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  • 1
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    Journal of the American Chemical Society 117 (1995), S. 1145-1146 
    ISSN: 1520-5126
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 2
    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).
    Additional Material: 4 Ill.
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  • 3
    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.
    Additional Material: 3 Ill.
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  • 4
    ISSN: 0044-8249
    Keywords: Arenkomplexe ; Brückenliganden ; Platin ; Silber ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 5
    ISSN: 0044-2313
    Keywords: [Mg3Cl5(Et2O)6] cation ; X-ray structure ; ab-initio calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Mg3Cl5(Et2O)6]+: Synthesis, Structure, and Ab-Initio CalculationsThe cation [Mg3Cl5(Et2O)6]+ of a chlorogallat has been prepared in a reaction of Ga2Cl4 with MgCp2* and was characterized by a X-ray single-crystal structure analysis. For understanding of the conditions of formation of neutral and charged magnesium chlorids and of the processes in the complex reaction system ab-initio calculations were performed.
    Notes: Das Kation [Mg3Cl5(Et2O)6]+ eines Chlorogallats wurde im Rahmen einer Umsetzung von Ga2Cl4 mit MgCp2* dargestellt und durch eine Kristallstrukturbestimmung röntgenographisch charakterisiert. Um die Bildungsbedingungen von neutralen und ionischen Magnesiumchloriden und die komplexen Reaktionsabläufe im Synthesegemisch zu verstehen, wurden quantenchemische ab-initio-Rechnungen angefertigt.
    Additional Material: 6 Ill.
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  • 6
    ISSN: 0044-2313
    Keywords: Magnesium Compounds ; Phosphoraneiminato Complexes ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphaneimine and Phosphoraneiminato Complexes of Magnesium. The Crystal Structures of [MgBr1,25I0,75(Me3SiNPMe3)(OEt2)], [MgI2(Me3SiNPMe3)2], [Mg2I2(Me3SiNPMe2CH2)(Me3SiNPMe2CH2CH(Me)O)(OEt2)], and [MgBr(NPMe3)]4 · C7H8By reactions of the silylated phosphaneimine Me3SiNPMe3 with the Grignard reagents EtMgBr and MeMgI, respectively, the carbanionic phosphoraneiminato derivatives [XMg(CH2PMe2NSiMe3)]n (X = Br, I) can be isolated as main products. The by-products of these reactions, [MgBr1.25I0.75(Me3SiNPMe3)(OEt2)], [MgI2(Me3SiNPMe3)2] and [Mg2I2(CH2PMe2NSiMe3)(O(Me)CHCH2PMe2NSiMe3)(OEt2)] were identified by crystal structure determinations. The phosphoraneiminato complex [MgBr(NPMe3)]4 · C7H8 with hetero cubane structure is formed by a metathesis reaction of [ZnBr(NPMe3)]4 with RMgBr (R = Ph. Mes).
    Notes: Als Hauptprodukte der Umsetzungen des silylierten Phosphanimins Me3SiNPMe3 mit den Grignard-Reagentien EtMgBr und MeMgl wurden die carbanionischen Phosphaniminato-Derivate [XMg(CH2Pme2NSiMe3)]n (X = Br, I) isoliert. Als Nebenprodukte wurden [MgBr1,25I0,75(Me3SiNPMe3)(OEt2)], [Mgl2(Me3SiNPMe3)2] und [Mg2I2(CH2PMe2NSiMe3)(O(Me)CHCH2PMe2NSiMe3(OEt2)] durch röntgenographische Strukturanalysen identifiziert. Den Phosphaniminato-Komplex [MgBr(NPMe3)]4 · C7H8 mit Heterocuban-Struktur erhielten wir durch Metathese-Reaktion aus [ZnBr(NPMe3)]4 und RMgBr (R = Ph, Mes).
    Additional Material: 4 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1306-1310 
    ISSN: 0044-2313
    Keywords: Lithium Cluster ; Carbdianion ; NMR spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Li7(CHPMe2NSiMe3)3(OSiMe2nBu)]2, a Mixed-Ligand-Li14 Cluster with the Carbdianion (CHPMe2NSiMe3)2-The title compound is formed as colourless moisture and oxygen sensitive crystals by the reaction of [LiCH2PMe2NSiMe3]4 with zinc or cobalt chloride in a toluene suspension in the presence of silicongrease (-OSiMe2-)n and n-butyllithium. It is characterized by multinucleus NMR spectroscopy and by crystal structure determinations of two different crystal individuals.1. Space group P1, Z = 1, lattice dimensions at -70 °C: a = 1272.0, b = 1392.6, c = 1417.6 pm, α = 115.33°, β = 96.75°, σ = 106.81°; R = 0.042.2. Space group P21/n, Z = 2, lattice dimensions at -50 °C: a = 1424.8, b = 1457.1, c = 1997.0 pm, β = 90.32, R = 0.069.
    Notes: Die Titelverbindung (farblose, feuchtigkeits- und sauerstoffempfindliche Kristalle) entsteht bei der Reaktion von [LiCH2PMe2NSiMe3]4 mit wasserfreiem Zink- oder Cobaltchlorid in einer Toluolsuspension in Gegenwart von Siliconfett (-OSiMe2-)n und n-Butyllithium. Sie wird durch Multikern-NMR-Spektroskopie und durch Kristallstrukturanalysen zweier kristallchemisch verschiedener Individuen charakterisiert.1. Raumgruppe P1, Z = 1, Gitterkonstanten bei -70 °C: a = 1272,0; b = 1392,6; c = 1417,6 pm; α = 115,33°; β = 96,75°; σ = 106,81°; R = 0,042.2. Raumgruppe P21/n, Z = 2, Gitterkonstanten bei -50 °C: a = 1424,8; b = 1457,1; c = 1997,0 pm; β = 90,32°; R = 0,069.
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  • 8
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes of Sulfur ; Syntheses ; IR Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorane Iminato Complexes of Sulfur. Synthesis and Crystal Structures of [SO(Cl)(NPPh3)], [SO2(Cl)(NPPh3)], and [SCl(NPPh3)2]ClThe title compounds have been prepared by the reaction of Me3SiNPPh3 with SOCl2, SO2Cl2, and SCl2, respectively. They form colourless, moisture sensitive crystals, which were characterized by IR spectroscopy and by crystal structure determinations.[SO(Cl)(NPPh3)]: Space group P21/n, Z = 4, structure determination with 2 434 observed unique reflections, R = 0.047. Lattice dimensions at 19°C: a = 1 304.8, b = 996.5, c = 1 339.5 pm, β = 93.75°. The compound forms monomeric molecules with a remarkably long S—Cl bond of 234.2 pm and distances SN and PN of 154.6 and 161.6 pm, respectively, which agree with double bonds.[SO2(Cl)(NPPh3)]: Space group P21/n, Z = 4, structure solution with 2 872 observed, unique reflections, R = 0.047. Lattice dimensions at 20°C: a = 956.9, b = 1 909, c = 1 002.0 pm, β = 106.06°. The compound forms monomeric molecules with distances S—Cl of 207.1 pm, SN of 154.5 pm, and PN of 161.6 pm.[SCl(NPPh3)2]Cl: Space group P21/c, Z = 4, structure solution with 5 224 observed, unique reflections, R = 0.042. Lattice dimensions at 20°C: a = 1 108.6, b = 1 603.8, c = 1 840.5 pm, β = 99.98°. The compound forms ions [SCl(NPPh3)2]+ and Cl-. In the cation the sulfur atom is ϕ-tetrahedrally coordinated with a long S—Cl distance of 248.5 pm and SN bond lengths of 154.5 and 156.0 pm.
    Notes: Die Titelverbindungen entstehen durch Umsetzung von Me3SiNPPh3 mit Thionylchlorid, Sulfurylchlorid bzw. Schwefeldichlorid als farblose, feuchtigkeitsempfindliche Kristalle, die wir durch die IR-Spektren und durch Kristallstrukturanalysen charakterisiert haben.[SO(Cl)(NPPh3)]: Raumgruppe P21/n, Z = 4, Strukturlösung mit 2 434 unabhängigen beobachteten Reflexen, R = 0,047. Gitterabmessungen bei 19°C: a = 1 304,8; b = 996,5; c = 1 339,5 pm, β = 93,75°. Die Verbindung bildet monomere Moleküle mit einer auffällig langen S—Cl-Bindung von 234,2 pm und Abständen SN und PN von 154,6 bzw. 161,6 pm, die Doppelbindungen entsprechen.[SO2(Cl)(NPPh3)]: Raumgruppe P21/n, Z = 4, Strukturlösung mit 2 872 unabhängigen beobachteten Reflexen, R = 0,047. Gitterabmessungen bei 20°C: a = 956,9; b = 1 909; c = 1 002,0 pm, β = 106,06°. Die Verbindung bildet monomere Moleküle mit Abständen S—Cl von 207,1 pm, SN von 154,5 pm und PN von 161,6 pm.[SCl(NPPh3)2]Cl: Raumgruppe P21/c, Z = 4, Strukturlösung mit 5 224 unabhängigen beobachteten Reflexen, R = 0,042. Gitterabmessungen bei 20°C: a = 1 108,6; b = 1 603,8; c = 1 840,5 pm, β = 99,98°. Die Verbindung bildet Ionen [SCl(NPPh3)2]+ und Cl-. Im Kation ist das Schwefelatom ϕ-tetraedrisch koordiniert mit einem langen S—Cl-Abstand von 248,5 pm und SN-Bindungslängen von 154,5 und 156,0 pm.
    Additional Material: 3 Ill.
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  • 9
    ISSN: 0044-2313
    Keywords: Alkoxy-Alkyne Complexes of Tungsten ; Synthesis ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of the Tungsten(VI)-alkyne Complexes [W2(O)(OMe)6(Et—Se—C≡C—Se—Et)2] and Li[W(OMe)5(Et—Te—C≡C—Te—Et)]The title compounds have been prepared by reactions of lithium methanolate with [WCl4(Et—Se—C≡C—Se—Et)(THF)] and [WCl4(Et—Te—C≡C—Te—Et)(THF)], respectively, in diethylether suspensions. Both complexes were characterized by crystal structure determinations.[W2(O)(OMe)6(Et—Se—C≡C—Se—Et)2]: Space group P1, Z = 2, structure determination with 4 320 observed unique reflections, R = 0.041. Lattice dimensions at -70°C: a = 949.3, b = 1 225.3, c = 1 285.0 pm, α = 82.48°; γ = 82.44°; β = 81.44°. The tungsten atoms are bridged by three μ2-O-atoms of the OMe groups; the alkyne ligands are coordinated side-on in a metallacyclopropene-like fashion.Li[W(OMe)5(Et—Te—C≡C—Te—Et)]: Space group P1, Z = 2, structure determination with 9 381 observed unique reflections, R = 0.038. Lattice dimensions at -70°C: a = 983.4, b = 1606.9, c = 1971.5 pm, α = 66.09°, β = 84.29°, γ = 79.83°. The lithium ions link the [W(OMe)5(Et—Te—C≡C—Te—Et)]- anions to a trimeric ion ensemble via the O atoms of three OMe groups of each anion.
    Notes: Die Titelverbindungen werden durch Reaktion von Lithiummethanolat mit [WCl4(Et—Se—C≡C—Se—Et)(THF)] bzw. mit [WCl4(Et—Te—C≡C—Te—Et)(THF)] in Diethylether hergestellt und durch Kristallstrukturanalysen charakterisiert.[W2(O)(OMe)6(Et—Se—C≡C—Se—Et)2]: Raumgruppe P1, Z = 2, Strukturlösung mit 4 320 beobachteten unabhängigen Reflexen, R = 0,041. Gitterabmessungen bei -70°C: a = 949,3; b = 1225,3; c = 1285,0 pm, α = 82,48°; β = 82,44°; γ = 81,44°. Die beiden Wolframatome sind über drei μ2-OMe-Brücken verknüpft; die Alkinliganden sind seitlich entsprechend von Metallacyclopropengruppen koordiniert.Li[W(OMe)5(Et—Te—C≡C—Te—Et)]: Raumgruppe P1, Z = 2, Strukturlösung mit 9 381 beobachteten unabhängigen Reflexen, R = 0,038. Gitterabmessungen bei -70°C: a = 983,4; b = 1606,9; c = 1971,5 pm, α = 66,09°; β = 84,29°; β = 79,83°. Die Lithiumionen verknüpfen die [W(OMe)5(Et—Te—C≡C—Te—Et)]--Anionen über die O-Atome dreier OMe-Gruppen zu einem trimeren Ionenensemble.
    Additional Material: 2 Ill.
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  • 10
    ISSN: 0044-2313
    Keywords: Phosphaneimine Complexes of Zinc and Cobalt ; Synthesis ; IR spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Phosphaneimine Complexes MCl2(Me3SiNPMe3)2 with M = Zn and Co, and CoCl2(HNPMe3)2The molecular complexes MCl2(Me3SiNPMe3)2 (M = Zn, Co) have been prepared by the reaction of the dichlorides of zinc and cobalt with Me3SiNPMe3 in CH3CN and CH2Cl2, respectively, whereas the complex CoCl2(HNPMe3)2 has been prepared by the reaction of CoCl2 with NaF in boiling acetonitrile in the presence of Me3SiNPMe3. All complexes were characterized by IR spectroscopy and by crystal structure determinations. The complexes MCl2(Me3SiNPMe3)2 crystallize isotypically.ZnCl2(Me3SiNPMe3)2: Space group P212121, Z = 4, 2677 observed unique reflections, R = 0.024. Lattice dimensions at -70°C: a = 1243.6; b = 1319.0; c = 1464.7 pm.CoCl2(Me3SiNPMe3)2: Space group P212121, Z = 4, 3963 observed unique reflections, R = 0,071. Lattice dimensions at -80°C: a = 1236.3; b = 1317.4; c = 1457.6 pm.CoCl2(HNPMe3)2 · CH2Cl2: Space group Pbca, Z = 8, 1354 observed unique reflections, R = 0.055. Lattice dimensions at -80°C: a = 1247.3; b = 998.4; c = 2882.4 pm.All complexes have monomeric molecular structures, in which the metal atoms are coordinated in a distorted tetrahedral fashion by the two chlorine atoms and by the nitrogen atoms of the phosphaneimine molecules.
    Notes: Die Molekülkomplexe MCl2(Me3SiNPMe3)2 (M = Zn, Co) entstehen aus den wasserfreien Dichloriden von Zink und Cobalt mit Trimethylsilyl-trimethylphosphanimin in Dichlormethan bzw. Acetonitril, während der Trimethylphosphanimin-Komplex CoCl2(HNPMe3)2 aus CoCl2 mit Natriumfluorid in Gegenwart von Me3SiNPMe3 in siedendem Acetonitril gebildet wird. Die Verbindungen werden durch ihre IR-Spektren und durch Kristallstrukturanalysen charakterisiert. Die Komplexe MCl2(Me3SiNPMe3)2 (M = Zn, Co) sind miteinander isotyp.ZnCl2(Me3SiNPMe3)2: Raumgruppe P212121, Z = 4, Strukturlösung mit 2677 beobachteten unabhängigen Reflexen, R = 0,024. Gitterkonstanten bei -70°C: a = 1243,6; b = 1319,0; c = 1464,7 pm.CoCl2(Me3SiNPMe3)2: Raumgruppe P212121, Z = 4, Strukturlösung mit 3963 beobachteten unabhängigen Reflexen, R = 0,071. Gitterkonstanten bei -80°C: a = 1236,3; b = 1317,4; c = 1457,6 pm.CoCl2(HNPMe3)2 · CH2Cl2: Raumgruppe Pbca, Z = 8, Strukturlösung mit 1354 beobachteten unabhängigen Reflexen, R = 0,055. Gitterkonstanten bei -80°C: a = 1247,3; b = 998,4; c = 2882,4 pm.Alle Komplexe haben monomere Molekülstrukturen, in denen die Metallatome verzerrt tetraedrisch von den beiden Chloratomen und den N-Atomen der beiden Phosphaniminmoleküle koordiniert sind.
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