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  • Inorganic Chemistry  (2)
  • Crystal Structure  (1)
  • 1990-1994  (2)
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  • 1
    ISSN: 0044-2313
    Keywords: Triphenylarsin-p-toluene sulfonylimine ; Zirconium tetrachloride complex ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of Triphenylarsin-p-toluene Sulfonylimine and of its Donor-Acceptor Complex [ZrCl4(Ph3AsNSO2Tol)]2The molecular structures of the title compounds are reported. In the donor-acceptor complex [ZrCl4(Ph3AsNSO2Tol)]2 the zirconium atoms are bridged by the oxygen atoms of the triphenylarsin-p-toluene sulfonylimine molecules, forming a centrosymmetric dimer with a puckered Zr2O4S2 eight-membered ring in the chair conformation.Ph3AsNSO2Tol: Space group P1, Z = 2, structure determination with 4 010 observed unique reflections, R = 0.036. Lattice dimensions at 19°C: a = 897.52(4), b = 1 071.82(6), c = 1 337,49(5) pm, α = 110.280(4)°, β = 98.814(4)°, γ = 109.872(4)°.[ZrCl4(Ph3AsNSO2Tol)]2: Space group P21/n, Z = 4, structure determination with 3 762 observed unique reflections, R = 0.078. Lattice dimensions at -60°C: a = 1 387.3(4), b = 1 434.9(2), c = 1 404.7(4) pm, β = 92.71(1)°.
    Notes: Es wird über die Molekülstrukturen der beiden Titelverbindungen berichtet. In dem Donor-Akzeptorkomplex [ZrCl4(Ph3AsNSO2Tol)]2 sind die Zirkoniumatome über die O-Atome der Triphenylarsin-p-toluolsulfonylimin-Moleküle zu einem zentrosymmetrischen Dimer mit einem Zr2O4S2-Achtring in der Sesselkonformation verknüpft.Ph3AsNSO2Tol: Raumgruppe P1, Z = 2, Strukturlösung mit 4 010 unabhängigen beobachteten Reflexen, R = 0,036. Gitterkonstanten bei 19°C: a = 897,52(4), b = 1 071,82(6), c = 1 337,49(5) pm, α = 110,280(4)°, β = 98,814(4)°, γ = 109,872(4)°.[ZrCl4(Ph3AsNSO2Tol)]2: Raumgruppe P21/n, Z = 4, Strukturlösung mit 3 762 unabhängigen beobachteten Reflexen, R = 0,078. Gitterkonstanten bei -60°C: a = 1 387,3(4), b = 1 434,9(2), c = 1 404,7(4) pm, β = 92,71(1)°.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0044-2313
    Keywords: Silanolato Complexes of Titanium and Zirconium ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Silanolato Complexes of Titanium and Zirconium. The Crystal Structures of Cp2TiCl(OSiPh3) and Cp2ZrCl(OSiPh3)The title compounds have been prepared by the reaction of Cp2MCl2 (M = Ti, Zr) with triphenylsilanole in diethylether in the presence of piperidine. They form only sparingly moisture sensitive orange (Ti) or colourless (Zr) crystal needles, which were characterized by X-ray crystallography.Cp2TiCl(OSiPh3): Space group P21/n, Z = 4, structure solution with 3961 observed unique reflections, R = 0.057. Lattice dimensions at 20°C: a = 1029.6, b = 1719.3, c = 1388.9 pm, β = 100.69°. The compound forms monomeric molecules with bond lengths TiO of 184.2 pm, SiO of 161.5 pm, and a TiOSi bonding angle of 164.5°.Cp2ZrCl(OSiPh3): Space group P3, Z = 18, structure solution with 2799 observed unique reflections, R = 0.047. Lattice dimensions at -20°C: a = b = 3518, c = 1058.3 pm. The structure consists of three symmetry-independent monomeric molecules, which differ only slightly. The bond lengths are (in average): ZrO 196.4 pm, SiO 162.1 pm, the ZrOSi bond angle is 173.7°.
    Notes: Die Titelverbindungen werden aus Cp2MCl2 (M = Ti, Zr) und Triphenylsilanol in Diethylether in Gegenwart von Piperidin hergestellt. Sie bilden nur wenig feuchtigkeits-empfindliche orange (Ti) bzw. farblose Kristallnadeln (Zr), die wir kristallographisch charakterisiert haben.Cp2TiCl(OSiPh3): Raumgruppe P21/n, Z = 4, Strukturlösung mit 3961 unabhängigen, beobachteten Reflexen, R = 0,057. Gitterkonstanten bei -50°C: a = 1029,6; b = 1719,3; c = 1388,9 pm, β = 100,69°. Die Verbindung bildet monomere Moleküle mit Abständen TiO von 184,2 pm, SiO von 161,5 pm und einem TiOSi-Bindungswinkel von 164,5°.Cp2ZrCl(OSiPh3): Raumgruppe P3, Z = 18, Strukturlösung mit 2799 unabhängigen, beobachteten Reflexen, R = 0,047. Gitterkonstanten bei -20°C: a = b = 3518; c = 1058,3 pm. Die Struktur enthält drei symmetrieunabhängige monomere Moleküle, die sich nur wenig voneinander unterscheiden. Die Abstände ZrO betragen im Mittel 196,4 pm, SiO im Mittel 162,1 pm und die Bindungswinkel ZrOSi im Mittel 173,7°.
    Additional Material: 3 Ill.
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