459(2) Å,Z=4, 380 reflections,R=0.026,R w=0.030.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00617994
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  • 170
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    Three-dimensional structure of the quinoprotein methylamine dehydrogenase from Paracoccus denitrificans determined by molecular replacement at 2.8 Å resolution (1992)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 14 (1992), S. 288-299 
    Details
    ISSN: 0887-3585
    Keywords: amino acid-derived cofactor ; crystal structure ; methylamine dehydrogenase ; molecular replacement ; oxidoreductase ; Paracoccus denitrificans ; pyrroloquinoline quinone ; quinoprotein ; tryptophan tryptophylquinone ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The three-dimensional structure of the quinoprotein methylamine dehydrogenase from Paracoccus denitrificans (PD-MADH) has been determined at 2.8 Å resolution by the molecular replacement method combined with map averaging procedures, using data collected from an area detector. The structure of methylamine dehydrogenase from Thio-bacillus versutus, which contains an “X-ray” sequence, was used as the starting search model. MADH consists of 2 heavy (H) and 2 light (L) subunits related by a molecular 2-fold axis. The H subunit is folded into seven four-stranded β-segments, forming a disk-shaped structure, arranged with pseudo-7-fold symmetry. A 31-residue elongated tail exists at the N-terminus of the H subunit in MADH from T. versutus but is partially digested in this crystal form of MADH from P. denitrificans, leaving the H subunit about 18 residues shorter. Each L subunit contains 127 residues arranged into 10 β-strands connected by turns. The active site of the enzyme is located in the L subunit and is accessible via a hydrophobic channel between the H and L subunits. The redox cofactor of MADH, tryptophan tryptophylquinone is highly unusual. It is formed from two co-valently linked tryptophan side chains at positions 57 and 107 of the L subunit, one of which contains an orthoquinone. © 1992 Wiley-Liss, Inc.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340140214
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  • 171
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    Physicochemical Properties of Salts of p-Aminosalicylic Acid. I. Correlation of Crystal Structure and Hydrate Stability (1992)
    Springer
    Pharmaceutical research 9 (1992), S. 1428-1435 
    Details
    ISSN: 1573-904X
    Keywords: pharmaceutical salt selection ; salts of p-aminosalicylic acid ; hydrates ; crystal structure ; thermal stability
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The potassium (K), sodium (NA), calcium (CA), and magnesium (MG) salts of p-aminosalicylic acid were obtained, and their thermal behavior was characterized by means of differential scanning calorimetry (DSC) and thermogravimetric analysis (TG). Their crystal and molecular structures were determined by single-crystal X-ray diffraction after powder patterns had shown them to be nonisomorphous. Different degrees of hydration were observed for the solid salts, and an assessment of hydrate stability to dehydration was made from thermogravimetric studies. The onset temperature of dehydration (T t) of each salt varied within the series and exhibited correlation with X-ray determined structure. The observed onset of dehydration of MG and CA was higher than that of NA and is consistent with stronger ion-dipole interactions for the divalent salts. Crystallographic determination of the bond lengths between the metal ion and the water oxygens were 2.4 and 2.9 Å for NA, between 2.0 and 2.1 Å for MG, and 2.4 Å for CA. The open nature and presence of a channel feature in the structure of the sodium salt may have facilitated escape of water molecules from the crystal. Particle presentation (e.g., size, crystallinity) was also shown to affect dehydration behavior.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1015806812349
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  • 172
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    The Structure of Celiprolol (1992)
    Springer
    Pharmaceutical research 9 (1992), S. 365-371 
    Details
    ISSN: 1573-904X
    Keywords: celiprolol ; crystal structure ; two-dimensional nuclear magnetic resonance (2D NMR)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure and nuclear magnetic resonance (NMR) spectra and assignments of celiprolol, N′-[3-acetyl-4[3-[N-t-butylamino-2-hydroxypropoxy]phenyl]-N, N-diethylurea, are reported. Celiprolol crystallizes in the monoclinic space group, P2l/a, with a = 9.081(2), b = 13.800(4), and c = 17.471(5) Å and β = 95.04(2)°. Structure was solved by direct methods; structure refinement to R of 0.058. Intermolecular hydrogen-bonding in the crystal is discussed. The 1H, 13C, and two-dimensional (2D) NMR spectra of the hydrochloride have been obtained and definitive signal assignments made.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1015895019791
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  • 173
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    Solid state structure of the hydrated potassium thiocyanate complex of benzodinaphthopyridino 21-crown-7, C37H31NO6·KSCN·H2O (1 : 1 : 1) (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 29-36 
    Details
    ISSN: 1573-1111
    Keywords: Crown compound ; potassium thiocyanate ; crown cation complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Single crystal X-ray analysis of the hydrated KSCN complex of benzodinaphthopyridino-21-crown-7 (1) (1 : 1 : 1) is reported. Crystals of the complex are orthorhombic,Pnma, withα = 16.946(4),b = 22.298(4),c = 10.390(8) Å andD c = 1.184 g cm−1,Z = 4. The host macroring (1) has a mirror symmetry and exists in a so-called ‘dentists chair’ conformation. The cation (K−) is coordinated to all the six ether oxygen atoms and also weakly to the pyridine N atom. The SCN− anion group has a statistical type of disorder with opposite orientations of S and N such that nitrogen and sulphur are coordinated to K+. Packing of the host molecules is in columns to form quasi channels with K+, SCN−, and H2O being located inside the stacks.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01076668
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  • 174
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    Complexation with hydroxy host compounds, part 5. Structures and thermal analyses of 1,2,3,4,5-pentaphenylcyclopenta-2,4-dien-1-ol and its inclusion compounds with water and dimethylsulphoxide (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 301-310 
    Details
    ISSN: 1573-1111
    Keywords: Inclusion compound ; hydroxy compound ; crystal structure ; thermal analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structures of the title host compound (I), C35H26O, and its inclusion complexes with water (II), C35H26O·H2O and dimethylsulphoxide (III), C35H26O·C2H6OS are reported. (I) is monoclinicC2/c,a = 9.725(1),b = 20.031(3),c = 26.545(3) Å, β = 90.60(1)0,V = 5170 Å3,Z = 8; (II) is triclinic, $$P\bar 1$$ ,a = 10.206(1),b = 10.324(2),c = 14.425(2) Å, α = 101.68(1), β = 89.92(2), γ = 116.34(1)0,V = 1327 Å3,Z = 2; (III) is monoclinicP21/n,a = 17.832(5),b = 10.109(3),c = 17.901(5) Å, β = 111.93(2)0,V = 2993 Å3,Z =4. The structures were solved by direct methods and refined to final residuals of 0.045, 0.048, and 0.071, respectively. Thermal analysis of the complexes corroborates the crystallographic results.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01133229
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  • 175
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    X-ray structural study of a zinc(II) inclusion complex of a phenolate-pendant cyclam (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 12 (1992), S. 377-387 
    Details
    ISSN: 1573-1111
    Keywords: Charles Pedersen ; crown ethers ; phenol-pendant cyclam-zinc(II) complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular structure of phenol-pendant cyclam-zinc(II) complex,4a, has been determined by X-ray structure analysis. Crystals of4a · ClO4 · CH3OH (C16H27N4OZn · ClO4 · CH3OH) are monoclinic, space groupP21/nn, with four molecules in the unit cell of dimensionsa=31.198(2) Å,b=8.426(1) Å,c=8.214(1) Å, andβ=93.96(1)°. The structure was solved by the heavy atom method and refined anisotropically toR=0.044,R w=0.062 for 1551 independent reflections. The complex assumes a five-coordinate, square pyramidal geometry, where zinc(II) is surrounded by the cyclam moiety in a planar fashion with the pendant phenolate anion occupying an axial position. An extremely short Zn-O(phenolate) bond distance of 1.983(5) Å, in conjunction with the 0.288 Å displacement of Zn(II) above the cyclam N4 plane toward the phenolate, accounts for the extremely low pK a value of 5.8 for the pendant phenol. These facts about4a, in comparison with the previous findings for the Ni(II) (4b) and Cu(II) complexes (4c) with the same ligand, illustrate well the characteristics of zinc(II) ion coordination properties.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01053875
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  • 176
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    Synthesis and crystal structure of a new paramagnetic complex salt of diprotonated dioxocyclam with PtCl 2− 4 and water (1:1:1) (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 195-202 
    Details
    ISSN: 1573-1111
    Keywords: Dioxocyclam ; 5,7-dioxo-1,4,8,11-tetra-azacyclotetradecane ; platinum tetrachloride ; crystal structure ; paramagnetic properties of ionic stacked structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The paramagnetic complex salt of diprotonated dioxocyclam (1,11-dihydro-5,7-dioxo-1,4,8,11tetra-azacyclotetradecane), Pt(II) tetrachloride and water has been synthesized in strongly acidic medium and identified by X-ray structure analysis. The crystals of [(C10H22N4O2)2+(PtCl4)2−]·H2O are monoclinic, space groupP21 c,M r=585.23,a=9.516(1) Å,b=11.926(1) Å,c=16.622(2) Å,β=102.88(2)°,V=1839(1)Å3,Z=4,D x=2.114 g cm−3, λ(MoK α)=0.70930 Å,μ=83.1 cm−1,F(000)=1128,T=292 K,R=0.019 for 2808 observed reflections withI 〉 3δ(I). Alternating moieties of diprotonated dioxocyclam and a PtCl 2− 4 anion form columns running down the c axis. Water molecules are localized in the intercolumnar space and contribute to the extensive hydrogen bond network. The macrocycle conformation is characterized by two sequences of torsional angles, corresponding to two different subunits. The shorter sequence idealized as (-sc, ap, -ac, + ac, ap, +sc) [sc( ±60°), ac( ±120°), ap(180°)], describing the C pseudosymmetric part of the molecule, is centered on a -CH2 group between the two peptide O-C-N-H fragments. The opposite C pseudosymmetric subunit has a nearly (-sc, ac, -SC, ap)2 conformation. Pt is square planar coordinated by four Cl atoms, Pt-Clαve = 2.306(8) Å. The shortest Pt ... Pt distance is 7.200(1) Å.
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    URL: http://dx.doi.org/10.1007/BF01053643
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  • 177
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    A hydrogen bond between a calixarene (as host and its guest: Crystal and molecular structure of thep-t-butyldihomooxacalix[4]arene : Triethylamine (1 : 2) complex/clathrate (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 247-256 
    Details
    ISSN: 1573-1111
    Keywords: Inclusion compounds ; calixarene ; crystal structure ; hydrogen bonding ; amines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structure of thep-t-butyldihomooxacalix[4]arene triethylamine (1 : 2 complex has been determined by X-ray crystallography. Crystals are monoclinic, space groupCc,a = 22.821(3),b = 15.257(3),c = 16.365(2) Å,β = 97.44(1)°,V = 5650(1) Å3,Z = 4,D calc = 1.03 g cm−3. One triethylamine (Et3N) molecule has one of its ethyl groups pointing inside the cavity of a calixarene molecule; its nitrogen atom is directed exo to this calixarene molecule and is involved in a hydrogen bond with one of the hydroxy groups of a neighbouring calixarene molecule. This scheme leads to columns of alternating host and guest molecules. The other Et3N molecule is in the interhost space. This feature allows us to define the title compound as a complex/clathrate hybrid.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01045984
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  • 178
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    The crystal structure of the syn-proximal-5,11,17,23-tetra-tert-butyl-25,26-bis[(2-pyridylmethyl)oxy]-27,28-dihydroxy-calix[4]arene ethanol 1 : 1 Inclusion Complex (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 14 (1992), S. 349-356 
    Details
    ISSN: 1573-1111
    Keywords: 1,2-Dialkylated calix[4]arene ; crystal structure ; ethanol inclusion complex ; intramolecular hydrogen bonding patterns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the title compound (1 · C2H5OH) has been determined by single-crystal X-ray analysis and refined to anR-value of 0.074 for 2732 observed reflections [I 〉 2.0σ(I)]. Crystals are triclinic, space group P $$\bar 1$$ , witha = 13.6150(18),b = 13.7195(11),c = 16.5497(16) Å, α = 73.132(7),β = 66.165(9), γ = 65.580(8)° andZ = 2. Calix[4]arene (1) adopts a relatively open distorted cone conformation in the solid state, with two pendantsyn-proximal O-CH2-Py groups. The major conformation determining features in (1 · C2H5OH) are the presence of (a) an intramolecular O-H...O hydrogen bond between adjacent proximal phenolic oxygens, O...O 2.719(7) Å and (b) an intramolecular O-H...N hydrogen bond between a phenolic oxygen and a proximal pyridinyl nitrogen, O...N 2.810(8) Å. The intramolecular hydrogen bonding and the interplanar angles of 65.1(3) and 50.7(3)° between opposite aromatic rings facilitate the inclusion of an ethanol molecule within the calixarene cup.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01045993
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  • 179
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    Tribracchial lariat ethers: Syntheses, binding, and formation of an intramolecular macroring-sidearm complex in the absence of any cation (1992)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 12 (1992), S. 187-197 
    Details
    ISSN: 1573-1111
    Keywords: Cation binding ; crown ether ; crystal structure ; lariat ether ; synthesis ; triaza-18-crown-6
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Details of a new synthetic approach to 4,10,16-triaza-18-crown-6 (‘triaza-18-crown-6’) are reported, along with the preparation and binding properties of the following derivatives having the indicated sidearms: CH2C≡CH, CH2CH2OH, CH2CH2OCH3, COCH2OCH3,CH2COOCH2CH3, CH2C6H5, and CH2C6H4−2−NO2. A key intermediate in the synthesis of triaza-18-crown-6 is 4-N-toluenesulfonyl-1,7,13-trioxa-4,10,16-triazacyclooctadecane-9,17-dione. This compound is found by solid state structure analysis to fold to form an intramolecular, doubly-hydrogen bonded complex in which the two N-H protons interact with the two tosyl group oxygens. Details of the structure are reported.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01053861
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  • 180
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    Absolute configuration and conformation of the pure opioid antagonist (+)-2,9α-dimethyl-5-(m-hydroxyphenyl)morphan (1992)
    New York, NY [u.a.] : Wiley-Blackwell
    Chirality 4 (1992), S. 377-383 
    Details
    ISSN: 0899-0042
    Keywords: crystal structure ; molecular mechanics ; MM2-87 ; phenylmorphan ; phenyl-equatorial ; opioid ligand model ; μ-receptors ; K-receptors ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (+)-2,9α-Dimethyl-5-(m-hydroxyphenyl)morphan is the only phenylmorphan analog whose affinity for opioid K-receptors is greater than its affinity for opioid κ-receptors. Pharmacologically, the compound is a pure opioid antagonist devoid of agonist activity in in vivo assays of antinociception. The absolute configuration of the compound has been determined to be (1R,5S,9R) from an X-ray crystallographic study of the chloride salt. Thus, the absolute configuration corresponds to that of the atypical opioid agonist (-)-phenylmorphan while the weak atypical agonist (-)-2,9α-dimethyl-5-(m-hydroxyphenyl)morphan corresponds to the potent morphine-like (+)-phenylmorphan. The preferred orientations of the phenyl ring for the two stereoisomers were determined using the molecular mechanics program MM2-87 and found to vary from that of the two parent compounds. The atypical properties of the two 9α-methyl analogs is consistent with an opioid ligand model which proposes that morphine-like properties require a particular range of phenyl orientations. There was good agreement between the structure obtained from X-ray crystallography and computed with the MM2-87 program. © 1992 Wiley-Liss, Inc.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chir.530040608
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  • 181
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    Lamellar and whisker single crystals of poly(2,6-oxynaphthoate) (1992)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 30 (1992), S. 1469-1482 
    Details
    ISSN: 0887-6266
    Keywords: poly(2,6-oxynaphthoate) ; crystal structure ; whiskers ; lamellae ; unit cell ; transitions ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Electron diffraction from single crystal lamellae and whiskers of poly(2,6-oxynaphthoate) reveals the presence of at least 3 unit cells. The equatorial reflections in the patterns from the whiskers correspond to the dominant (phase I) hk0 diffraction pattern from the lamellae; phase I is monoclinic with 2 chemical repeats per physical repeat. The intensity distributions in the hk0 patterns of phase I and II resemble those of the same phases in poly(p-oxybenzoate). The hk0 reflections of phase III suggest a common internapthalene unit spacing, but variable lateral (and possibly axial) shifts; apparently related orthorhombic and monoclinic patterns, with variable γ*, are observed. At elevated temperature, above the crystalliquid crystal transition (ca. 330°C), quadrant reflections are retained; the change in the hk0 pattern from any given crystal is gradual, extending over some 40°C. Above the liquid crystal-liquid crystal transition (ca. 460°C) the pattern can be interpreted in terms of nematic or possibly smectic A packing. © 1992 John Wiley & Sons, Inc.
    Additional Material: 19 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/polb.1992.090301306
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  • 182
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    Ein neues Syntheseverfahren für die Wolframbronze Cs0,29WO3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 95-98 
    Details
    ISSN: 0044-2313
    Keywords: Tungsten bronze, Cs0.29WO3 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Novel Synthetic Access to the Tungsten Bronze Cs0.29WO3 and its Crystal StructureThe hexagonal tungsten bronze Cs0.29WO3 was obtained in form of black, prismatic crystal by the reduction of WO3 with molten cesium iodide at 700°C. Its crystal structure was determined by X-ray diffraction (399 unique observed reflexions, R = 0.058). Crystal data: a = 741.2(3), c = 760.0(5) pm, space group P6322, Z = 6. It corresponds to the known structure of hexagonal tungsten bronzes, having tungsten atoms displaced from the octahedra centres by 11.9 pm and with three different W—O bond lengths (198, 191, 187 pm). The WO6 octahedra are slightly titled mutually.
    Notes: Bei der Reaktion von WO3 in einer Caesiumiodid-Schmelze bei 700°C entsteht die hexagonale Wolframbronze Cs0.29WO3 in Form schwarzer, hexagonal-prismatischer Kristalle. Ihre Struktur wurde durch Röntgenbeugung bestimmt (399 beobachtete unabhängige Reflexe, R = 5,8%). Kristalldaten: a = 741,2(3), c = 760,0(5) pm, Raumgruppe P6322, Z = 6. Es handelt sich um die bekannte Struktur der hexagonalen Wolframbronzen mit Wolframatomen, die aus den Oktaedermitten um 11,9 pm herausgerückt sind und mit drei verschiedenen W—O-Bindungslängen (198, 191, 187 pm). Die WO6-Oktaeder sind leicht gegeneinander verkippt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090318
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  • 183
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    Röntgenstrukturanalyse des 1,3-Bis(diethylamino)-1,3-dibenzyl-2,4-diphenyl-1λ5, 3λ5-diphosphets (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 99-102 
    Details
    ISSN: 0044-2313
    Keywords: Diphosphete ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: X-Ray Crystal Structure Determination of 1,3-Bis(diethylamino)-1,3-dibenzyl-2,4-diphenyl-1λ5, 3λ5-diphospheteBenzylidene-diethylamino-benzylfuorophosphorane, 1, reacts with lithium bis(trimethylsilyl)amide to give the title compounds 2 and 1-diethylamino-2,3-diphenylphosphirane, 3. Only one of the stereoisomers of 2 is formed in which the two benzyl groups are located on the same side of the planar four-membered ring. 2 crystallizes in the monoclinic space group P21/n.
    Notes: Benzyliden-diethylamino-benzylfuorphosphoran, 1, reagiert mit Lithium-bis(trimethylsilyl)-amid zur Titelverbindung 2 und 1-Diethylamino-2,3-diphenylphosphiran, 3. Von 2 wird nur das Stereoisomer gebildet, bei dem die beiden Benzylgruppen auf der gleichen Seite des ebenen viergliedrigen Rings angeordnet sind. 2 kristallisiert in der monoklinen Raumgruppe P21/n.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090319
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    Structures of Xenon Oxygen Compounds (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 153-156 
    Details
    ISSN: 0044-2313
    Keywords: Xenon oxygen compounds ; Xe(OTeF5)4 ; O2Xe(OTeF5)2 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturen von Xenon-Sauerstoff-VerbindungenDie Struktur des lange bekannten Xe(OTeF5)4 wurde durch die Kristallstrukturanalyse aufgeklärt. Das Xenonatom ist von vier Sauerstoffatomen in einer regelmäßigen quadratisch planaren Anordnung umgeben. O2Xe(OTeF5)2 ensteht gemäß O — Xe(OTeF5)4 → O2Xe(OTeF5)2 + F5Te—O—TeF5. Die Struktur - wiederum mit Hilfe der Röntgenstrukturanalyse bestimmt - zeigt das Xenonatom in einer sehr verzerrten tetraedrischen oder pseudo-trigonal bipyramidalen Umgebung. Das Elektronenpaarabstoßungsmodell versagt hier bei der Erklärung der Feinheiten dieser Struktur.
    Notes: The structure of long known Xe(OTeF5)4 is established by x-ray crystallography. The xenon atom is surrounded by four equidistant oxygen atoms in a square planar manner. O2Xe(OTeF5)2 is formed according to OXe(OTeF5)4 → O2Xe(OTeF5)2 + F5TeOTeF5, Its structure, again established by x-ray crystallography, shows a very distorted tetrahedral or pseudo-trigonal bipyramidal xenon environment. The electron pair repulsion models fails here in explaining the details of this geometry.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926090327
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  • 185
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    Synthese und Kristallstruktur von Hydronium-tris-ethylendiamin-cobalt(rhodium)-μ-trichloro-nonachlorotrirhenat(II)-chlorid, H3O[MEn3][Re3Cl12]Cl (M=Co, Rh) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 91-95 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium complexes ; 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 Hydronium-tris-ethylenediamine-cobalt(rhodium)-μ-trichloro-nonachlorotrirhenate(III)-chloride, H3O[MEn3][Re3Cl12]Cl (M=Co, Rh)The chlorides H3O[MEn3][Re3Cl12]CI (M = Co, 1; Rh, 2) crystallize from hydrochloric acid solutions of ReCl3 and MEn3 · 3H2O as deep red hexagonal columns. They are isotypic and crystallize with the hexagonal system (P6, Z = 1; 1: a = 1010.87(3); c = 794.30(4) pm, R = 0.023, Rw = 0.016; 2: a = 1018.58(3); c = 794.74(4) pm, R = 0.026, Rw = 0.018). The anions [Re3Cl12]3- are connected via H3O+ cation (C.N. 3). The large channels that run in the [001] direction contain, alternatively, the cations [MEn3]3+ and the lonesome Cl--anions
    Notes: Die Chloride H3O[MEn3][Re3CI12]CI(M = Co, 1; Rh, 2) Kristallisieren in Form tiefroter hexagonaler Säulen aus salzsauren Lösungen von ReCI3 und MEn3CI3 · 3H2O aus. Sie sind isotyp und Kristallisieren im hexagonalen System (P6, Z = 1; 1: a = 1010,87(3); C = 794,30(4)pm, Rw = 0,016; : a = 1018,58(3); c = 794,74(4)pm, R = 0,026, Rw = 0,018). Die Anionen [ Re3Cl12]3- werden über H3O+ (C.N. 3) verknüpft; in die entstehenden Kanäle sind längs [001] abwechselnd die Kationen [MEn3]3+ und die einsamen Cl--Ionen eingelagert.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926070115
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  • 186
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    Neue Untersuchungen an quaternären Fluoriden (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 607 (1992), S. 121-123 
    Details
    ISSN: 0044-2313
    Keywords: Quaternary fluorides ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Investigations on Quaternary FluoridesFor the first time the quaternary fluorides M12MIILnF7 (M1 = Na, Ag; MII = Ca, Cd; Ln = Er—Lu) had been prepared and examined with with X-ray diffraction. All these compounds crystallize in a cubic face-centered lattice. Colourless single crystals of Na2CdYbF7 were obtained and the structure was determined. Na2CdYbF7 crystallizes in the space group Fm3M-O5h, No. 225. The single-crystal diffraction data refer to a Defect-Fluorite-Structure. The R-value for 332 observed (29 independend) reflections is 2.2%.
    Notes: Erstmals wurden die quarternären Fluoride M12M11LnF7 (M1 = Na, Ag; M11 = Ca, Cd; Ln = Er—Lu) dargestellt und röntgenographisch untersucht. Alle Verbindungen kristallisieren kubisch flächenzentriert. An farblosen Einkristallen von Na2CdYbF7 wurde eine Strukturbestimmung durchgeführt. Na2CdYbF7 kristallisiert in der Raumgruppe Fm3m-O5h, Nr. 225. Die Meßwerte verweisen auf eine Defekt-Fluorit-Struktur. Der R-Wert fär 332 beobachtete (29 unabhängige) Röntgenreflexe beträgt 2,2%.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19926070120
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    Zur Addition von Übergangsmetallhalogeniden an Acetylacetonate zweiwertiger Metallionen (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 65-72 
    Details
    ISSN: 0044-2313
    Keywords: Transition metal halides acetylacetonate complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Addition of Transition Metal Dihalides to Acetylacetonates of Divalent Metal IonsTransition metal dihalides aMIIX2 (FeCl2, CoCl2 NiBr2 etc.) are added by the chelates MII(acac)2 under formation of binuclear complexes (THF)2MII(acac)2(aMIIX2). The octahedral and the tetrahedral centre of these compounds are connected by tridentate oxygen atoms of the two acetylacetonato ligands which are simultaneously included in four-membered rings (MIIO2aMII). The addition is combined with a deformation of the octahedral centre, as a prerequisite of a closest package of the atoms within the MIIO2aMII-ring.In the trinuclear complex (THF)2Ni(acac)2(HgCl2)2 III the interaction between the three coordination centres is weak. No structural change of the octahedral centre (THF)2Ni(acac)2 is found, but the HgCl2-groups diverge slightly from linearity (Cl—Hg—Cl 171.1°).No binuclear complexes with a central ion of the oxidation state III in the octahedral centre were obtained. One reason is the lowered donor strength of the bidentate Lewis base function of the octahedral centre [(THF)2Mn+(acac)2]n-2 with M+3 as a centralatom. Reacting systems with di- and trivalent ions prefer ionic complexes, as it is shown by the formation of [(THF)2V(acac)2][(THF)CoCl3] IV from VCl3 and Co(acac)2.The crystal structures of (THF)2Co(acac)2CoCl2II and [(THF)2V(acac)2][(THF)CoCl3] IV were determined by x-ray diffraction. II: orthorhombic-primitive; space group P212121, Z = 4; a = 967.4(2), b = 1453.4(3), c = 1715.9(4) pm; R = 0.049 for 3084 observed reflections. IV: triclinic; space group P1, Nr. 2; Z = 2; a = 871,5(2), b = 930,6(3), c = 1865,6(6) pm; α = 101,70(2), b̃ = 92,45(2), γ = 91,06(2)°; R = 0,060 für 4221 observed reflections.
    Notes: Bis(acetylacetonate) von Magnesium(II), Cobalt(II) oder Nickel(II) addieren Dihalogenide wie FeCl2, CoCl2 oder NiBr2 (aMIIX2) unter Bildung binuklearer Komplexe (THF)2MII(acac)2(aMIIX2), in denen ein oktaedrisches und ein tetraedrisches Zentrum über zwei dreibindige Sauerstoffatome der Acetylacetonatliganden miteinander verknüpft sind (Bildung eines viergliedrigen MIIO2aMII-Ringes). Die Addition ist mit einer Deformation des oktaedrischen Zentrums verbunden, die eine dichte Packung der vier Atome des MIIO2aMII-Ringes ermöglicht.Im trinuklearen Komplex (THF)2Ni(acac)2(HgCl2)2 III bleibt die Wechselwirkung zwischen den drei Koordinationszentren gering. Das oktaedrische Zentrum (THF)2Ni(acac)2 wird strukturell nicht verändert, allerdings weichen die beiden HgCl2-Bausteine (Valenzwinkel 171,1°) von der Linearität ab.Es gelang nicht, binukleare Komplexe mit einem Zentralatom der Oxidationsstufe III im oktaedrischen Zentrum darzustellen. Ein Grund dafür ist die verringerte Donorstärke der zweizähligen Lewisbasen-Funktion im oktaedrischen Zentrum [(THF)Mn+(acac)2]n-2 für M+3 als Zentralion. Reaktive Systeme mit zwei- und dreiwertigen Kationen weichen auf die Seite von ionischen Komplexen aus, wie die Bildung von [(THF)2V(acac)2][(THF)CoCl3] IV aus VCl3 und Co(acac)2 zeigt.Die Kristallstrukturen von (THF)2Co(acac)2CoCl2 II und [(THF)2V(acac)2][(THF)CoCl3] IV wurden durch Röntgenbeugung bestimmt.II: orthorhombisch primitiv, Raumgruppe P212121, Z = 4; a = 967,4(2), b = 1453,4(3), c = 1715,9(4) pm; R = 0,049 für 3084 beobachtete Reflexe.IV: triklin, Raumgruppe P1, Nr.2; Z = 2; a = 871,5(2), b = 930,6(3), c = 1865,6(6) pm; α = 101,70(2), b̃ = 92,45(2), γ = 91,06(2)°; R = 0,060 für 4221 beobachtete Reflexe.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926140813
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    Die Kristallstrukturen von Me3SiI · β-Picolin und Me3SiI · γ-Picolin Vergleich der Lewis-Basen Pyridin, β-Picolin und γ-Picolin (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 145-150 
    Details
    ISSN: 0044-2313
    Keywords: Iodinetrimethylsilane · β-picoline ; -.γ-picoline ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Me3SiI · β-Picoline and Me3SiI · γ-Picoline A Comparison between the Lewis-Bases Pyridine, β-Picoline, and γ-PicolineThe reaction of Iodinetrimethylsilane with β- und γ-Picoline (Pic) leads to solid 1 : 1 compounds Me3SiI · β-Picoline 1, Me3SiI · γ-Picoline 2. The reaction was performed at room temperature. Yellow single crystals were obtained by sublimation. Single crystal X-ray investigations confirm that both compounds are ionic [Me3SiPic]+I-. The comparison of β-Picoline with γ-Picoline and Pyridine (Py) demonstrates that the presence of a methyl group and also its position has no significant influence on the Si—N bond length in compound 1, 2 and on the adduct Me3SiI · Py.
    Notes: Iodtrimethylsilan reagiert mit β- und γ-Picolin (Pic) bei Raumtemperatur zu festen 1 : 1 Addukten (M3SiI · β-Picolin 1, Me3SiI · γ-Picolin 2), die durch Sublimation leicht gelblich gefärbte Einkristalle bilden. Die Röntgenstrukturanalyse beider Verbindungen beweist eine ionische Struktur des Typs [Me3SiPic]+ I-. Der Vergleich von β-Picolin mit γ-Picolin und Pyridin (Py) zeigt, daß die Anwesenheit einer Methylgruppe und auch deren Position keinen signifikanten Einfluß auf die Si—N-Bindungslänge in Verbindung 1, 2 und dem Addukt Me3SiI · Py hat.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926100124
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    Hydrate schwacher und starker Basen. VII. Zum System Caesiumhydroxid-Wasser: Die Kristallstrukturen von CsOH · 2H2O und CsOH · 3H2OHerrn Professor Joseph Grobe zum 60. Geburtstage am 2. November 1991 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 608 (1992), S. 123-130 
    Details
    ISSN: 0044-2313
    Keywords: Cesium hydroxide hydrates ; 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. VII. Concerning the System Cesium Hydroxide - Water: The Crystal Structures of CsOH · 2H2O and CsOH · 3H2OIn the context of structural studies of hydrates of the alkali metal hydroxide the crystal structure of CsOH · 2H2O and CsOH · 3H2O have been determined for the first time. The diffractometer data, obtained at -150 · C,made it possible to locate and refine also all the H-atoms. The dihydrate was found to probably form only one phase, melting incongruently at 2,5 · C. It is orthorhombic with space group Pca21 and Z = 8 formula units per unit cell. The lattice constants are a = 13.238, b = 6.747 and c = 9.121 A. With 1870 independent observed reflection a final R value of 0.013 was obtained. The trihydrate, melting congruently et -5.5 ·C, is monoclinic with space group P21/n,Z = 4 and lattice constants a = 8.637, b = 5.984, c = 10.061 Å and ß = 96.57 ·. With 2098 independent observed reflection the final R is 0.026. In both hydrate structures there are no simple characteristic coordination polyhedra for the cations; in each case it is rather the hydrogen-bonded and fully ordered anionic water structure which shows up as the determining building principle. Both these water structures are altogether three-dimensional, but primarily contain layers. The anionic layers are formed by condensation of small and medium rings, namely four-, five- and seven-membered rings in CsOH · 2H2O and four-, five- and six membered ones in CsOH · 3H2O. They are linked together by one set each of extra H2O molecules between the layers as well as by the Cs+ ions.
    Notes: In Zusammenhang mit Untersuchungen zur Struktur von Hydraten der Alkalimetallhydroxide wurden die Kristallstrukturen von CsOH · 2H2O und CsoH · 3H2O erstmalig bestimmt. Die bei - 150°C erhaltenen Diffraktometerdaten erlaubten dabei auch die Lokalisierung und Verfeinerung Sämtlicher H-Atome. Das nach eigenen Untersuchungen wahrscheinlich nur einphasig vorliegende Dihydrat schmilzt inkongruent bei 2,5°C und kristallisiert orthorhombisch mit der Raumgruppe Pca21 und Z = 8 Formeleinheiten pro Elementarzelle sowie den Gitterkonstanten a = 13,238, b = 6,747 und c = 9,121 ß. Mit 1870 unabhängigen beobachteten Reflexen wurde ein abschließender R-Wert von 0,013 erreicht. Das bei - 5,5°C kongruent schmelzende Trihydrat ist monoklin mit der Raumgruppe P21/n und Z = 4. Die Gitterkonstanten betragen a = 8,637, b = 5,984, c = 10,061 A und ß = 96,57°. Mit 2098 unabhängigen beobachteten Reflexen liegt der abschließende R-Wert bei 0,026. In beiden Hydratstrukturen gibt es keine einfachen charakteristischen Koordinationspolyeder für die Kationen; vielmehr wird jeweils die durch H-Brücken gebildete und vollständig geordnete anionische Wasserstruktur zum bestimmenden Bauprinzip. Beide Wasserstrukturen sind insgesamt dreidimensional, enthalten primär aber Schichten. Die aus Kondensierten Kleinen und mittleren Ringen, nämlich Vier-, Fünf - und Siebenringen (CsOH · 2H2O) bzw. Vier-, Fünf- und Sechsringen (CsOH · 3H2O), bestehenden anionischen Schichten werden jeweils über einen Satz weiterer H2O-Moleküle zwischen den Schichten sowie über die Cs+-Ionen miteinander verknüpft.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926080218
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    Bis(triphenylphosphaniminato)niobtrichlorid, [NbCl3(NPPh3)2], ein Komplex mit fünffach koordiniertem NiobProfessor Osvald Knop zum 70. Geburtstage am 11. Juli 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 7-10 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane iminato complex of niobium ; synthesis ; IR spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bis(triphenylphosphorane-iminato)niobium Trichloride, [NbCl3(NPPh3)2], a Complex with Coordination Number Five at the Niobium AtomThe title compound has been prepared from niobium pentachloride with Me3SiNPPh3 in acetonitrile solution, forming colourless, moisture sensitive crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. [NbCl3(NPPh3)2] crystallizes monoclinically in the space group Cc with four formula units per unit cell, 3682 observed, unique reflections, R = 0.042%. Lattice dimensions at 20°C: a = 1025.1(2); b = 1870.6(6); c = 1832.5(5) pm, β = 91.83(2)°. The niobium atom of the complex is coordinated in a distorted trigonal bipyramidal fashion, while the nitrogen atoms of the two phosphorane iminato ligands are in equatorial position along with one chlorine atom. NbN and PN distances accord with double bonds; with a mean value of 242.0 pm the Nb—Cl distances are remarkably long.
    Notes: Die Titelverbindung entsteht in Form farbloser, feuchtigkeitsempfindlicher Kristalle bei der Reaktion von Niobpentachlorid mit Me3SiNPPh3 in Acetonitrillösung. Sie wird durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert. [NbCl3(NPPh3)2] kristallisiert monoklin in der Raumgruppe Cc mit vier Formeleinheiten pro Elementarzelle, 3682 beobachtete unabhängige Reflexe, R = 4,2%. Gitterabmessungen bei 20°C: a = 1025,1(2); b = 1870,6(6); c = 1832,5(5) pm, β = 91,83(2)°. In dem Komplex ist das Niobatom verzerrt trigonal-bipyramidal koordiniert, wobei die N-Atome der beiden Phosphaniminatoliganden zusammen mit einem Chloratom äquatorial angeordnet sind. NbN- und PN-Abstände entsprechen Doppelbindungen; die Nb—Cl-Abstände sind mit dem Mittelwert von 242,0 pm auffällig lang.
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    URL: http://dx.doi.org/10.1002/zaac.19926150902
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    Die Kristallstruktur von Na2NiAlF7 - ein Beitrag zum Problem der wahren Raumgruppe orthorhombischer WeberiteProfessor Osvald Knop zum 70. Geburtstage am 11. Juli 1992 gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 11-15 
    Details
    ISSN: 0044-2313
    Keywords: Weberite ; crystal structure ; nickel aluminium fluoride ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Na2NiAlF7  -  a Contribution to the Problem of the True Space Group of Orthorhombic WeberitesThe X-ray single crystal structure determination of the orthorhombic weberite Na2NiAlF7 (a = 707.4(2), b = 1003.8(2), c = 731.5(1) pm; Z = 4) was performed in space group Imma, after all reflections hk0 with h(k) = 2n + 1 could be eliminated, as they proved simulated by Renninger effect and/or λ/2 reflections. The alternative space groups Imm2 resp. I212121 of former weberite structure determinations thus became obsolete. The refinement using 880 independent reflections ended at wR = 0.0232. The resulting average distances within the framework of octahedra are Ni—F = 197.3, Al—F = 180.4 pm.
    Notes: Die Röntgen-Einkristallstrukturbestimmung des orthorhombischen Weberits Na2NiAlF7 (a = 707,4(2), b = 1003,8(2), c = 731,5(1) pm; Z = 4) wurde in der Raumgruppe Imma vorgenommen, nachdem alle Reflexe hk0 mit h(k) = 2n + 1 eliminiert werden konnten, weil sie sich durch Renninger-Effekt und/oder λ/2-Reflexe als vorgetäuscht erwiesen. Damit wurden die alternativen Raumgruppen Imm2 bzw. I212121 früherer Weberit-Strukturbestimmungen obsolet. Die Verfeinerung mit 880 unabhängigen Reflexen schloß ab mit wR = 0,0232. Die resultierenden Mittelwerte für die Abstände im Oktaedernetz betragen Ni—F = 197,3 pm, Al—F = 180,4 pm.
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    URL: http://dx.doi.org/10.1002/zaac.19926150903
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    Molekül- und Kristallstruktur von Ytterbium(III)-triaqua-trinitrat, Yb(H2O)3(NO3)3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 16-18 
    Details
    ISSN: 0044-2313
    Keywords: Ytterbium nitrates ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Molecular and Crystal Structure of Ytterbium(III)-triaqua-trinitrate, Yb(H2O)3(NO3)3Yb(H2O)3(NO3)3 crystallizes from a concentrated solution of Yb2O3 in nitric acid in a vacuum desiccator at ambient temperature as colourless single crystals. The crystal structure was determined from single crystal four-circle diffractometer data (R3, Z = 6, a = 1175.5(1), c = 1117.7(2) pm, Vm = 134.25 cm3/mol, R = 3.0%, Rw = 2.9%). The structure may be viewed at as a heavily compressed packing of [Yb(H2O)3(NO3)3] molecules. Yb3+ is coordinated by three bidentate nitrate ligands and three water molecules so that a tricapped trigonal prism (C.N. 9) of oxygen atoms results as the coordination polyhedron.
    Notes: Yb(H2O)3(NO3)3 kristallisiert aus einer konzentrierten Lösung von Yb2O3 in Salpetersäure im Vakuumexsikkator bei Raumtemperatur in Form farbloser Einkristalle aus. Die Kristallstruktur wurde aus Einkristall-Vierkreis-Diffraktometer-Daten bestimmt (R3, Z = 6, a = 1175,5(1), c = 1117,7(2) pm, Vm = 134,25 cm3/mol, R = 3,0%, Rw = 2,9%). Sie kann als stark gestauchte Kugelpackung von [Yb(H2O)3(NO3)3]- Molekülen aufgefaßt werden. In diesen ist Yb3+ von drei zweizähnigen Nitratliganden und drei Wassermolekülen in Form eines dreifach bekappten trigonalen Prismas (C. N. 9) von Sauerstoffatomen umgeben.
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    URL: http://dx.doi.org/10.1002/zaac.19926150904
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    Chelate von Chinolin-8-ol-Derivaten. XIIXI. Mitt. s. [1].. Die Kristall- und Molekülstruktur von Bis(7-isopropylchinolin-8-olato)nickel(II) (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 39-42 
    Details
    ISSN: 0044-2313
    Keywords: Bis(7-isopropyl-8-quinolinato)nickel(II) ; crystal structure ; association of nickel 8-quinolates ; steric hindrance ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chelates of 8-Quinolinol Derivatives. XII. Crystal and Molecular Structure of Bis(7-isopropyl-8-quinolinato)nickel(II)The crystal and molecular structure of bis(7-isopropyl-8-quinolinato)nickel(II) was determined by X-ray diffraction. The structure is monoclinic with the space group P21/n (Z = 2, 1403 observed independent reflections, R = 0.049. Lattice dimensions at 20°C: a = 1328.3(5) pm, b = 632.8(2) pm, c = 1330.0(5) pm, β = 112.99(3)°). The coordination of the nickel atom is planar with the quinoline rings in trans position.
    Notes: Die Kristallstruktur von Bis(7-isopropylchinolin-8-olato)nickel(II) wurde durch eine Röntgenkristallstrukturuntersuchung bestimmt. Es liegt ein monoklines Kristallsystem mit der Raumgruppe P21/n vor (Z = 2, beobachtete unabhängige Reflexe 1403, R = 4,9%, Gitterabmessungen bei 20°C: a = 1328,3(5) pm, b = 632,8(2) pm, c = 1330,0(5) pm, β = 112,99(3)°). Das Nickelatom ist planar koordiniert mit den beiden Chinolinringen in trans-Stellung.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926150908
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    Zur Kristallstruktur von Ba2ZnO3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 17-20 
    Details
    ISSN: 0044-2313
    Keywords: Barium ; zinc ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structure of Ba2ZnO3Single crystals of Ba2ZnO3 were prepared by solid state reaction. It crystallizes monoclinic: space group C62h — C12/c1; a = 5.833; b = 11.376; c = 12.585 Å; β = 93.63°; Z = 8. The crystal structure is characterised by 1∞[ZnO3] chains along [100]. They are connected by Ba2+ in seven fold oxygen coordination.
    Notes: Ba2ZnO3 wurde durch Festkörperreaktion in einkristalliner Form dargestellt. Es kristallisiert in der Raumgruppe C62h — C12/c1; a = 5,833; b = 11,376; c = 12,585 Å, β = 93,63°; Z = 8. Die Kristallstruktur ist durch 1∞[ZnO3]-Ketten längs [100] gekennzeichnet. Diese werden durch Ba2+ (siebenfach durch O2- koordiniert) verknüpft.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926120104
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  • 195
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    Ein neues Oxometallat mit Mangan(II): Ba5Mn4Nd8O21 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 21-24 
    Details
    ISSN: 0044-2313
    Keywords: Barium ; manganese ; neodymium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On a New Oxometallate of Manganese (II): Ba5Mn4Nd8O21Single crystals of Ba5Mn4Nd8O21 were prepared for the first time by CO2-Laser technique using H2-atmosphere. It was investigated by a single crystal X-ray diffractometer study. Ba5Mn4Nd8O21 crystallizes with tetragonal symmetry space group: C54h—I4/m; a = 14.2104 Å; c = 5.8581 Å; Z = 2. Mn2+ is found in square pyramids of oxygen.
    Notes: Ba5Mn4Nd8O21 wurde erstmals mit CO2-Lasertechnik in H2-Atmosphäre dargestellt und an Einkristallen röntgenographisch untersucht. Es kristallisiert tetragonal in der Raumgruppe C54h—I4/m; a = 14,2104 Å; c = 5,8581 Å; Z = 2. Mn2+ liegt in tetragonal pyramidaler Sauerstoffkoordination vor.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926120105
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  • 196
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    Synthese und Strukturuntersuchungen von Iodocupraten(I). XV Iodocuprate(I) mit solvatisierten Kationen: [Li(CH3CN)4]1∞[Cu2I3] und [Mg{(CH3)2CO}6][Cu2I4] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 45-50 
    Details
    ISSN: 0044-2313
    Keywords: Iodocuprates(I) ; solvated cations ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Investigations of Iodocuprates(I). XV Iodocuprate(I) with Solvated Cations: [Li(CH3CN)4]1∞[Cu2I3] and [Mg{(CH3)2CO}6][Cu2I4][Li(CH3CN)4]1∞[Cu2I3] 1 and [Mg((CH3)2CO)6][Cu2I4] 2 were prepared by reactions of CuI with LiI in acetonitrile and of CuI with MgI2 in acetone. 1 crystallizes orthorhombic, Pnma, a = 552.7(2), b = 1258.8(8), c = 2516(1) pm, z = 4. [Li(CH3CN)4]+ cations are located between rod packings of CuI4 tetrahedra double chains 1∞ [(CuI2/2I2/4)2]- parallel to the axis. Short intermolecular anion/cation contacts were observed. The crystal structure of 2 (monoclinic, P21/n, a = 1840(2), b = 1059.2(2), c = 1879(2)pm, β = 112.94(4)°, z = 4) is built up by [Mg((CH3)2CO)6]2+ cations forming a simple hexagonal sphere packing. The binuclear anions [Cu2I4]2- occupy holes in the trigonal prismatic channels formed by the cations.
    Notes: [Li(CH3CN)4]1∞[Cu2I3] 1 und [Mg((CH3)2CO)6][Cu2I4] 2 wurden durch Umsetzung von CuI mit LiI in Acetonitril bzw. von CuI mit MgI2 in Aceton dargestellt. 1 kristallisiert orthorhombisch, Pnma, a = 552,7(2), b = 1258,8(8), c = 2516(1) pm, z = 4. Zwischen Stabpackungen von CuI4-Tetraederdoppelketten 1∞[(CuI2/2I2/4)2]- parallel zur a-Achse sind [Li(CH3CN)4]+ -Kationen unter Ausbildung kurzer, intermolekularer Anionen-Kationen-Kontakte eingelagert. In der Kristallstruktur von 2 (monoklin, P21/n, a = 1840(2), b = 1059,2(2), c = 1879(2) pm, β = 112,94(4)°, z = 4) sind [Mg((CH3)2CO)6]2+ -Kationen in der Art einer hexagonal einfachen Kugelpackung angeordnet. In die dabei gebildeten, trigonal prismatischen Kanäle sind die zweikernigen Anionen [Cu2I4]2- eingebaut.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926120109
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  • 197
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    Vorstufen für polymere Silazane mit Fluoralkyl-Seitenketten und ihr Kondensationsverhalten (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 101-106 
    Details
    ISSN: 0044-2313
    Keywords: (Trifluoroethyl)aminosilane ; silane tetramin; alkylsilazalane ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preliminary Stages of Polymeric Silazanes with Fluoroalkyl Side Chains and their Condensation BehaviourTetrakis(2,2,2-trifluoroethyl)aminosilane has been synthesized by aminolysis of silicon tetrachloride with 2,2,2-trifluorethylamine. The characterisation of the silane tetramine was carried out spectroscopically and by X-ray-methods. The thermal condensation has been investigated between 60°C and 300°C. At 300°C the formation of oligospirocycloorganoazanes was observed which have been identified spectroscopically. The new silane tetramine reacts with trimethylalumina in toluene. The product has been characterized by crystal structure analysis to be a dimeric (C18H26N8F24Si2Al2). (P1; a = 920.39(9), b = 943.32(2), c = 1235.4(1) pm, α = 68.8(7)°, β = 86.9(4)°, γ = 62.6(4)°, Z = 1, 3923 independent reflections; R = 0.059, Rw = 0.054)
    Notes: Tetrakis[(2,2,2-trifluorethyl)amino]-silan wurde durch Aminolyse von Siliciumtetrachlorid mit 2,2,2-Trifluorethylamin dargestellt, spektroskopisch und röntgenographisch charakterisiert, sowie das thermische Kondensationsverhalten im Bereich von 60 - 300°C untersucht. Bei 300°C konnte die Bildung von Oligospirocyclo-silaorganoazanen massenspektrometrisch nachgewiesen werden. Das neu erhaltene Silantetramin wurde bei 80°C mit Trimethylaluminium im Verhältnis 1 : 1 in Toluol umgesetzt. Nach der Kristallstrukturanalyse liegt das erhaltene Alkylsilazalan im Kristall als Dimeres C18H26N8F24Si2Al2 vor. (P1; a = 920,39(9), b = 943,32(2), c = 1235,4(1) pm, α = 68,8(7)°, β = 86,9(4)°, γ = 62,6(4)°; Z = 1, 3923 unabhängige Reflexe, R = 0,059, Rw = 0,054)
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926120117
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  • 198
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    Korrektur zur Kristallstruktur von „Cs4PbO3“ und die Strukturverwandtschaft zwischen den Modifikationen von Cs4PbO4 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 143-148 
    Details
    ISSN: 0044-2313
    Keywords: Caesium tetraoxoplumbate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Correction of the Crystal Structure of “Cs4PbO3” and the Structural Relationship between the Modifications of Cs4PbO4The compound that has been described as Cs4PbO3 really is Cs4PbO4. It does not crystallize in the space group P21, as assumed, but in P21/c. The observed fictitiuous violation of the extinction law for the c glide plane is due to twinning. The structure was refined using the original data as well as new data from an untwinned crystal. The denomination β-Cs4PbO4 is used to distinguish this structure from another known modification (α-Cs4PbO4). Both structures, α-Cs4PbO4 and β-Cs4PbO4, can be derived from the sphere packing of γ-plutonium when certain voids in its packing are occupied with oxygen atoms.
    Notes: Bei der früher als Cs4PbO3 beschriebenen Substanz handelt es sich tatsächlich um Cs4PbO4. Dieses kristallisiert nicht, wie angenommen, in der Raumgruppe P21, sondern in P21/c. Die beobachtete scheinbare Verletzung des Auslöschungsgesetzes für die c-Gleitspiegelebene ist auf Verzwillingung zurückzuführen. Die Struktur wurde sowohl mit den ursprünglichen Daten wie auch mit neuen Daten eines unverzwillingten Kristalls verfeinert. Die Bezeichnung β-Cs4PbO4 dient zur Unterscheidung von einer bereits bekannten Modifikation (α-Cs4PbO4). Beide Strukturen, α-Cs4PbO4 und β-Cs4PbO4, lassen sich von der des γ-Plutoniums ableiten, wenn bei dieser bestimmte Lücken mit Sauerstoffatomen besetzt werden.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926120124
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    Darstellung und Kristallstruktur von LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) und thermischer Abbau zu LnBr3 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 45-48 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanoide bromoaluminates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) and Thermal Decomposition to LnBr3LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) was prepared in crystalline form for the first time. The crystal structures of LaAl3Br12, PrAl3Br12, and NdAl3Br12 were determined on single crystals by X-ray methods. The isotypic compounds crystallize with trigonal symmetry, space group P 3112, Z = 3. A structural comparison to lanthanoide chloroaluminates of equal composition is given and thermal decomposition of LnAl3Br12 (Ln = Nd) to the corresponding lanthanoide tribromide is described.
    Notes: Die Bromide LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) wurden erstmals in kristalliner Form dargestellt und die Kristallstrukturen von LaAl3Br12, PrAl3Br12 anhand von röntgenographischen Einkristalluntersuchungen bestimmt. Alle kristallisieren in der trigonalen Raumgruppe P 3112, Z = 3. Ein struktureller Vergleich mit Lanthanoidchloroaluminaten der gleichen Zusammensetzung und der thermische Abbau von LnAl3Br12 (Ln = Nd) zum entsprechenden Lanthanoidtribromid werden beschrieben.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926130107
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    Zur Kristallstruktur von Cu3NbTaO8 (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 60-62 
    Details
    ISSN: 0044-2313
    Keywords: Copper ; tantalum ; niobium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structure of Cu3NbTaO8Single crystals of Cu3NbTaO8 were prepared by solid state reaction. X-ray investigations led to triclinic symmetry, space group C1i—P1 with a = 5.179; b = 5.474; c = 6.003 Å; α = 72.85°; β = 83.39°; γ = 65.77°; Z = 1. Nb5+ and Ta5+ occupy one point position statistically. Both ions show an octahedral oxygen surrounding. Cu(1) is inside an elongated CuO6 octahedra and Cu(2) is coordinated by 5 O2- forming a distorted square pyramid. The polyhedra connection is shown and discussed.
    Notes: Einkristalle von Cu3NbTaO8 wurden durch Feststoffreaktion dargestellt. Die röntgenographische Untersuchung führte zu trikliner Symmetrie, Raumgruppe C1i  -  P1 mit a = 5,179; b = 5,474; c = 6,003 Å; α = 72,85°; β = 83,39°; γ = 65,77°; Z = 1. Nb5+ und Ta5+ besetzen eine Punktlage statistisch. Beide Ionen sind oktaedrisch von O2- koordiniert. Cu(1) zeigt ein stark gestrecktes CuO6-Oktaeder, während Cu(2) tetragonal pyramidal koordiniert ist. Die Polyederverknüpfung wird gezeigt und diskutiert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926130110
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