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  • 1995-1999  (134)
  • 1890-1899
  • 1850-1859
  • 1997  (134)
  • crystal structure  (134)
  • 101
    Electronic Resource
    Electronic Resource
    Tetrameres Di(-tert-butylamino)di(-N-lithiummethylamino)silan, (Me3CHN)2Si(NLiMe)2 - Darstellung und KristallstrukturProfessor Peter Sartori zum 65. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 288-291 
    Details
    ISSN: 0044-2313
    Keywords: Tetraaminosilane ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetrameric Di(-tert-butylamino)di(-N-lithiomethylamino)silane, (Me3CHN)2Si(NLiMe)2 - Synthesis and Crystal StructureDi(-tert.-butylamino)dichlorosilane reacts with an excess of methylamine to give di(-tert.-butylamino)di(methylamino)silane 1, (Me3CHN)2Si(NHMe)2. The dilithiumderivative 2, (Me3CHN)2Si(NLiMe)2, is obtained in the reaction of 1 with a molar ratio 1:2 of n-buli in n-hexane. In absence of donorsolvents 2 crystallizes tetrameric. Lithium is coordinated in three different ways and substitutes the methylamino-hydrogen. In the crystal structure two eight-membered (NLiNSi)2-rings are connected by two lithium.
    Notes: Di(-tert.-butylamino)dichlorsilan reagiert mit Methylamin im überschuß zu Di(-tert.-butylamino)di(methylamino)silan 1, (Me3CHN)2Si(NHMe)2. Nach Metallierung mit der bimolaren Menge n-BuLi in n-Hexan wird das Lithiumderivat 2, (Me3CHN)2Si(NLiMe)2, gebildet. In Abwesenheit von Donorsolventien kristallisiert 2 aus n-Hexan als Tetramer. Lithium liegt dabei in drei verschiedenen Koordinationen vor und ersetzt den Methylamin-Wasserstoff. Im Kristall werden zwei achtgliedrige (NLiNSi)2 Ringe über zwei Lithiumionen verbunden.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230146
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  • 102
    Electronic Resource
    Electronic Resource
    Metallkomplexe mit biologisch wichtigen Liganden. XC. Chirale Cyclopentadienyl-Nitrosyl-Molybdän-Komplexe mit α-Aminocarboxylat-Chelat-Liganden: (η5-C5R5)(ON)(I)Mo(α-Aminocarboxylat) (R = H, Me)Professor Klaus Brodersen zum 70. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 299-303 
    Details
    ISSN: 0044-2313
    Keywords: Cyclopentadienyl nitrosyl molybdenum complexes ; α-aminocarboxylate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal Complexes of Biologically Important Ligands. XC [1]. Chiral Cyclopentadienyl-Nitrosyl-Molybdenum Complexes of α-Amino Carboxylates: (η5-C5R5)(ON)(I)Mo(α-aminocarboxylate) (R = H, Me)The reactions of [(η5-C5H5)Mo(NO)I2]2 with glycinate, D-phenylglycinate, L-prolinate and L-azetidine-2-carboxylate give the chiral chelate complexes (η5-C5H5)(ON)(I)Mo(η-aminocarboxylate) as mixtures of isomers. The x-ray diffraction of a crystal of shows trans configuration of the amino acid and nitrosyl donors in a tetragonal pyramid.
    Notes: Die iodoverbrückten Komplexe [(η5-C5H5)Mo(NO)I2]2 setzen sich mit Glycinat, D-Phenylglycinat, L-Prolinat und L-Azetidin-2-carboxylat zu den chiralen Chelat-Komplexen (η5-C5H5)(ON)(I)Mo(α-Aminocarboxylat) um, die als Mischung von Isomeren entstehen. Die Röntgenstrukturanalyse eines Kristalls von zeigt die trans-Konfiguration der Amino- und Nitrosyl-Liganden in einer tetragonalen Pyramide.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230148
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  • 103
    Electronic Resource
    Electronic Resource
    Darstellung und Kristallstruktur von LnCu4-xP2 (Ln: Y, La-Yb) sowie von LuCu3-xP2 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 608-612 
    Details
    ISSN: 0044-2313
    Keywords: Ternary copper phosphides ; yttrium ; rare earth ; 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 LnCu4-xP2 (Ln: Y, La-Yb) and LuCu3-xP2Several new ternary Cu phosphides were prepared by heating mixtures of the elements. The compounds LnCu4-xP2 (Ln: Y, La-Yb) crystallize in the rhombohedral CaCu4P2 type structure (R3m; Z = 3). Single crystal X-ray investigations of EuCu3.8P2, PrCu3.7P2 and GdCu3.7P2 (hexagonal axes see “Inhaltsübersicht”) confirmed this structure and revealed a deviation from full occupancy of one copper position. LuCu3-xP2 (R3m; Z = 6; a = 3.957(1), c = 40.109(3) Å; hex. axes) crystallizes in the YbCu3P2 type structure, which is derived from the CaAl2Si2 and Cu3P type structure.
    Notes: Durch Erhitzen entsprechender Elementgemenge konnte eine Reihe neuer ternärer Cu-Phosphide dargestellt werden. Die Verbindungen LnCu4-xP2 (Ln: Y, La-Yb) kristallisieren in der rhomboedrischen CaCu4P2-Struktur (R3m; Z = 3) mit einer geringfügig unterbesetzten Cu-Punktlage. Dies ergaben Strukturbestimmungen, die mit Einkristallmethoden an EuCu3,8P2 (a = 4,064(1), c = 22,762(2) Å), PrCu3,7P2 (a = 4,035(1), c = 22,318(4) Å) sowie GdCu3,7P2 (a = 3,994(1), c = 21,953(2) Å) (Gitterkonstanten jeweils in hexagonaler Aufstellung) durchgeführt wurden. LuCu3-xP2 (R3m; Z = 6; a = 3,957(1), c = 40,109(3) Å; hex. Aufstellung) kristallisiert im YbCu3P2-Typ, in dem sich längs [001] Baueinheiten abwechseln, die auf den CaAl2Si2- bzw. Cu3P-Strukturtyp zurückzuführen sind.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230195
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  • 104
    Electronic Resource
    Electronic Resource
    Synthesis and Characterization of cis- and trans-Tetrachlorobis(pyridine)platinum(IV)Dedicated to Professor Siegfried Engels on the Occasion of his 65th Birthday (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 603-607 
    Details
    ISSN: 0044-2313
    Keywords: Platinum complex ; crown ether ; Raman and IR data ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Charakterisierung von cis- und trans-Tetrachlorobis(pyridin)platin(IV)[Na(15-cr-5)]2[PtCl6] · 2 H2O reagiert mit Pyridin in Wasser als Lösungsmittel zu cis-[PtCl4(py)2] (1) und in MeCN, DMF sowie in CH2Cl2 zu trans-[PtCl4(py)2] (2). Die Substitutionsreaktion wird durch Bestrahlung mit sichtbarem Licht beschleunigt. Sowohl gelöst in DMSO, DMF und MeCN als auch bei 503 K im festen Zustand isomerisiert 1 zu 2.1 und 2 sind umfassend IR- und ramanspektroskopisch charakterisiert worden. Die Molekülstruktur des trans-Isomeren 2 wurde auch durch Röntgeneinkristallstrukturunterschung ermittelt (monoklin, C2/m, a = 14.143(5), b = 7.171(3), c = 7.199(3) Å, β = 116.42(4)°, Z = 2, R1 = 0.0331, wR2 = 0.0727). 2 weist angenähert D2h Symmetrie auf, wobei die beiden trans-ständigen Pyridinliganden in einer Ebene liegen. Nach quantenchemischen Berechnungen ist 2 (D2h-Symmetrie) um 48.28 kJ/mol stabiler als 1 (C2v-Symmetrie).
    Notes: [Na(15-cr-5)]2[PtCl6] · 2 H2O reacts with pyridine in water as solvent to give cis-[PtCl4(py)2] (1) and in MeCN, DMF or in CH2Cl2 to give trans-[PtCl4(py)2] (2). The substitution reaction can be accelerated by irradiation with visible light. 1 isomerizes to give 2 in DMSO, DMF and MeCN as well as in solid state at 503 K.1 and 2 were thoroughly characterized IR and Raman spectroscopically. The molecular structure of the trans isomer 2 was also established by X-ray structure analysis (monoclinic, C2/m, a = 14.143(5), b = 7.171(3), c = 7.199(3) Å, β = 116.42(4)°, Z = 2, R1 = 0.0331, wR2 = 0.0727). 2 has nearly D2h symmetry with two trans standing pyridine ligands lying in a plane. According to quantum chemical calculations, 2 (D2h symmetry) is more stable (48.28 kJ/mol) than 1 (C2v symmetry).
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230194
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  • 105
    Electronic Resource
    Electronic Resource
    Die erste Kristallstrukturanalyse einer IodylverbindungProfessor Welf Bronger zum 65. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1055-1060 
    Details
    ISSN: 0044-2313
    Keywords: Iodyldisulfate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Crystal Structure Analysis of an Iodyl CompoundSingle crystals of (IO2)2S2O7 were obtained for the first time by reacting iodic acid and oleum at 195°C. According to the results of a X-ray structure determination (monoclinic, P21/a, a = 885.0(2), b = 1037.3(2), c = 915.8(2) pm, β = 94.75(2)°, Z = 4, 1466 diffractometer data, R1 = 0.033, wR2 = 0.063), (IO2)2S2O7 contains dimeric iodyl cations (IO2)22+, which are connected by disulfate groups thus forming polymeric strands. Strikingly, the I—O-distances range almost continously from 174 pm (strong intramolecular bonds) to — 300 pm (van der Waals contacts).
    Notes: Durch Umsetzung von Iodsäure in Oleum bei 195°C wurden erstmals Einkristalle von Iodyldisulfat erhalten. Nach der Röntgenstrukturanalyse (monoklin, P21/a, a = 885,0(2), b = 1037,3(2), c = 915,8(2) pm, β = 94,75(2)°, Z = 4, 1466 unabhängige Reflexe, R1 = 0,033, wR2 = 0,063) liegen dimere Iodylkationen (IO2)22+ vor, die über Disulfatgruppen zu polymeren Strängen verknüpft sind. Auffällig ist eine nahezu gleichmäßige Verteilung der I—O-Abstände über den gesamten Bereich von starken intramolekularen Bindungen (174 pm) bis zu intermolekularen Kontakten vom van der Waals Typ (〉 300 pm).
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230708
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  • 106
    Electronic Resource
    Electronic Resource
    Komplexchemie P-reicher Phosphane und Silylphosphane. XIII [1]. [η2-{tBu2P—P=PtBu2} PtBr(PPh3)]Professor Welf Bronger zum 65. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1088-1092 
    Details
    ISSN: 0044-2313
    Keywords: [η2-{tBu2P—P=PtBu2} PtBr(PPh3)] ; crystal structure ; 1H-, 13C-, 31P-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Coordination Chemistry of P-rich Phosphanes and Silylphosphanes. XIII [1]. [η2-{tBu2P—P=PtBu2} PtBr(PPh3)][η2-{tBu2P—P=PtBu2} PtBr(PPh3)] 1 is the first transition metal complex compound resulting from a phosphino-phosphinidene-phosphorane. The yellow crystals of 1 (fp. 201-203°C, decomp.) were obtained by reacting tBu2P—P=P(Br)tBu2 with either (Ph3P)2Pt · C2H4, or with Pt(PPh3)4, resp. Compound 1 crystallizes triclinic in the space group P1 (no. 2) with a = 1076.80(8) pm, b = 1344.61(8) pm, c = 1381.16(9) pm, α = 81.773(6)°, β; = 85,110(8), γ = 88,776(7).
    Notes: [η2-{tBu2P—P=PtBu2} PtBr(PPh3)] 1 ist die erste Komplexverbindung aus einem Phosphino-phosphiniden-phosphoran. Die gelben Kristalle von 1, Smp. 201-203°C (unter Zersetzung) bilden sich bei der Umsetzung von tBu2P—P=P(Br)tBu2 mit (Ph3P)2Pt · C2H4 oder Pt(PPh3)4. 1 kristallisiert triklin in P1 (Nr. 2) mit a = 1076,80(8) pm, b = 1344,61(8) pm, c = 1381,16(9) pm, α = 81,773(6)°, β; = 85,110(8)°, γ = 88,776(7).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230713
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  • 107
    Electronic Resource
    Electronic Resource
    Derivate des Imidazols. XXIV [1].[Li12O2Cl2(ImN)8(THF)4] · 8 THF: Ein Peroxo-Komplex des Lithiums mit neuartiger KäfigstrukturProfessor Welter Siebert zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1121-1124 
    Details
    ISSN: 0044-2313
    Keywords: Lithium ; imidazole derivatives ; peroxo complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Imidazole Derivatives. XXIV. [Li12O2Cl2(ImN)8(THF)4] · 8 THF: a Peroxo Lithium Fragment in a Novel Cage Structure1,3-dimethyl-2-iminoimidazoline (8, ImNH) reacts with methyl lithium to give [ImNLi]n (9). In tetrahydrofuran, crystals of C56H96Cl2Li12N24O6 · 8 C4H8O (10) are obtained. The structure of 10 consists of a Li12Cl2N8O2 core in which a peroxo unit is incorporated into a stack of ladder fragments. Over all, four tetrahydrofuran and eight imidazoline ligands are attached at the lithium and nitrogen atoms.
    Notes: 1,3-Dimethyl-2-iminoimidazolin (8, ImNH) reagiert mit Methyllithium in Diethylether zu [ImNLi]n (9). In Tetrahydrofuran werden Kristalle von [Li12O2Cl2(ImN)8(THF)4] · 8 THF (10) erhalten. In 10 liegt ein Li12Cl2N8O2-Käfig in Form gestapelter Leiterfragmente mit O22 als zentraler Einheit vor. Hieran sind über die Lithium- und Stickstoffatome insgesamt vier Tetrahydrofuran- und acht Imidazolin-Liganden koordiniert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230719
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  • 108
    Electronic Resource
    Electronic Resource
    The Structures and Characterization of Two New Oxides of the Sr4PtO6 Type: NaCa3IrO6 and NaCa3RuO6 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1131-1134 
    Details
    ISSN: 0044-2313
    Keywords: Iridium ; ruthenium ; sodium ; calcium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturen und Charakterisierung von zwei neuen Oxiden vom Sr4PtO6-Typ: NaCa3IrO6 und NaCa3RuO6NaCa3IrO6 (I) und NaCa3RuO6 (II) kristallisieren mit trigonaler (rhomboedrischer) Symmetrie in der Raumgruppe R3c, Z = 6, I: a = 9,272(3) Å, c = 11,214(1) Å, II: a = 9,244(3) Å, c = 11,201(1) Å. I und II sind isotyp zu Verbindungen vom Sr4PtO6-Typ. Die Strukturen wurden mittels Röntgen-Einkristallstrukturanalyse gelöst mit einem R-Wert von 0,032 und Rw = 0,039 für I bzw. R = 0,024 und Rw = 0,031 für II. Die Struktur besteht aus unendlichen Ketten von flächenverknüpften MO6-Oktaedern mit M=Ir bzw. Ru und trigonalen Prismen von NaO6. Die Ketten sind getrennt durch Calcium-Kationen.
    Notes: NaCa3IrO6 (I) and NaCa3RuO6 (II) crystallize with trigonal (rhombohedral) symmetry in the space group R3c, Z = 6, for I a = 9.272(3) Å, c = 11.214(1) Å; for II a = 9.244(3) Å, c = 11.201(1) Å. NaCa3IrO6 (I) and NaCa3RuO6 (II) are isotypic to compounds of the Sr4PtO6 structure type. The structures have been solved by means of single crystal X-ray diffraction data analysis with the reliability factors for I of R = 0.032 and Rw = 0.039; and the the reliability factors for II of R = 0.024 and Rw = 0.031. The structure consists of infinite chains of alternating face-sharing MO6 octahedra, where M=Ir or Ru, and NaO6 trigonal prisms. The chains are separated by the calcium cations.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230721
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  • 109
    Electronic Resource
    Electronic Resource
    Thia- und Selena-arachno-undecaboran 6,7-μ-(CH3E)B10H13 Kristallstruktur von arachno-6,7-μ-(CH3Se)B10H13 Theoretische Untersuchungen der Molekülstrukturen und 11B-NMR-Verschiebungen von arachno-6,7-μ-(CH3E)B10H13 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1157-1162 
    Details
    ISSN: 0044-2313
    Keywords: Thia- and selena-arachno-undecaborane ; preparation ; spectroscopy ; ab initio/IGLO ; GIAO/NMR method ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thia- and Selena-arachno-undecaborane 6,7-μ-(CH3E)B10H13. Crystal Structure of arachno-6,7-μ-(CH3Se)B10H13. Theoretical Investigations of the Molecular Structures and 11B NMR Shifts of arachno-6,7-μ-(CH3E)B10H13The reaction of B10H14 with (CH3)2S yields with loss of H2 the base adduct 6,9-[(CH3)2S]2B10H12. Although an analogous reaction between B10H14 with disulfanes or diselenanes was expected to produce 6,9 bridged dichalcogen derivatives, (CH3)2S2 failed to react even under reflux conditions. Trisulfane (CH3)2S3 does react, but the pathway is different and leads to (CH3S)B10H13 2 without loss of H2. Unlike of (CH3)2S2, (CH3)2Se2 yields (CH3Se)B10H13, 3. Both 2 and 3 are formed by substitution of a bridging hydrogen and could be obtained in pure form and characterized 11B NMR spectroscopically. A single crystal X-ray structure analysis also was performed on 3 (space group P21/c). The molecular structures of 2 and 3 were optimized at the MP2 level and 11B NMR shifts were computed at the IGLO-SCF, GIAO-SCF and GIAO-B3LYP levels of theory.
    Notes: Bei der Reaktion zwischen B10H14 und (CH3)2S erfolgt unter H2-Abspaltung eine zweifache Adduktbildung, die zu 6,9-[(CH3)2S]2B10H12 führt. Die analoge Umsetzung zwischen B10H14 mit Disulfanen bzw. Diselenanen führte jedoch nicht zu den 6,9-Dichalkogen-verbrückten Derivaten. Bei der Umsetzung mit (CH3)2S2 findet selbst unter Refluxbedingungen keine Reaktion statt, wohl aber mit dem Trisulfan (CH3)2S3. Die Reaktion verläuft aber nicht unter H2-Abspaltung. Vielmehr wird dabei ein Brücken-H-Atom durch eine CH3S-Gruppe substituiert unter Bildung von (CH3S)B10H13 2. Im Gegensatz zu (CH3)2S2 findet aber mit (CH3)2Se2 ebenfalls eine Brücken-H-Substitution statt, wobei (CH3Se)B10H13 3 gebildet wird. 2 und 3 konnten in reiner Form isoliert und 11B-NMR-spektroskopisch charakterisiert werden. Von 3 wurde eine Röntgenstrukturanalyse durchgeführt (Raumgruppe P21/c) und von 2 und 3 die Molekülstrukturen auf MP2-Niveau optimiert sowie 11B-NMR- Verschiebungen mit IGLO-SCF, GIAO-SCF und GIAO-B3LYP berechnet.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230725
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  • 110
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    Electronic Resource
    Zur Synthese und Kristallstruktur der ternären Carbide Na2PdC2 und Na2PtC2Professor Welf Bronger zum 65. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1208-1210 
    Details
    ISSN: 0044-2313
    Keywords: Ternary carbides ; crystal structure ; sodium ; palladium ; platinum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Syntheses and Crystal Structures of Ternary Carbides Na2PdC2 and Na2PtC2Na2PdC2 and Na2PtC2 were synthesized by the reaction of sodium carbide with palladium and platinum respectively. The crystal structures could be solved from X-ray powder diffraction data (space group: P3m1, Z = 1). Both compounds crystallize in a new structure type with 1∞[M(C2)2/22-] chains (M≡Pd, Pt) as the characteristic structural unit. The existence of a C—C triple bond was confirmed by Raman spectroscopy.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230805
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  • 111
    Electronic Resource
    Electronic Resource
    Phosphan-, Phosphit- und Phosphido-Komplexe des Vanadiums(V) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1220-1228 
    Details
    ISSN: 0044-2313
    Keywords: Phosphane ; phosphite ; phosphido complexes of vanadium(V) ; syntheses ; 1H, 51V, 31P NMR ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphane, Phosphite, Phosphido, Complexes of Vanadium(V)Complex formation of tert-butylimidovanadium(V)trichloride (1) with phosphanes und phosphites has been studied. Syntheses of phosphidovanadium(V) compounds tC4H9N=VCp(NHtC4H9)[P(SiMe3)2] and tC4H9N=VCp(NiProp2)(PR2) (R=SiMe3, Ph) are described starting from the corresponding chlorovanadium(V) complexes. The reaction of 1 with silver hexafluorophosphate yields a bis(fluoro)phosphidovanadium(IV complex [(μ-PF2)2V2Cl2)(NtC4H9)2]; as primary intermediate product of the unknown redox reaction a cationic vanadium(V) complex [tC4H9N=VCl2 · PPh3]+PF6- has been isolated. 1 reacts with an excess of diisopropylamine forming tC4H9N=V(NiProp2)Cl2 (16); in addition the following diisopropylamido-tert-butylimidovanadium(V) compounds tC4H9N=VCp(NiProp2)Cl (3) and tC4H9N=V(NiProp2)X2 (X=CH2CMe3, OtC4H9, CH3COO) has been prepared. All compounds obtained are characterized by 1H, 51V, 31P NMR spectroscopy. The X-ray diffraction analysis of 16 and 3 indicate a planar coordination sphere of the amido nitrogen atom.
    Notes: Die Komplexbildung des tert-Butylimidovanadium(V)-trichlorids (1) mit Phosphanen und Phosphiten wurde untersucht. Die Darstellung der Phosphidovanadium(V)-Verbindungen tC4H9N=VCp(NHtC4H9)[P(SiMe3)2] und tC4H9N=VCp(NiProp2)(PR2) (R=SiMe3, Ph) wird beschrieben; als Ausgangsverbindungen werden entsprechende Chorovanadium(V)-Komplexe eingesetzt. Die Reaktion von 1 mit Silberhexafluorophosphat führt zu einem Difluorphosphidovanadium(IV)-Komplex [(μ-PF2)2V2Cl2(NtC4H9)2]; als erste Zwischenstufe der unbekannten Redoxreaktion wurde ein kationischer Vanadium(V)-Komplex [tC4H9N=VCl2 · PPh3]+PF6- isoliert. 1 reagiert mit überschüssigem Diisopropylamin unter Bildung von tC4H9N=V(NiProp2)Cl2 (16); weitere Umsetzungen lieferten die Diisopropylamido-tert-butylimido-vanadium(V)-Verbindungen tC4H9N=VCp(NiProp2)Cl (3) und tC4H9N=V(NiProp2)X2 (X=CH2CMe3, OtC4H9, CH3COO). Alle dargestellten Verbindungen werden 1H-, 51V- und 31P-NMR-spektroskopisch charakterisiert. Die Röntgenstrukturanalyse von 16 und 3 zeigt eine planare Koordinationssphäre des Amido-Stickstoffatoms.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230807
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    Reaktionen von Lanthanoidhalogeniden mit Alkalibenzylverbindungen. Darstellung und Kristallstrukturen von [(tmeda)(C6H5CH2)2Y(μ-Br)2Li(tmeda)], [(tmeda)2SmBr(μ-Br)2Li(tmeda)] und [(dme)2SmBr(μ-Br)]2 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1542-1546 
    Details
    ISSN: 0044-2313
    Keywords: Yttrium(III) ; samarium(II) ; benzyl complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Lanthanide Halides with Alkalibenzyl Compounds. Synthesis and Crystal Structures of [(tmeda)(C6H5CH2)2Y(μ-Br)2Li(tmeda)], [(tmeda)2SmBr(μ-Br)2Li(tmeda)] and [(dme)2SmBr(μ-Br)]2Alkali-benzyl compounds react via a metathesis reaction with lanthanide halides to benzyl complexes of the rare earths. Reaction of [(C6H5CH2)Li(tmeda)] with YBr3 leads to the complex [(tmeda)Y(C6H5CH2)2 (μ-Br)2Li(tmeda)] 1, in which Yttrium and lithium are linked via two bromide bridges. However, the reaction of [(C6H5CH2)Li(tmeda)] with SmBr3 in toluene/tmeda leads under reduction of the Sm ion to the compound [(tmeda)2SmBr(μ-Br)2Li(tmeda)] 2. 2 reacts with DME to yield the dimeric compound [(dme)2SmBr(μ-Br)]2 3. The structures of 1-3 were determined by X-ray single crystal structure analysis:1:Space group P21/c, Z = 4, a = 829.5(6) pm, b = 1477.9(11) pm, c = 2575.0(10) pm, β = 92.03(6)°,2:Space group P21, Z = 2, a = 954,7(3) pm, b = 1338.5(6) pm, c = 1244.9(5) pm, β = 107.51(3)°,3:Space group P1, Z = 1, a = 797.2(7) pm, b = 818.3(7) pm, c = 1169.7(8) pm, α = 100.96(6)°, β = 92.03(6)°, γ = 91.75(7)°.
    Notes: Alkalibenzylverbindungen reagieren mit Lanthanoidhalogeniden unter Salzabspaltung zu Benzylkomplexen der Seltenen Erden. [(C6H5CH2)Li(tmeda)] bildet mit YBr3 den Komplex [(tmeda)(C6H5CH2)2Y(μ-Br)2Li(tmeda)] 1, in dem das Yttriumion mit Lithium über zwei Bromo-Brücken verknüpft ist. Bei der Reaktion von [(C6H5CH2)Li(tmeda)] mit SmBr3 in Toluol/TMEDA erfolgt hingegen unter Reduktion die Bildung von [(tmeda)2SmBr(μ-Br)2Li(tmeda)] 2. Diese Verbindung bildet mit DME den zweikernigen Komplex [(dme)2SmBr(μ-Br)]2 3. Die Strukturen von 1, 2 und 3 wurden durch Einkristallstrukturanalyse geklärt:1:Raumgruppe P21/c, Z = 4, a = 829,5(6) pm, b = 1477,9(11) pm, c = 2575,0(10) pm, β = 92,03(6)°,2:Raumgruppe P21, Z = 2, a = 954,7(3) pm, b = 1338,5(6) pm, c = 1244,9(5) pm, β = 107,51(3)°,3:Raumgruppe P1, Z = 1, a = 797,2(7) pm, b = 818,3(7) pm, c = 1169,7(8) pm, α = 100,96(6)°, β = 92,03(6)°, γ = 91,75(7)°.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231012
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    Two New Modifications of [P(C6H5)4]2[Cu2I4] (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1555-1560 
    Details
    ISSN: 0044-2313
    Keywords: Iodocuprate(I) ; [Cu2I4]2- ; tetraphenylphosphonium ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zwei neue Modifikationen von [P(C6H5)4]2[Cu2I4]Bei der Reaktion von granuliertem Kupfer mit Iod und [P(C6H5)4]I in trockenem Aceton unter Stickstoffatmosphäre wurden Einkristalle von zwei neuen Modifikationen von [P(C6H5)4]2[Cu2I4] erhalten. Sie kristallisieren monoklin, Raumgruppe P21/n (Nr. 14), a = 11.550(6), b = 7.236 (2), c = 27.232 (13) Å, β = 98.13(3)°, V = 2253(2) Å3 und Z = 2 ([P(C6H5)4]2[Cu2I4]-C) bzw. Raumgruppe Cc (Nr. 9), a = 17.133(5), b = 15.941(5), c = 18.762(6) Å, β = 114.02(1)°, V = 4681(3) Å3 und Z = 4 ([P(C6H5)4]2[Cu2I4] -D). In diesen Verbindungen liegen dimere di-μ-iodo-diiodocuprat(I)-Einheiten vor, die planar (C) bzw. gewinkelt (D) sind.
    Notes: Single crystals of two new modifications of [P(C6H5)4]2[Cu2I4] were obtained by reaction of granulated copper with iodine and [P(C6H5)4]I in dry acetone under nitrogen atmosphere. They crystallise monoclinically, space group P21/n (No. 14), a = 11.550(6), b = 7.236(2), c = 27.232(13) Å, β = 98.13(3)°, V = 2253(2) Å3, and Z = 2 ([P(C6H5)4]2[Cu2I4]-C), and space group Cc (No. 9), a = 17.133(5), b = 15.941(5), c = 18.762 (6) Å, β = 114.02(1)°, V = 4681(3) Å3, and Z = 4 ([P(C6H5)4]2[Cu2I4]-D), respectively. In these compounds the [CuI2]- anions form dimers di-μ-iodo-diiodocuprate(I), which are either planar (C) or folded (D).
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    URL: http://dx.doi.org/10.1002/zaac.19976231014
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    Tetraphenylphosphonium-tetradecachlorotetraarsenat(III), (PPh4)2As4Cl14 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1033-1034 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium-tetradecachlorotetraarsenate(III) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetraphenylphosphonium Tetradecachlorotetraarsenate(III), (PPh4)2As4Cl14The title compound was obtained by reaction of As4S4, PPh4Cl and chlorine in dichloromethane. According to its X-ray crystal structure analysis, the As4Cl142- ion can be described as an association product of two AsCl4- units and two AsCl3 molecules. The As atoms and ten Cl atoms are approximately in a plane, the remaining four Cl atoms alternately take positions above and below this plane. The As atoms have distorted ψ octahedral coordination.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230702
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    Metallkomplexe mit biologisch wichtigen Liganden. XCV. η5- Pentamethylcyclopentadienyl-Rhodium-, -Iridium-, (η6-Benzol)-Ruthenium- und Phosphan-Palladium-Komplexe von Prolinmethylester und ProlinamidProfessor Anton Meller zum 65. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1903-1911 
    Details
    ISSN: 0044-2313
    Keywords: Rhodium ; ruthenium ; iridium ; palladium ; proline ; amide complexes ; proline methylester complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal Complexes of Biologically Important Ligands. XCV. η5-Pentamethylcyclopentadienyl Rhodium, Iridium, η6- Benzene Ruthenium, and Phosphine Palladium Complexes of Proline Methylester and Proline AmideProline methylester (L1) and proline amide (L2) give with the chloro bridged complexes [(η5 -C5Me5)MCl2]2 (M = Rh, Ir), [(η6 -benzene)RuCl2]2 and [Et3PPdCl2]2 N and N,O coordinated compounds: (η5 -C5Me5)M(Cl2)L1 (1, 2 M = Rh, Ir), [(η5-C5Me5) Rh(Cl)(L2)]+Cl- (5), [(η6- C6Me6) Ru(Cl)(L2)]+Cl- (6), [(η6-p-cymene)Ru(Cl)(L2)]+Cl- (7), [(eta;5-C5Me5)M(Cl)(L2-H+)] (9, 10 M = Rh, Ir), (Et3P)Pd(Cl)2L1 (3), and [(Et3P)Pd(Cl)(L2)]+Cl- (8). The NMR spectra indicate that for 5 and 6 only one diastereoisomer is formed. The complexes 1, 2, 3 and 5 were characterized by X-ray diffraction.
    Notes: Prolinmethylester (L1) und Prolinamid (L2) bilden mit den chlorverbrückten Komplexen [(η5-C5Me5)MCl2]2 (M = Rh, Ir), [(η6-p-Cymol)RuCl2]2 und [Et3PPdCl2]2 Verbindungen mit N- und N,O-Koordination: (η5-C5Me5)M(Cl2)L1 (1, 2 M = Rh, Ir), [(η5-C5Me5) Rh(Cl) (L2)]+Cl- (5), [(η6- C6Me6)Ru(Cl) (L2)]+Cl- (6), [(η6-p- Cymol)Ru(Cl)(L2)]+Cl- (7), [(η5- C5Me5)M(Cl)(L2-H+)] (9, 10 M = Rh, Ir), (Et3P)Pd(Cl)2L1 (3) und [(Et3P)Pd(Cl)(L2)]+Cl- (8). Die NMR Spektren weisen darauf hin, daß von 5 und 6 jeweils nur ein Diastereoisomeres entsteht. Die Komplexe 1, 2, 3 und 5 wurden durch Röntgenstrukturanalyse charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19976231214
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    The Crystal Structure of an “Old” Potassium Uranyl Acetate, K(UO2)(CH3COO)3 · 0.5 H2O (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 35-38 
    Details
    ISSN: 0044-2313
    Keywords: Potassium uranyl acetate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die Kristallstruktur eines „alten“ Uranylacetats, K(UO2)(CH3COO)3 · 0,5 H2ODie Uranylgruppe der Titelsubstanz, K(UO2)(CH3COO)3 · 0.5 H2O, wird von drei bidentaten Essigsäure-Anionen sechsfachkoordiniert. Die Verbindung kristallisiert tetragonal, Raumgruppe I41/a(N° 88 Int. Tab.) mit Z = 16 und a = 1447,1(4), c = 2626,5(8) pm.Die Kristallstruktur wurde unter Verwendung von 2056 unabhängigen Reflexen Fo 〉 4σ (Fo) mit einem wR2 Wert von 0,1234 (SHELXL-93) gelöst.Die einzelnen Moleküle werden durch Wasserstoffbrückenbindungen über Wassermoleküle verknüpft.
    Notes: The uranyl group in the title compound, K(UO2)(CH3COO)3 · 0.5 H2O is sixfold coordinated by three bidentate acetic acid anions. It crystallizes tetragonal, space group I41/a (N° 88 Int. Tab.) with Z = 16 and a = 1447.1(4), c = 2626.5(8) pm.The crystal structure was solved by using 2056 unique reflections Fo ° 4σ (Fo) with a final wR2 value of 0.1234 (SHELXL-93).Individual molecules are linked by hydrogen bonds between coordinated water molecules and acetate O atoms.
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    URL: http://dx.doi.org/10.1002/zaac.19976230106
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    Über kristalline Natriumhydroxogallate (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1483-1488 
    Details
    ISSN: 0044-2313
    Keywords: Nonasodium bis(hexahydroxogallate) trihydroxide hexahydrate ; decasodium bis(hexahydroxogallate) tetrahydroxide ; disodium tetrahydroxogallate chloride ; crystal structure ; 71Ga MAS NMR ; 23Na MAS NMR ; DTA, DTG, guinier lenné technique ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Crystalline Sodium HydroxogallatesTwo crystalline sodium hydroxogallates 4,5 Na2O · Ga2O3 · 13,5 H2O (I) and 5 Na2O · Ga2O3 · 8 H2O (II), as well as a crystalline phase of the composition Na2O · Ga2O3 · 4 H2O · 2 NaCl (III) are described.
    Notes: Es werden zwei kristalline Natriumhydroxogallate 4,5 Na2O · Ga2O3 · 13,5 H2O (I) und 5 Na2O · Ga2O3 · 8 H2O (II) sowie eine kristalline Phase der Zusammensetzung Na2O · Ga2O3 · 4 H2O · 2 NaCl (III) beschrieben.(I) kristallisiert aus Natriumgallatlösungen eines breiten Konzentrationsfeldes und hat nach Einkristallröntgenstrukturanalyse [1] eine dreidimensional vernetzte Struktur aus monomeren [Ga(OH)6]3--Anionen, die über NaO6-Koordinationspolyeder untereinander verbunden sind; daneben sind Kristallwasser und weitere Hydroxidionen enthalten.Damit ist (I) als Nonanatrium-bis(hexahydroxogallat)-trihydroxid-hexahydrat (Na9[Ga(OH)6]2(OH)3 · 6 H2O) zu formulieren; Isotypie besteht zu dem entsprechenden Natriumhydroxoaluminat [2, 3]. 5 Na2O · Ga2O3 · 8 H2O II) läßt sich aus (I) in Gegenwart von Natriumhydroxid durch Entwässern über P4O10 bei Raumtemperatur unter Schutzgas (N2) erhalten. Es kristallisiert tetragonal, ist isotyp mit Na10[Al(OH)6]2(OH)4 [4] und dementsprechend als Na10[Ga(OH)6]2(OH)4 zu formulieren. Durch Zusatz von Natriumchlorid zu Natriumgallatlösungen läßt sich Na2O · Ga2O3 · 4 H2O · 2 NaCl (III) isolieren, das ebenfalls tetragonal und isotyp zu Na2[Al(OH)4]Cl [5] ist. Es handelt sich demnach um das Dinatriumtetrahydroxogallatchlorid Na2[Ga(OH)4]Cl. Die Ergebnisse der 71Ga- und 23Na-MASNMR-Messungen an den Verbindungen (I) bis (III) und deren thermisches Verhalten werden diskutiert.(I) crystallizes from sodium gallate solutions in a wide concentration field; from the X-ray single crystal diffraction analysis [1] results a three dimensional network structure, consisting of monomeric [Ga(OH)6]3- anions connected by NaO6 octahedra groups. Furthermore the structure contains water of crystallization and further hydroxide ions. (I) has to be formulated as nonasodium bis(hexahydroxogallate) trihydroxide hexahydrate Na9[Ga(OH)6]2(OH)3 · 6 H2O; it is isotypic with the corresponding sodium hydroxoaluminate [2, 3]. 5 Na2O · Ga2O3 · 8 H2O (II) was obtained from (I) in presence of sodium hydroxide by dehydration over P4O10 in an inert atmosphere (N2) at room temperature. (II) crystallizes tetragonally and is isotypic with Na10[Al(OH)6]2(OH)4 [4]. Accordingly it could be described as a decasodium bis(hexahydroxogallate) tetrahydroxide, Na10[Ga(OH)6]2(OH)4. Na2O · Ga2O3 · 4 H2O · 2 NaCl (III) was obtained by addition of sodium chloride to sodium gallate solutions, (III) crystallizes also tetragonally and is isotypic with (Na2[Al(OH)4]Cl [5]. Correspondingly, it has to be formulated as disodium tetrahydroxogallate chloride Na2[Ga(OH)4]Cl. The results of 71Ga and 23Na MAS NMR investigations of the compounds (I) to (III) and their thermal behaviour are discussed.
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    Diorganozinn(IV)-Derivate dreizähniger Dithiocarbazone - Strukturuntersuchungen in Lösung und im festen ZustandProfessor Lothar Beyer zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 141-146 
    Details
    ISSN: 0044-2313
    Keywords: Diorganotin complexes ; dithiocarbazone complexes ; chelate complexes ; crystal structure ; i.r.-, mass-, multinuclear n.m.r. spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Diorganotin(IV) Derivatives of Tridentate Dithiocarbazones - Structure Determination in the Solid and Liquid StateThe tridentate ligands with the S-Methyldithiocarbazate Schiff Base of 2-Salicylaldehyde (H2Sal) and 2-Pyridinaldehyde (HPyr) react in different way with diorganotin(IV) oxides, in the first case to the five-coordinate complex R2Sn—Sal with trigonal bipyramidal structure and in the second case to the binuclear complex [(R2Sn—Pyr)2CO3] with a bridging carbonat anion. The structures were elucidated by X-ray diffraction and by multinuclear NMR in solution. IR- and Mass-spectrometric measurements complete the results.
    Notes: Die dreizähnigen Liganden S-Methyl-β-N-(2-hydroxyphenyl)-methyliden- (H2Sal) und S-Methyl-β-N-(2-pyridyl)-methyliden-dithiocarbazon (HPyr) reagieren in unterschiedlicher Weise mit Diorganozinn(lV)-oxiden. Mit dem erstgenannten Liganden zu dem fünffach koordinierten Komplex R2Sn—Sal mit trigonal bipyramidaler Struktur, in der Reaktion mit dem zweiten Liganden zu dem Zweikernkomplex [(R2Sn—Pyr)2CO3] mit einem Carbonatanion als Brückenligand. Die Strukturaufklärungen erfolgten mittels Röntgenkristallstrukturanalyse und in Lösung mit multinuklearer NMR-Spektroskopie. IR- und massenspektrometrische Messungen ergänzen die Aussagen.
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    URL: http://dx.doi.org/10.1002/zaac.19976230123
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    Zur Chemie des Dimesityleisens. XI. Reaktion von Dimesityleisen mit β-Diketonen - Strukturen von Bis(diethylether)-bis(1,3-diphenylpropan-1,3-dionato)eisen(II) und Poly[bis(2,2,6,6-tetramethylheptan-3,5-dionato)eisen(II)-μ-(1,4-dioxan)] (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 155-158 
    Details
    ISSN: 0044-2313
    Keywords: Dimesityliron ; diketonate complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemistry of Dimesityl Iron. XI. Reaction of Dimesityl Iron with β-Diketones - Structures of Bis(diethylether)-bis(1,3-diphenylpropane-1,3-dionato)iron(II) and Poly[bis(2,2,6,6-tetramethylheptane-3,5-dionato)iron(II)-μ-(1,4-dioxan)]Reactions of tetramesityl diiron, Fe2Mes4 1, with β-diketones in the molar ratio of 1:4 form the diketonate complexes [Fe(diketonate)2]. Acidolysis of 1 with 1,3-diphenylpropane-1,3-dione (Hdbm) forms [Fe(dbm)2(OEt2)2] and with 2,2,6,6-tetramethylheptane-3,5-dione the coordination polymer [{Fe(dpm)2(μ-dioxane)}n] is obtained. The crystal structures of both complexes are presented.
    Notes: Die Umsetzung von Tetramesityldieisen, Fe2Mes4 1, mit β-Diketonen im Verhältnis 1 : 4 ergibt die Diketonatoeisenkomplexe [Fe(diketonat)2]. Aus 1 und Dibenzoylmethan (Hdbm) sowie Dipivaloylmethan (Hdpm) wurden [Fe(dbm)2(OEt2)2] und [{Fe(dpm)2(μ-dioxan)}n] hergestellt und ihre Strukturen bestimmt.
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    URL: http://dx.doi.org/10.1002/zaac.19976230126
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    Cs2CaH4, ein neues Hydrid: Das Volumeninkrement des Wasserstoffs als Kriterium zur Überprüfung von Struktur und Zusammensetzung (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 119-121 
    Details
    ISSN: 0044-2313
    Keywords: Metal hydrides ; crystal structure ; neutron diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cs2CaH4, a New Hydride: The Atomic Volume of Hydrogen as a Criterion to Check Crystal Structure and CompositionAccording to the investigations of Park, Pezat, and Darriet CsCaH3 crystallizes in the GdFeO3 structure type. As the resulting atomic volume of hydrogen is too small for a ionic hydride a re-examination of the crystal structure has been carried out. The results of our investigations show that the compound under discussion is actually Cs2CaH4. It crystallizes in the K2NiF4 structure type with the expected atomic volume for hydrogen. The complete crystal structure has successfully been determined by a neutron diffraction experiment on the deuteride Cs2CaD4.
    Notes: Nach Untersuchungen von Park, Pezat und Darriet soil CsCaH3 im GdFeO3-Typ kristallisieren. Anlaß für eine Neuuntersuchung war das für salzartige Hydride wesentlich zu geringe Volumeninkrement des Wasserstoffs in der angegebenen Struktur von CsCaH3. Die Ergebnisse unserer Untersuchungen zeigen, daß es sich um die Verbindung Cs2CaH4 handelt, die im K2NiF4-Typ mit dem für Wasserstoff zu erwartenden Volumeninkrement kristallisiert. Die vollständige Strukturbestimmung gelang über ein Neutronenbeugungsexperiment, bei dem das Deuterid Cs2CaD4 eingesetzt wurde.
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    URL: http://dx.doi.org/10.1002/zaac.19976230119
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    The Synthesis and Crystal Structure of Hg3TeI4Professor Rudolf Hoppe zum 75. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1843-1846 
    Details
    ISSN: 0044-2313
    Keywords: Mercury iodide telluride ; crystal structure ; ccp anion packing with partially filled tetrahedral holes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Kristallstruktur von Hg3TeI4Die Struktur von kubischem Hg3TeI4 wurde aus Pulverdaten bestimmt. Auf die vier Positionen der kubisch-dichtesten Packung der Anionen sind 0.8 Te-Atome und 3.2 I-Atome statistisch verteilt. Die beiden Sorten von Tetraederlücken sind zu 2/4 bzw. 0.4/4 von Hg-Atomen besetzt. Mit einem Ordnungsmodell niederer Symmetrie kann die stöchiometrische Zusammensetzung erklärt und eine homogene Ladungsverteilung erreicht werden. Das Ordnungsmodell enthält Regionen der Struktur von rotem HgI2, die durch Fragmente vom SiS2-Typ miteinander verbunden sind.
    Notes: The structure of cubic Hg3TeI4 was determined from powder data. The four positions of the cubic closestpacking of the anions are statistically occupied by 0.8 Te-atoms and 3.2 I-atoms. The two types of tetrahedral holes are occupied to the extent of 2/4 and 0.4/4, respectively, by Hg-atoms. With an ordered model of lower symmetry, the stoichiometric composition can be explained and a homogeneous charge distribution can be achieved. The ordered model contains regions of the structure of red HgI2, which are connected by fragments of the SiS2-type.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231129
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  • 122
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    Crystal Structure of Mixed Crystals of the Tetra(n-butyl)ammonium Salts of cis-Tetrafluorophthalocyaninato(2-)tantalate(V) and cis-Trifluorophthalocyaninato(2-)tantalate(IV) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1853-1854 
    Details
    ISSN: 0044-2313
    Keywords: Phthalocyaninates ; tantalum compounds ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: cis-Trichlorophthalocyaninato(2-)tantalate(V) reacts with excess tetra(n-butyl)ammonium fluoride trihydrate yielding mixed crystals of the tetra(n-butyl)ammonium salts of cis-tetrafluorophthalocyaninato(2-)tantalate(V) and cis-trifluorophthalocyaninato(2-)tantalate(IV) in the ratio five to four. These crystallize in the monoclinic space group P21/ n with cell parameters: a = 13.368(2) Å, b = 13.787(2) Å, c = 23.069(3) Å, β = 93.35(1)°, Z = 4. Tav is octacoordinated with four F atoms and four Niso atoms in an antiprismatic cis-arrangement. The Tav-F distance varies from 1.919(7) to 1.966(4) Å. TaIV is heptacoordinated with three F atoms in a cis-arrangement. The TaIV-F distance varies from 1.74(1) to 1.966(4) Å. The Ta atom is located out of the centre of the N4 plane towards the F atoms by 1.234(3) Å. The Ta-N distances range from 2.261(6) to 2.310(6) Å.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231204
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  • 123
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    P—H-funktionalisierte Phosphanidoliganden in der Übergangsmetallchemie: Molekülstruktur von CpZr(μ-PHtBu)2(μ-PtBu)2 {Zr(μ-Cl)Cp}2Professor Roger Blachnik zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 277-280 
    Details
    ISSN: 0044-2313
    Keywords: Trinuclear zirconium complex ; phosphanido ligand ; phosphinidene ligand ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: P—H-functionalised Phosphanido Ligands in Transition Metal Chemistry: Molecular Structure of CpZr(μ-PHtBu)2(μ-PtBu)2 {Zr(μ-Cl)Cp}2The reaction of polymeric [CpZrCl3]n with solvent-free LiPHtBu yields the trinuclear ZrIII/ZrIV complex CpZr(μ-PHtBu)2(μ-PtBu)2 {Zr(μ-Cl)Cp}2 (1) in a redox reaction in low yield. The oxidation product (PHtBu)2 is observed by 31P-NMR spectroscopy. 1 crystallises tetragonal in the space group P43212 with a = 1130.5(5) pm and c = 3415.7(5) pm.
    Notes: Die Reaktion von polymerem [CpZrCl3]n mit solvatfreiem LiPHtBu liefert in einer Redoxreaktion den dreikernigen ZrIII/ZrIV-Komplex CpZr(μ-PHtBu)2(μ-PtBu)2{Zr(μ-Cl)Cp}2 (1) in geringer Ausbeute. 31P-NMR-spektroskopisch kann die Bildung des Oxidationsprodukts (PHtBu)2 gezeigt werden. 1 kristallisiert tetragonal in der Raumgruppe P43212 mit a = 1130,5(5) pm und c = 3415,7(5) pm.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230144
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    Synthese und Strukturuntersuchungen von Iodocupraten(I). XVII. Die Kristallstrukturen polymerer Iodo-thiocyanato-metallate(I) mit heterocubanartigen Baueinheiten: [(C2H5)4N+]2∞3[Cu4I4(SCN)4/22-] · 2(CH3)2CO und [(C2H5)4N+]2∞2[Ag 4I4(SCN)4/22-] · (CH3)2COProfessor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 687-694 
    Details
    ISSN: 0044-2313
    Keywords: Iodo-thiocyanato cuprate(I) ; Iodo-thiocyanato argentate(I) ; crystal structure ; heterocubane type anions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Investigations on Iodocuprates(I). XVII. Crystal Structures of Polymeric Iodo-thiocyanato Metallates(I) with Heterocubane-like Structure Units: [(C2H5)4N+]2∞3[Cu4I4(SCN)4/22-] · 2(CH3)2CO and [(C2H5)4N+]2∞2[Ag 4I4(SCN)4/22-] · (CH3)2COThe reaction of CuSCN and AgSCN with (C2H5)4NI in acetone results in the formation of new Iodothiocyanato cuprates(I) or argentates(I) with polymeric anion lattices and areas of holes in which the cations and solvent molecules are inserted.[(C2H5)4N+]2∞3[Cu 4I4(SCN)4/22-] · 2(CH3)2CO 1 crystallizes in the monoclinic space group P21 with a = 1205.7(1), b = 2489.1(3), c = 1238.0(1) pm; β = 93.04(1)°; V = 3710.1(8) 106 pm3; Z = 2. Two different, negatively charged heterocubane units [Cu4I4(SCN)4/22-] are three-dimensionally connected by 1,3-μ-thiocyanato ligands forming a crystal structure with hose-shaped channels where cations and acetone molecules are placed.[(C2H5)4N+]2∞2[Ag 4I4(SCN)4/22-] · (CH3)2CO 2 crystallizes in the orthorhombic space group C2221 with a = 1206.7(1), b = 1398.2(1), c = 2318.8(2) pm; V = 3912.4(7) · 106 pm3; Z = 8. In this compound 1,3-μ-thiocyanato-bridged heterocubane units [Ag4I4(SCN)4/22-] form a layer structure with channel-shaped cavities vertical to them. Within these hollows there is again place for the cations and acetone molecules.
    Notes: Umsetzungen von CuSCN und AgSCN mit Tetraethylammoniumiodid in Aceton führen zu neuartigen, Iodo-thiocyanato-cupraten(I) bzw. -argentaten(I) mit polymeren Anionengittern, in deren Hohlräumen Kationen und Lösungsmittelmoleküle Platz finden.[(C2H5)4N+]2∞3[Cu 4I4(SCN)4/22-] · 2(CH3)2CO 1 kristallisiert in der monoklinen Raumgruppe P21; a = 1205,7(1), b = 2489,1(3), c = 1238,0(1) pm; β = 93,04(1)°; V = 3710,1(8) 106 pm3; Z = 2. Die Kristallstruktur ist aus zwei unterschiedlichen, zweifach negativ geladenen Heterocuban-Einheiten [Cu4I4(SCN)4/22-] aufgebaut. Diese sind über 1,3-μ-Thiocyanat-Liganden dreidimensional vernetzt. Zwischen den eckenverknüpften Heterocuban-Einheiten verlaufen schlauchförmige Kanäle, in denen sich die Kationen und Lösungsmittelmoleküle (Aceton) befinden.[(C2H5)4N+]2∞2[Ag 4I4(SCN)4/22-] · (CH3)2CO 2 kristallisiert in der orthorhombischen Raumgruppe C2221 mit den Zellparametern a = 1206,7(1), b = 1398,2(1), c = 2318,8(2) pm; V = 3912,4(7)· 106 pm3; Z = 8. In dieser Verbindung bilden 1,3-μ-SCN-verbrückte Heterocuban-Gruppen [Ag4I4(SCN)4/22-] polymere Schichten mit senkrecht dazu angeordneten, kanalförmigen Hohlräumen, in denen Kationen und Lösungsmittelmoleküle (Aceton) Platz finden.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301109
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    Ta5Se1.2Te1.8 - eine tetraedrisch dicht gepackte metallreiche SchichtstrukturProfessor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 742-748 
    Details
    ISSN: 0044-2313
    Keywords: Tantalum-rich chalcogenides ; selenides ; tellurides ; high temperature synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ta5Se1.2Te1.8 - a Tetrahedrally Close-packed Metal-rich Layer StructureTa5Se1.2Te1.8 was prepared by reducing a mixture of TaSe2 and TaTe2 with tantalum at 1540°C. A X-ray single crystal structure analysis was performed. Space group; P1, a = 1008.5(4) pm, b = 1052.1(4) pm, c = 1440,2(5) pm, α = 90.32(2)°, β = 96.42(2)°, γ = 108.28(2), Z = 8, Pearson-Symbol; aP64, 5684 reflexions, 300 variables, RI = 0.066. The structure is built up of hetero-nuclear, distorted icosahedral clusters penetrating mutually into pentagonal anti-prismatic columns. The connection of these units by inter-columnar Ta-Ta- and Ta-Se, Te-contacts affords tetrahedral close-packed layers. The chalcogen atoms are one-sidedly coordinated by three, four or six tantalum atoms.
    Notes: Ta5Se1.2Te1.8 wurde aus einem Gemenge aus TaSe2 und TaTe2 durch Reduktion mit Tantal bei 1540°C dargestellt. Die Struktur wurde aus Röntgenbeugungsintensitäten eines Einkristalls aufgeklärt. Raumgruppe: P1, a = 1008,5(4) pm, b = 1052,1(4) pm, c = 1440,2(5) pm, α = 90,32(2)°, β = 96,42(2)°, γ = 108,28(2), Z = 8, Pearson-Symbol: aP64, 5684 Reflexe, 300 Variablen, RI = 0,066. Die Struktur besteht aus zentrierten, verzerrt ikosaedrischen, heteronuklearen Clustern, die sich zu Strängen durchdringen. Die pentagonal-antiprismatischen Stränge sind untereinander über interkolumnare Ta-Ta- und Ta-Se, Te-Kontakte zu tetraedrisch dicht gepackten Schichten verknüpft. Die Chalkogen-Atome sind stels einseitig drei-, vier-, oder sechsfach von Tantal-Atomen koordiniert.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301117
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  • 126
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    The Reaction of P3N3Cl4(NH2)2 with HCl; The Crystal Structure of P3N3Cl5(NH2) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 637-641 
    Details
    ISSN: 0044-2313
    Keywords: 2-amino-2,4,4,6,6-pentachloro-2λ5,4λ5,6λ5-cyclo-triphosphaza-l,3,5-trien ; 2,4-diamino-4,4,6,6-tetrachloro-2λ5,4λ5,6λ5-cyclotriphosphaza-l,3,5-trien ; 2,4-diamino-4,4,6,6-tetrachloro-2λ5,4λ5,6λ5-cyclotriphosphaza-l,3,5-trien-l-ium-chloride ; preparation ; crystal structure ; molecular structure ; vibrational spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die Reaktion von P3N3Cl4(NH2)2 mit HCl; Die Kristallstruktur von P3N3Cl5(NH2)P3N3Cl5(NH2) kann in hoher Reinheit und mit guten Ausbeuten durch Reaktion von P3N3Cl4(NH2)2 mit gasförmigem HCI in Acetonitril erhalten werden. Wird, Diethylether oder Dichlormethan als Lösungsmittel verwendet, scheidet sich die salzartige Verbindung [P3N3CI4H(NH2)2]+Cl als mikrokristallines Produkt aus. Die Kristallstruktur von P3N3Cl5(NH2) wurde durch Röntgen Kristallstrukturanalyse untersucht. Schwingungsspektren und thermisches Verhalten sowohl des P3N3Cl5 (NH2) als auch des [P3N3Cl4H(NH2)2]+Cl - werden kurz diskutiert.
    Notes: P3N3Cl5(NH2) in high purity and a good yield can be obtained by the reaction of P3N3Cl4(NH2)2 with gaseous HCl in acetonitrile. If diethylether or dichlormethane is used as a solvent, a salt-like compound [P3N3Cl4H(NH2)2]+Cl - is formed as a microcrystalline product instead of P3N3Cl5(NH2). The crystal structure of P3N3Cl5(NH2) was determined by X-ray structure analysis. Vibrational spectra and thermic behavior of both P3N3Cl5(NH2) and [P3N3Cl4H(NH2)2]+Cl - are also briefly discussed.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301101
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    Crystal, molecular, and electronic structure of Trans-bis[ethanone, 1-(2-hydroxyphenyl)-oximato]Nickel(II) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 627-632 
    Details
    ISSN: 0044-2313
    Keywords: 2-Hydroxyacetophenoneoxime complex ; nickel complex ; Ni(C8H8NO2)2 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristall-, Molekular- und Elektronenstruktur von Trans-Bis[ethanon,1-(2-hydroxyphenyl)oximato]nickel(II)[Ni(apox)2] (apox = Anion des 2-Hydroxyacetophenonoxims, C8H8NO2-) wurde dargestellt und durch spektroskopische Messungen (IR, 1H NMR, UV-Vis) und theoretische Berechnungen mit der Hückel-Methode untersucht. Die Struktur wurde durch Röntgenstrukturanalyse ermittelt. Elementarzelle: monoklin, Raumgruppe P21/c mit a = 7,845(1), b = 9,911(2), c = 19,371(2)Å, β = 94,37(1)°, Z = 4. Hückel-Rechnungen im Zusammenhang mit dem Elektronenspektrum zeigen, daß die Banden bie 2,73 und 2,62 μm-1 als MLCT und bie 1,62 μm-1 als d-d-Übergang charakterisiert werden können, während die bie 2,14 μm-1 einen gemischten Charakter von MLCT und d-d-Übergang aufweist.
    Notes: The compound [Ni(apox)2], (where apox - denotes the anion of 2-hydroxyacetophenoneoxime, C8H8NO2-), was prepared and studied by means of spectroscopic (IR, 1H NMR, UV-Vis) measurements and theoretical calculations employing the Hückel method. The structure was determined by X-ray diffraction studies. The unit cell is monoclinic (space group P21/c) with dimensions a = 7.845(1), b = 9.911(2), c = 19.371(2) Å, β = 94.37(1)° and contains four formula units. Hückel investigations in comparison with the electronic excitation spectrum revealed that the two bands at 2.73 and 2.62 μm-1 can be characterised as MLCT, the band at 1.62 μm-1 as d-d transition, while the band at 2.14 cm-1 has a mixed character of both MLCT and d-d transition.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230199
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    Darstellung und Strukturanalyse von Tetrakis-(N-Methylimidazolium)-silacyclopentandichlorid · 2 NMI (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 633-636 
    Details
    ISSN: 0044-2313
    Keywords: Tetrakis-(N-methylimidazolium)-silacyclopentane-dichloride · 2 NMI ; 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 Tetrakis-(N-Methylimidazolium)-silacyclopentanedichloride · 2 NMIThe reaction of 1,1-dichlorosilacyclopentane with N-methylimidazole in aprotic solvents leads to a 1 : 4 compound, stable at room temperature. The silicon-center of the resulting dication enlarges the coordination number from four to six. Therefore we find the chloride-ions removed from the first area of coordination. They have lost their bonding to the silicon atom. This species is the first Lewisacid/base compound consisting of a heterocyclic alkylsilicon-halide and a nitrogen-base. Two single NMI-molecules per dication are present in the unit cell with no coordination at all. That leads to an exact 1 : 6-ratio of silane to base.
    Notes: 1,1-Dichlorsilacyclopentan reagiert unter Anlagerung von vier N-Methylimidazol (NMI)-Molekülen in aprotischer Lösung zu einem sechsfach koordinierten Siliciumdikation, bie dem beiden Chloridionen aus der ersten Koordinationssphäre verdrängt werden. Hier liegt der erste Verbindungstyp eines Lewis-Säure/Lewis-Base-Adduktes bestehend aus einem heterocyclischen Alkylhalogensilan mit einer Stickstoffbase vor. Zwei weitere NMI-Moleküle befinden sich pro Dikation in der Elementarzelle, was einem exakten Verhältnis von Silan zu NMI von 1 : 6 entspricht.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301100
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    Synthesis and Crystal Structure of Te8[ReCl6], containing the heavy homologue Te82+ of the chalcogen polycations S82+ and Se82+Dedicated to Professor Alois Haas on the Occasion of his 65th Birthday (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 409-413 
    Details
    ISSN: 0044-2313
    Keywords: Octatellurium (2+) ; hexachlororhenate (IV) ; chalcogen polycations ; main group element clusters ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Kristallstruktur von Te8[ReCl6], einer Verbindung mit dem schweren Homologen der Chalkogen-Polykationen S82+ und Se82+Durch Reaktion von ReCl4 mit Te und TeCl4 in einer evakuierten, geschlossenen Glasampulle erhält man bei 230°C silberne, metallisch glänzende und luftempfindliche Kristalle von Te8[ReCl6]. Die Kristallstrukturbestimmung zeigt (monoklin, C2/c, Z = 8, a = 1232,5(9) pm, b = 976,4(4) pm, c = 3114(2) pm, β = 90,85(5)°), daβ die Verbindung aus oktaedrischen [ReCl6]2-- und aus Te82+-Ionen aufgebaut ist. Die Kationen sind achtgliedrige Ringe mit einer exo-endo-Konformation und isostrukturell zu den bereits bekannten leichteren Homologen S82+ und Se82+. Die mittlere Te—Te-Bindungslänge beträgt 272 pm, der kürzeste transannulare Te—Te-Abstand 315 pm. Te8[ReCl6] enthält eine neue Form des Te82+-Polykations, dessen Struktur von der des Te82+ in Te8[WCl6]2 abweicht, wo eine ausgeprägt bizyklische Struktur mit einer transannularen Bindung von 299 pm und Kation-Kation-Kontakten, die zu einer gewellten Kette Tenn/4+ führen, gefunden wurde. In der Struktur von Te8[ReCl6] sind die Kationen dagegen voneinander isoliert und nur von Anionen umgeben.
    Notes: The reaction of ReCl4 with Te and TeCl4 in a sealed evacuated glass ampoule at 230°C yields silvery, lustrous, moisture sensitive crystals of Te8[ReCl6]. The crystal structure determination (monoclinic, C2/c, Z = 8, a = 1232.5(9) pm, b = 976.4(4) pm, c = 3114(2) pm, β = 90.85(5)°) shows, that the compound consists of octahedral [ReCl6]2 and of Te82+ ions. The cations are eight-membered rings in an exo-endo conformation and are isostructural to the already known S82+ and Se82+. The mean Te—Te bond length in the ring is 272 pm, the shortest transannular Te—Te bond is 315 pm. Te8[ReCl6] contains a new form of the Te82+ polycation. In contrast, the cations in the previously reported Te8[WCl6]2 have a pronounced bicyclic structure and intercationic bonds leading to an ondulated polymeric Tenn/4+ chain while the cations in the structure of Te8[ReCl6] are isolated from each other and surrounded by anions only.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230165
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    Die Kristallstruktur von β-Al2Te3Professor Rainer Mattes zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1006-1010 
    Details
    ISSN: 0044-2313
    Keywords: Aluminium telluride ; crystal structure ; layer structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of β-Al2Te3The crystal structure of β-Ab2Te3 has been determined by means of single crystal x-ray diffractometry. The examined crystal can be described as a pseudomerohedric twin with a plane of reflection in (001) as twin element. The refinement in P21/c (No. 14) with the crystal parameters a = 7.181(1) Å, b = 12.848(3) Å. c = 14.167(3) Å, β = 90.04(2)°, V = 1307.1 Å3 and Z = 8 resulted in a final R-value (based on F) of 0.0245. β-Al2Te3 crystallizes in a layered arrangement and represents a new structure type.
    Notes: Die Kristallstruktur von β-Al2Te3 konnte auf der Grundlage von Einkristalldaten ermittelt werden. Der vermessene Kristall lag als pseudomeroedrischer Reflektionszwilling nach (001) vor. Die Verfeinerung in P21/c (Nr. 14) mit a - 7,181(1) Å, b = 12,848(3) Å, c = 14,167(3) Å, β = 90,04(2)°, V = 1307,1 Å3 und Z = 8 konvergierte gegen einen konventionellen R-Wert von 0,0245. β-Al2Te3 kristallisiert in einer Schichtstruktur und stellt einen neuartigen Strukturtyp dar.
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    URL: http://dx.doi.org/10.1002/zaac.199762301157
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  • 131
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    Zur Struktur und Phasenbreite von Na2Gd4Cl9NO (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1011-1016 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanoide ; gadolinium nitride oxide halide ; Na2Gd4Cl9NO ; crystal structure ; oxide nitride ; condensed clusters ; range of homogeneity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure and Range of Homogeneity of Na2Gd4Cl9NONa2Gd4Cl9NO could be prepared as colourless compound by heating NaCl, GdN. Gd2O3 and GdCl3 in the ratio of 6 : 3 : 1 : 7 for several months at 810 K in a closed tantalum crucible (space group P21/m, a = 796,1(6) pm, b = 1112.3(5) pm, c = 916.1(7) pm, β = 106.45(6)°, Z = 2 and V = 778.0(9) · 106 pm3). The structure is built from chains of trans edge-shared [Gd4Z]-tetrahedra (Z = N or O). It is isotypic with Na2Pr4Cl9O2 and Na2Pr4Br9NO. X-ray structure determinations from two different single crystals give a hint to a range of homogeneity, Na2-xGd4Cl9N1-xO1+x, which conserves the purely salt like character of the compound via Na+ vacancies.
    Notes: Na2Gd4Cl9NO wurde durch Tempern von Nacl, GdN, Gd2O3 und GdCl3 im Verhältnis 6:3:1:7 bei 810 K im zugeschmolzenen Tantaltiegel in Form farbloser Kristalle erhalten (Raumgruppe P21/m, a = 796.1(6) pm, b = 1112.3(5) pm, c = 916.1(7) pm, β = 106.45(6)°, Z = 2, V = 778.0(9) · 106 pm3). Die Struktur ist aus Ketten trans-kantenkondensierter [Gd4Z]-Tetraeder (Z = N, O) aufgebaut Die Phase ist isotyp mit den bereits beschriebenen Verbindungen Na2Pr4Cl9O2 und Na2Pr4Br9NO. Röntgenstrukturanalysen zweier Kristalle geben Hinweise auf das Vorliegen einer Phasenbreite Na2-xGd4Cl9N1-xO1+x mit Erhalt des Charakters einer normalen Valenzverbindung.
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    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.199762301158
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  • 132
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    Organostannate derivatives of dicyclohexylammonium hydrogen 2,6-pyridinedicarboxylate: solution/solid-state 13C,119Sn NMR and in vitro antitumour activity of bis(dicyclohexylammonium) bis(2,6-pyridinedicarboxylato)dibutylstannate, and the crystal structure of its monohydrate (1997)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 11 (1997), S. 39-45 
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    ISSN: 0268-2605
    Keywords: organotin ; solid-state NMR ; crystal structure ; antitumor activity ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bis(dicyclohexylammonium) bis(2,6-pyridinedicarboxylato)dibutylstannate is assigned seven-fold coordination at tin on the basis of its 119Sn CP/MAS NMR chemical shift (δ=-424.9 ppm). The assignment has been corroborated by a crystal structure determination of its monohydrate, whose tin atom has the trans-C2SnNO4 pentagonal bipyramidal [Sn-C=2.040(9), 2.067(8) Å; C-Sn-C =168.9(5)°] geometry. One 2,6-pyridine- dicarboxylato group chelates to the tin atom (Sn-O=2.234(4), 2.260(4); Sn-N =2.279(5) Å) whereas the other binds through only one carboxyl -CO2 end (Sn-O=2.416(5), 2.441(5) Å). Hydrogen bonds link the cation and the stannate into a linear chain parallel to the b-axis. The lattice water molecule is hydrogen-bonded to the free carboxyl end. The anhydrous compound showed higher in vitro antitumor activity than those of carboplatin and cisplatin when screened against breast (MCF-7, EVSAT), colonic (WiDr), ovarian (IGROV) and renal (A498) carcinoma, and melanoma (M19 MEL) cell lines. © 1997 by John Wiley & Sons, Ltd.
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    Synthesis, Characterization and Biological Activity of Organotin Derivatives of 2-Thionaphthalene, Including the Crystal Structures of (Naphthalenethiolato-S)triphenyltin(IV) and Bis(naphthalenethiolato-S)dimethyltin(IV) (1997)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 11 (1997), S. 47-55 
    Details
    ISSN: 0268-2605
    Keywords: organotin ; 2-thionaphthalene ; synthesis ; crystal structure ; biological activity ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of di- and tri-organotin complexes of 2-thionaphthalene of general formula RR′R″SnL (R=R′=R″=C6H5, CH3, n-C4H9, C6H11, C6H5CH2; R=R′=C6H5CH2, R″=Cl; R=R′=Me, R″=C10H7S and L=2-thio-naphthalene, C10H7S) have been prepared by the reaction of di-or tri-organotin chloride(s) with 2-thionaphthalene. All compounds have been characterized by elemental analysis, IR, MS, NMR (1H, 13C, 119Sn) and 119Sn Mössbauer spectroscopies. X-ray crystal structures of the representative compounds (C6H5)3SnL and (CH3)2SnL2 confirm a tetrahydral geometry about tin. The biological activities of these compounds against various bacteria and fungi have been investigated. © 1997 by John Wiley & Sons, Ltd.
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    Mono-organotin(IV) and tin(IV) derivatives of 2-mercaptopyridine and 2-mercaptopyrimidine: X-ray structures of methyl-tris(2-pyridinethiolato)tin(IV) and phenyl-tris(2-pyridinethiolato)tin(IV)·1.5CHCl3 (1997)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 11 (1997), S. 869-888 
    Details
    ISSN: 0268-2605
    Keywords: organotin ; pyridine-2-thiolate complexes ; pyrimidine-2-thiolate complexes ; crystal structure ; Mössbauer ; IR ; NMR ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mono-organotin(IV) and tin(IV) derivatives of 2-mercaptopyridine (HSPy) and 2-mercaptopyrimidine (HSPym), RSnL3 (R=Me, n-Bu, Ph; L=SPy, SPym; R=Bz=benzyl, o-ClBz, o-ClC6H4, p-ClC6H4, o-tolyl, p-tolyl; L=SPy), RSnClL2 (R=Me, n-Bu, Ph; L=SPy, SPym), RSnCl2L (R=Me, n-Bu; L=SPy, SPym) and SnCl4-nLn (L=SPy, SPym; n=2, 4) were obtained from RSnCl3 or SnCl4 and NaL or by neutralization (R=Ph, p-tolyl; L=SPy, SPym). RSnClL2 and RSnCl2L were better prepared by comproportionation of RSnCl3 and RSnL3.MeSn(SPy)3 and PhSn(SPy)3·1.5CHCl3 crystals, as determined by single-crystal X-ray diffraction, are monoclinic. In the discrete monomeric RSn(SPy)3 units, three bidentate SPy ligands together with R form a distorted pentagonal bipyramid around tin. One S and the C(R) atom are in the axial positions. Two S atoms and three N atoms form the pentagonal plane.From 119Sn Mössbauer and IR data, analogous structures are inferred for the other solid RSnL3 compounds, except for R=Bz, o-ClBz, o-ClC6H4 and o-tolyl, in which tin would be hexacoordinated. In the compounds RSnClL2 and RSnCl2L, tin is at the center of an octahedron or a trigonal bipyramid, respectively. For Sn(SPym)4 and SnCl2(SPym)2, the same type of octahedral structure as was previously found for Sn(SPy)4·HSPy and SnCl2(SPy)2 is proposed.According to IR and 1H, 13C and 119Sn NMR data, the solid-state molecular structures are retained in chloroform and dimethyl sulfoxide solution. © 1997 John Wiley & Sons, Ltd.
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