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  • 1
    ISSN: 0044-2313
    Keywords: Silylated λ5-Phosphazenes ; Synthesis ; NMR spectra ; 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 Silylated λ5-Phosphazenes R—C(CH2PPh2NSiMe3)3 with R = H and CH3The title compounds are obtained by Staudinger reaction from the corresponding tripodal phosphanes R—C(CH2PPh2)3 and trimethylsilylazide. Both complexes are characterized by their IR and NMR spectra and by crystal structure analyses.H—C(CH2PPh2NSiMe3)3 (1): Space group P21/c, Z = 4, structure determination with 7833 independent reflections, R = 0.055. Lattice dimensions at -50°C: a = 1399.5, b = 2311.4, c = 1678.9 pm, β = 112.92°.CH3—C(CH2PPh2NSiMe3)3 (2): Space group P1, Z = 2, structure determination with 9251 independent reflections, R = 0.057. Lattice dimensions at -50°C: a = 1276.5, b = 1386.9, c = 1790.2 pm; α = 85.55°, β = 69.39°, γ = 62.99°.1 and 2 form monomeric molecules which are distinguished by their conformation.
    Notes: Die Titelverbindungen werden durch Staudinger-Reaktion aus den entsprechenden tripodalen Phosphanen R—C(CH2PPh2)3 und Trimethylsilylazid hergestellt und durch ihre IR- und NMR-Spektren sowie durch Kristallstrukturanalysen charakterisiert.H—C(CH2PPh2NSiMe3)3 (1): Raumgruppe P21/c, Z = 4, Strukturbestimmung mit 7833 unabhängigen Reflexen, R = 0,055. Gitterkonstanten bei -50°C: a = 1399,5; b = 2311,4; c = 1678,9 pm; β = 112,92°.CH3—C(CH2PPh2NSiMe3)3 (2): Raumgruppe P1, Z = 2, Strukturbestimmung mit 9251 unabhängigen Reflexen, R = 0,057. Gitterkonstanten bei -50°C: a = 1276,5; b = 1386,9; c = 1790,2 pm; α = 85,55°; β = 69,39°; γ = 62,99°.1 und 2 bilden monomere Moleküle, die sich durch ihre Konformation unterscheiden.
    Additional Material: 1 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1035-1036 
    ISSN: 0044-2313
    Keywords: Titanium compound ; Phosphorane iminato derivatives ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetrakis(triphenylphosphoraneiminato)titanium, [Ti(NPPh3)4]The title compound has been prepared by the reaction of [TiCl2(NPPh3)2] with methyllithium and cyclopentadienyllithium, respectively, in hexane solution. [Ti(NPPh3)4] · 3 C7H8 crystallizes from toluene solution to form colourless, only slightly moisture sensitive crystals which were characterized by a crystal structure determination. Space group I41/a, Z = 8, lattice dimensions at -80°C: a = b = 2160.7(2), c = 3334.2(3) pm, merohedral (110) twin, R = 0.077. The compound forms monomeric molecules with tetrahedrally coordinate titanium atoms and bonding parameters of TiN = 187.3 pm, PN = 155.1 pm, TiNP 150.4° in average.
    Additional Material: 1 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 351-356 
    ISSN: 0044-2313
    Keywords: Organomanganese Compounds ; Phosphoraneiminato Complexes ; Syntheses ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organomanganese Phosphoraneiminato Complexes with Heterocubane StructureThe organomanganese phosphoraneiminato complexes [MnR(NPEt3)]4 (R = Me, C=C—Ph, C=C—Tol, C=C—CMe3, C=C—SiMe3) with heterocubane structures have been prepared by reaction of the bromo derivative [MnBr(NPEt3)]4 with the corresponding lithium reagents LiR in THF/hexane solution, forming shiny red, very reactive compounds which are well soluble in hydrocarbons. They were characterized by mass spectroscopy, IR spectroscopy and by crystal structure determinations. According to these the compounds form nearly perfect Mn4N4 heterocubane frameworks with m̈3-N bridges of the phosphoraneiminato groups with Mn—N bond lengths of 214.5 pm in average which leads to Mn … Mn contacts of 299.5 pm in average. The organic residues R are terminal bonded with Mn—C distances Mn—Me of 219.5 pm and Mn—C=C—R of 207.6 pm in average.
    Notes: Die organisch substituierten Phosphanimi nato-Komplexe des Mangan(II) mit Heterocubanstruktur [MnR(NPEt3)]4 (R = Me, C=C—Ph, C=C—Tol, C=C—CMe3, C=C—SiMe3) werden durch Reaktion des Bromoderivates [MnBr(NPEt3)]4 mit den entsprechenden Lithium-Reagentien LiR in THF/Hexan als leuchtend rote, sehr reaktive, in Kohlenwasserstoffen leicht lösliche Verbindungen erhalten. Sie werden durch die Massen- und IR-Spektren sowie durch Kristallstrukturanalysen charakterisiert. Danach werden je vier Manganatome über je vier m̈3-N-Atome der Phosphan-iminato-Gruppen zu nur wenig verzerrten m̈3-N4-Kuben mit Mn—N-Abständen von im Mittel 214,5 pm verbrückt, was zu Mn … Mn-Kontakten von 299,5 pm führt. Die Reste R sind terminal gebunden mit Mn—C-Abständen Mn—Me von 219,5 pm und Mn—C=C—R von im Mittel 207,6 pm.
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