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  • single crystal X-ray structure  (3)
  • (difluoro)methylphosphine  (1)
  • 1
    ISSN: 0044-2313
    Keywords: μ-Sulfurdisulfonium salts ; preparation ; single crystal X-ray structure ; Raman, NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of μ-Sulfurdisulfonium Salts [(CH3)2S—Sx—S(CH3)2]2+2A- (x = 1-3, A- = AsF6-, SbF6-, SbCl6-). On the Analogy of the Reactivity of Sulfanes and Sulfonium SaltsThe preparation of the μ-sulfurdisulfonium salts [(CH3)2S—Sx—S(CH3)2]2+(A-)2 with x = 1-3 and A- = AsF6-, SbF6-, SbCl6- is reported. The salts are formed by reaction of (CH3)2SH+A- and (CH3)2SSH+A- with SCl2 and S2Cl2, resp. They are characterized by vibrational spectroscopic measurements. [(CH3)2S—S2—S(CH3)2]2+(SbF6-)2 crystallizes in the space group C2/c with a = 1 884.5(7) pm, b = 1 302.8(5) pm, c = 1 477.2(5) pm, β = 98.62(3)° und Z = 8.
    Notes: Es wird über die Darstellung der μ-Schwefeldisulfoniumsalze [(CH3)2S—Sx—S(CH3)2]2+ (A-)2 mit x = 1-3 und A- = AsF6-, SbF6-, SbCl6- berichtet. Die Salze werden durch Kondensationsreaktionen von (CH3)2SH+A- und (CH3)2SSH+A- mit SCl2 bzw. S2Cl2 gebildet. Ihre Charakterisierung erfolgt schwingungsspektroskopisch. Das [(CH3)2S—S2—S(CH3)2]2+(SbF6-)2 kristallisiert in der Raumgruppe C2/c mit a = 1 884,5(7) pm, b = 1 302,8(5) pm, c = 1 477,2(5) pm, β = 98,62(3)° und Z = 8.
    Additional Material: 3 Ill.
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  • 2
    ISSN: 0044-2313
    Keywords: Bis(triphenylsilyl)sulfanes ; preparation ; single crystal X-ray structure ; vibrational spectra ; NMR spectra ; UV-VIS spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Preparation of Bis(triphenylsilyl)sulfanes (C6H5)3Si—Sx—Si(C6H5)3 (x = 3, 4) and the Crystal Structure of (C6H5)3Si—S4—Si(C6H5)3The preparation of the bis(triphenylsilyl)sulfanes Ph3Si—Sx—SiPh3 (x = 3, 4) from Ph3SiSNa and SCl2 resp. S2Cl2 is reported. They are characterized by vibrational, NMR and UV-VIS spectroscopic measurements. Ph3Si—S4—SiPh3 crystallizes in space group P1 with a = 943.6(6) pm, b = 945.7(5) pm, c = 1 881.7(12) pm, α = 82.11(5)°, β = 78.95(5)°, γ = 83.15(5)° and Z = 2.
    Notes: Es wird über die Darstellung der Bis(triphenylsilyl)-sulfane Ph3Si—Sx—SiPh3 (x = 3, 4) aus Ph3SiSNa und SCl2 bzw. S2Cl2 berichtet. Ihre Charakterisierung erfolgt schwingungs-, NMR-, und UV-VIS-spektroskopisch.Ph3Si—S4—SiPh3 kristallisiert in der Raumgruppe P1 mit a = 943,6(6) pm, b = 945,7(5) pm, c = 1 881,7(12) pm, α = 82,11(5)°, β = 78,95(5)°, γ = 83,15(5)° und Z = 2.
    Additional Material: 3 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 877-884 
    ISSN: 0044-2313
    Keywords: triphenylsilanesulfenylbromide and -iodide ; triphenylsilanthiol ; preparation ; vibrational spectra ; UV-VIS spectra ; single crystal X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of (C6H5)3SiSH and (C6H5)3SiSBr and the Preparation of the Iodosulfane (C6H5)3SiSIThe preparation of the halogenosulfanes Ph3SiSBr and Ph3SiSI from Ph3SiSH and N-halogenosuccinimide is reported. They are characterized by vibrational spectroscopic measurements. Ph3SiSBr crystallizes in space group P1 with a = 899.3(8) pm, b = 941.3(7) pm, c = 1 051.4(7) pm, α = 109.88(5)°, β = 99.23(6)°, γ = 96.78(6)° and Z = 2. Ph3SiSH crystallizes in space group P21/c with a = 1 879.4(8), b = 966.3(5), c = 1 845.2(9), β = 107.84(4), Z = 8. The halogenosulfanes decompose in polar solvents by formation of sulphur and triphenylsilanhalide.
    Notes: Es wird über die Darstellung der Halogensulfane Ph3SiSBr und Ph3SiSI aus Ph3SiSH und N-Halogensuccinimid berichtet. Ihre Charakterisierung erfolgt schwingungsspektroskopisch. Das Ph3SiSBr kristallisiert in der Raumgruppe P1 mit a = 899,3(8) pm, b = 941,3(7) pm, c = 1 051,4(7) pm, α = 109,88(5)°, β = 99,23(6)°, γ = 96,78(6)° und Z = 2, das Ph3SiSH in der Raumgruppe P21/c mit a = 1 879,4(8) b = 966,3(5), c = 1 845,2(9), β = 107,84(4), Z = 8. Die Halogensulfane zerfallen in polaren Lösungsmitteln unter Schwefeleliminierung zu Triphenylsilylhalogeniden.
    Additional Material: 5 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 509-513 
    ISSN: 0044-2313
    Keywords: (difluoro)methylphosphine ; (difluoro)methylphosphonium salts ; preparation ; single crystall X-ray structure ; vibrational and NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structures of CH3PF2H+AsF6- and CH3PF2H+SbF6- and a simple Method for Preparation of CH3PF2A simple method for preparation of CH3PF2 from CH3PCl2 is reported. The phosphonium salts CH3PF2H+MF6- are obtained by the reaction of CH3PCl2 with superacidic systems HF/MF5 (M = As, Sb). CH3PF2H+SbF6- crystallizes in the space group P1 with a = 548.4(4) pm, b = 695.5(8) pm, c = 960.2(9) pm, α = 94.68(5)°, β = 97.19(6)°, γ = 94.41(6)° and Z = 2. CH3PF2H+SbF6- crystallizes in P1 with a = 554.3(3), b = 724.2(4), c = 970.4(5), α = 94.73(4)°, β = 96.14(5)°, γ = 95.30(4)°.
    Notes: Es wird über eine einfache Darstellung von CH3PF2 aus CH3PCl2 berichtet, welches in den supersauren Systemen HF/MF5 (M = As, Sb) zu den Phosphoniumsalzen CH3PF2H+MF6- protoniert wird. CH3PF2H+AsF6- kristallisiert in der Raumgruppe P1 mit a = 548,4(4) pm, b = 695,5(8) pm, c = 960,2(9) pm, α = 94,68(5)°, β = 97,19(6)°, γ = 94,41(6)° und Z = 2, das isostrukturelle CH3PF2H+SbF6- mit a = 554,3(3), b = 724,2(4), c = 970,4(5), α = 94,73(4)°, β = 96,14(5)°, γ = 95,30(4)°.
    Additional Material: 2 Ill.
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