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  • Inorganic Chemistry  (12)
  • Synthesis  (2)
  • Arenkomplexe
  • 1995-1999  (12)
  • 1996  (12)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 253-257 
    ISSN: 0009-2940
    Keywords: Lithiated phosphane imines ; Phosphane imines, lithiated ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Lithiated Phosphane Imines. Synthesis and Crystal Structures of [LiCH2PMe2NSiMe3]4 and [LiCMe2P(iPr)2NSiMe3]2The title compounds were prepared by the reaction of Me3-SiNPMe3 and Me3SiNP(iPr)3, respectively, with n-Butylli-thium at 20°C in n-hexane solution. They form white, moisture- and oxygen-sensitive crystals, which were characterized by IR spectroscopy and by crystal structure determinations. - [LiCH2PMe2NSiMe3]4 (1) forms a Li4 tetrahedron, the faces of which are capped with CH2 groups with average Li-C distances of 233 and 251 pm, while the nitrogen atoms occupy the corners of the Li4 tetrahedron. - [LiCMe2P(iPr)2N-SiMe3]2 (2) forms molecules of symmetry C2 in which the lithium atoms have coordination number three by two carbon atoms and one nitrogen atom with Li-C distances of 215.2 and 237.9 pm and Li-N of 192.8 pm.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1621-1625 
    ISSN: 0009-2940
    Keywords: Organo-zinc compounds ; Phosphaneiminato complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organo-Zinc Phosphaneiminato Complexes with Heterocubane StructureThe organo-zinc heterocubanes [ZnR(NPMe3)]4 with R = CH3 (1) and n-C4H9 (2) were prepared by the reaction of [ZnBr(NPMe3)]4 with MeLi and nBuLi, respectively, in hexane solution. In a similar reaction of nBuLi with [ZnI(NPMe3]4 the phosphaneiminato complex [Zn4I(nBu)4(NPMe3)3] (3) is formed. 1-3 were characterized by IR, NMR and MS spectroscopy, and by crystal-structure determinations. 1 and 2 possess heterocubane structures in which the zinc atoms are linked via μ3-N bridges of the phosphaneiminato groups, and all bond angles in the Zn4N4 core are close to 90°. A distorted heterocubane structure is observed for 3 with one of the NPMe3 moieties replaced by an iodine atom.
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  • 3
    ISSN: 0009-2940
    Keywords: Amido complexes ; Titanium(III) compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Syntheses, Properties, and Crystal Structures of the Titanium(III) Amido Complexes Ti[N(SiMe3)2]3, [TiCl2{N(SiMe3)2}(THF)2], and [Na(12-Crown-4)2][TiCl2{N(SiMe3)2}2]TiCl3(THF)3 reacts with NaN(SiMe3)2 to furnish [TiCl2{N(SiMe3)2}(THF)2] (1), whereas in the presence of 12-crown-4 the ionic amido complex [Na(12-crown-4)2][TiCl2{N(SiMe3)2}2] (5) is obtained besides [Na(12-crown-4)2][TiCl4(THF)] (4). On the other hand, the titanium(III) amido complex Ti[N(SiMe3)2]3 (2), the crystal structure of which was solved, reacts with NaN(SiMe3)2 in the presence of 12-crown-4 with deprotonation of one of the methyl groups to give the carbometalated complex [Na(12-crown-4)2][Ti{N(SiMe3)2}2{N(SiMe 3CH2)}] (3).
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 259-262 
    ISSN: 0009-2940
    Keywords: Halide complexes of diiodacetylene ; Crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complexes of Halide Ions with Diiodoacetylene. The Crystal Structures of PPh4[X(I-C≡C-I)2] with X = Cl, Br, IThe complexes PPh4[X(I-C≡C-I)2] with X = Cl (1), Br (2), and I (3) have been prepared from the phosphonium salts PPh4X and 1-C≡C-I in dichloromethane solutions. 1-3 form colourless crystals, which according to crystal structure analysis crystallize isotypically in the space group P421m with two formula units per unit cell. The diiodacetylenes are coordinated by the halide ions X- in a distorted tetragonal fashion, the I-C≡C-I molecules being in μ2-bridging function. Thus, a polymeric anionic network [X(I-C≡C-I)2]nn- with a layered structure results.
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  • 5
    ISSN: 0009-2940
    Keywords: Halide complexes of 1-Halogen-2-phenylacetylenes ; Acetylenes, 1-halogen-2-phenyl-, halide complexes of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complexes of Halide Ions with 1-Halogen-2-phenylacetylenes. Crystal Structures of PPh4[X(I - C≡C - Ph)4] with X = Cl, Br, I, of PPh4[Br(Br - C≡C - Ph)4], and of NMe4[F(I - C≡C - Ph)2]Herrn Prof. Dr. H. Brunner zum 60. Geburtstag gewidmet.The complexes PPh4[X(I - C≡C - Ph)4] with X = Cl (1), Br (2), I (3), PPh4[Br(Br - C≡C - Ph)4] (4), and NMe4[F(I - C≡C - Ph)2] (5) were prepared from the corresponding salts PPh4X and NMe4F, respectively, with the 1-halogen-2-phenylacetylenes X - C≡C - Ph (X = Br, I) in dichloromethane solutions. 1 - 5 form colourless crystals, which were characterized by vibrational spectroscopy. According to the crystal structure determinations the halide ions in 1 - 4 are coordinated by the halogen atoms of the 1-halogen-2-phenylacetylenes in a tetragonal-pyramidal fashion. The fluoride ion in 5 is only twofold coordinated with a bond angle I - F - I of 110.45°.
    Additional Material: 8 Ill.
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  • 6
    ISSN: 0009-2940
    Keywords: Phosphane iminato complexes ; Arsenic compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Phosphane Iminato Complexes of Arsenic. Crystal Structures of [AsCl(NPMe3)]2Cl2, [AsCl(NPMe3)2SbCl4]SbCl6, and [AsCl(NPMe3)2SnCl4] · CH3CN[AsCl(NPMe3)]2Cl2 (1) was prepared by the reaction of arsenic trichloride with the silylated phosphane imine Me3-SiNPMe3 in acetonitrile solution. According to the crystal structure determination, 1 has an ionic structure with [AsCl(NPMe3)]22+ ions, in which the As atoms are linked by the μ2-N atoms of the NPMe3- groups. Compound 1 reacts with antimony pentachloride to give [AsCl(NP-Me3)2SbCl4]+SbCl6- (2), with tin tetrachloride to form [AsCl(NPMe3)2SnCl4] (3), which is isoelectronic to the cation of 2. In 2 and 3 AsCl(NPMe3)2 acts as a chelating agent forming and , respectively, four-membered ring structures.
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  • 7
    ISSN: 0009-2940
    Keywords: Amido Complexes ; Manganese Compounds ; Iron Compounds ; Cobalt Compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Syntheses and Crystal Structures of the Amido Complexes [Na(12-Crown-4)2][M{N(SiMe3)2}3] with M = Mn, Fe, and CoThe ionic amido complexes [Na(12-crown-4)2][M[N-(SiMe3)2}3] with M = Mn (1), Fe (2) and Co (3) were prepared by the reaction of M[N(SiMe3)2]2 (M = Mn, Co) and Fe[N-(SiMe3)2]3, respectively, with sodium bis(trimethylsilyl)amide in toluene solution in the presence of 12-crown-4. 1-3 were characterized by IR spectroscopy and by crystal structure determinations. The complexes consist of cations [Na(12-crown-4)2]+ with a sandwich-like structure and anions [M{N(SiMe3)2}3]- in which the metal atoms are planarly coordinate by the three nitrogen atoms of the bis(trimethylsilyl)amido groups.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 863-866 
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complex of Sulfur ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [(Me3PN)3SNS(NPMe3)2]Cl2, a Mixed Valenced Phosphorane Iminato Complex of SulfurThe title compound has been prepared from trithiazyl chloride and the silylated phosphaneimine Me3SiNPMe3 in acetonitrile solution, forming red crystals, which were characterized by IR spectroscopy and by a crystal structure determination.Space group P21/c, Z = 4, structure solution with 4250 independent reflections, R = 0.054. Lattice dimensions at 20°C: a = 1077.8, b = 2036.6, c = 1480.5 pm, β = 102.39°. The compound consists of dications [(Me3PN)3SNS(NPMe3)2]2+ and chloride ions. In the cations the sulfur atoms of oxidation number +VI and +IV are connected by an asymmetric, bent nitrido bridge with SN bond lengths of 156.9 and 167.0 pm.
    Notes: Die Titelverbindung entsteht als rote Kristalle bei der Reaktion von Trithiazylchlorid mit dem silylierten Phosphanimin Me3SiNPMe3 in Acetonitrillösung. Die Verbindung wird durch das IR-Spektrum und durch eine Kristallstruktur-analyse charakterisiert.Raumgruppe P21/c, Z = 4, Strukturlösung mit 4250 unabhängigen Reflexen, R = 0,054. Gitterabmessungen bei 20°C: a = 1077,8; b = 2036,6; c = 1480,5 pm, β = 102,39°. Die Verbindung besteht aus den Dikationen [(Me3PN)3SNS(NPMe3)2]2+ und Chloridionen. In den Kationen sind die Schwefelatome der Oxidationszahl +VI und +IV über eine asymmetrische, gewinkelte Nitridobrücke mit SN-Abständen von 156,9 und 167,0 pm verknüpft.
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  • 9
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato-Phosphaneimine Complex of Titanium ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of [TiF3(NPPh3)(HNPPh3)]2 and of HNPPh3The phosphoraneiminato-phosphaneimine complex [TiF3(NPPh3)(HNPPh3)]2 was obtained by the reaction of TiF4 with Me3SiNPPh3 in boiling dichloromethane. It crystallizes from 1,2-dichloroethane as yellow crystals which include four molecules C2H4Cl2 per dimeric formula unit. Space group P21/n, Z = 2, structure solution with 7270 independent reflections, R = 0.060 for reflections with I 〉 2σ(I). Lattice dimensions at -50°C: a = 1417.5, b = 1896.9, c = 1586.6 pm, β = 101.22°. The compound forms centrosymmetric dimeric molecules via μ2-F bridges with TiF distances of 194.6 and 223.3 pm, the longer one being in trans-position to the N atom of the (NPPh3)- ligand. Its TiN bond length of 177.7 pm corresponds with a double bond. The TiN bond length of the HNPPh3 donor molecule of 213.4 pm is typical for a donor acceptor bond.According to the crystal structure determination the phosphaneimine HNPPh3 forms monomeric molecules without intermolecular hydrogen bridges with a PN bond length of 152.4 pm. Space group P21/c, Z = 4, structure solution with 3229 independent reflections, R = 0.062 for reflections with I 〉 2σ(I). Lattice dimensions at -70°C: a = 1460.4, b = 928.9, c = 1096.6 pm, β = 93.35°.
    Notes: Der Phosphaniminato-Phosphanimin-Komplex [TiF3(NPPh3)(HNPPh3)]2 wird aus TiF4 und Me3SiNPPh3 in siedendem Dichlormethan erhalten. Er kristallisiert aus 1,2-Dichlorethan als gelbe Kristalle unter Einschluß von vier Molekülen C2H4Cl2 pro dimere Formeleinheit. Raumgruppe P21/n, Z = 2, Strukturlösung mit 7270 unabhängigen Reflexen, R = 0,060 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -50°C: a = 1417,5; b = 1896,9; c = 1586,6 pm; β = 101,22°. Die Verbindung bildet zentrosymmetrische Dimere, in denen die Titanatome über μ2-F-Brücken mit TiF-Abständen von 194,6 und 223,3 pm verknüpft sind. Die lange Ti—F-Bindung befindet sich in trans-Position zum N-Atom des (NPPh3)--Liganden, dessen TiN-Bindung mit 177,7 pm einer Doppelbindung entspricht. Der vom HNPPh3-Liganden ausgehende Ti—N-Abstand beträgt 213,4 pm.Das Phosphanimin HNPPh3 bildet nach der Kristallstrukturanalyse monomere Moleküle mit einer PN-Bindungslänge von 152,4 pm ohne intermolekulare Wasserstoffbrücken. Raumgruppe P21/c, Z = 4, Strukturlösung mit 3229 unabhängigen Reflexen, R = 0,062 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -70°C: a = 1460,4; b = 928,9; c = 1096,6 pm; β = 93,35°.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1205-1208 
    ISSN: 0044-2313
    Keywords: Osmium Nitridotrichloride ; synthesis ; IR spectrum ; magnetic susceptibility ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Osmium Nitridotrichloride, OsNCl3OsNCl3 was prepared by the reaction of (NH4)2[OsNCl5] with chlorine at 300°C, forming a black, X-ray amorphous moisture sensitive, paramagnetic powder which was characterized by IR spectroscopy and measurement of the magnetic susceptibility in the range of 5-300 K.
    Notes: OsNCl3 wird als schwarzes, röntgenamorphes, feuchtigkeitsempfindliches paramagnetisches Pulver durch Reaktion von (NH4)2[OsNCl5] mit Chlor bei 330°C hergestellt und IR-spektroskopisch sowie durch magnetische Suszeptibilitätsmessungen im Bereich von 5-300 K charakterisiert.
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