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  • 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.
    Additional Material: 5 Ill.
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  • 2
    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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  • 3
    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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