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  • 1
    ISSN: 0044-2313
    Keywords: dimercapto(methyl)sulfonium salts ; bis(chlorothio)methylsulfonium ; salts ; preparation ; Ramanspectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Preparation of Dimercapto(methyl)Sulfonium Salts [CH3S(SH)2]+ AsF6- and [CH3S(SH)2]+SbCl6- and the Bis(chlorothio)methylsulfonium Salts [CH3S(SCI)2]+ AsF6- and [CH3S(SCI)2]+ SbCl6-The preparation of the dimercapto(methyl)sulfonium salts [CH3S(SH)2]+ AsF6- and [CH3S(SH)2]+SbCl6- from [CH3SCl2]+ salts and H2S at 195 K is reported. The salts are stable below 210 K. They are characterized by additional Raman spektroscopic measurements of the isotopic labelled cations [CH3S(SD)2]+, [CH3S(34SH)2]+ and [CH3S(34SD)2]+. The dimercapto(methyl)sulfonium salts are transfered into bis(chlorthio)methylsulfonium salts by reaction with Cl2 at 195 K.
    Notes: Es wird über die Darstellung der Dimercapto(methyl)sulfoniumsalze [CH3S(SH)2]+ AsF6- und [CH3S(SH)2]+SbCl6- aus den [CH3SCl2]+-salzen und H2S bei 195 K berichtet. Beide Verbindungen sind unterhalb 210 K haltbar. Ihre Charakterisierung erfolgt Raman-spektroskopisch durch zusätzliche Messungen an den markierten Kationen [CH3S(SD)2]+, [CH3S(34SH)2]+ und [CH3S(34SD)2]+. Beide [CH3S(SH)2]+-Salze reagieren mit Chlor zu den Bis(chlorthio)methylsulfonium-salzen [CH3S(SCl)2]+AsF6- und [CH3S(SCl)2]+SbCl6-.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 40-44 
    ISSN: 0044-2313
    Keywords: Fluorophosphonium salts ; preparation ; vibrational spectra ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Spectroscopic Characterization of the Fluorophosphonium Salts X2FPSCH3+MF6- (X = Br, Cl; M = As, Sb) and XF2PSCH3+SbF6- (X = Br, Cl, F)The preparation of the fluorophosphonium salts X2FPSCH3+MF6- (X = Br, Cl; M = As, Sb) and XF2PSCH3+SbF6- (X = Br, Cl, F) by methylation of the corresponding thiophosphorylhalides in the system CH3F/SO2/MF5 (M = As, Sb) is reported. The new salts are characterized by their vibrational and NMR spectra.
    Notes: Es wird über die Darstellung der Fluorphosphoniumsalze X2FPSCH3+MF6- (X = Br, Cl; M = As, Sb) and XF2PSCH3+SbF6- (X = Br, Cl, F) durch oxidative Methylierung der korrespondierenden Thiophosphorylhalogenide mit dem System CH3F/SO2/MF5 (M = As, Sb) berichtet. Die Salze werden durch ihre Schwingungs- und NMR-Spektren charakterisiert.
    Additional Material: 3 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 35-39 
    ISSN: 0044-2313
    Keywords: CF3S(O)F2 +SbF6- ; (CF3)2SOXeP+SbF6- ; preparation ; vibrational spectra ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die Reaktion von XeF+SbF6- mit Sulfuranen; Präparation von CF3S(O)F2+SbF6- und (CF3)2SOXeF+SbF6-CF3S(O)F, (CF3)2SO, CF3SF3, (CF3)2SF2, und SF4 reagieren in unterschiedlicher Weise mit XeF+MF6- (M=As, Sb). Eine oxidative Fluorierung wird beobachtet beim CF3S(O)F unter Bildung des Persulfoniumsalzes CF3S(O)F2+SbF6-, während mit (CF3)2SO ein einfaches Xenon-enthaltendes Additionsprodukt (CF3)2SOXeF+SbF6- isoliert werden kann. Im Gegensatz dazu führt der Lewis-saure Charakter des XeF+ -Kations gegenüber (CF3)nSF4-n (n = 0 - 2) zu den entsprechenden Fluorsulfoniumsalzen (CF3)nSF3-n +MF6- (M=As. Sb) und XeF2.
    Notes: CF3S(O)F, (CF3)2SO, CF3SF3, (CF3)2SF2, and SF4 react in different manner with XeF+MF6- (M=As, Sb). An oxidative fluorination is observed by CF3S(O)F forming the persulfonium salt CF3S(O)F2+SbF6-, whereas by (CF3)2SO a simple addition product containing xenon can be isolated in form of the sulfonium salt (CF3)2SOXeF+SbF6-. On the contrary, the Lewis-acidic character of the XeF+-cation predominates against (CF3)nSF4-n (n = 0 - 2) leading to the corresponding fluorosulfonium salts (CF3)nSF3-n +MF6- (M=As, Sb) and XeF2.
    Additional Material: 2 Ill.
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  • 4
    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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  • 5
    ISSN: 0044-2313
    Keywords: Methoxy(oxy)sulfonium hexafluoroarsenate ; preparation ; IR spectra ; force field calculation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure, Vibrational Spectra, and Valence Force Field of Methoxy(oxy)-sulfonium Hexafluoroarsenate CH3OSO+ AsF6-Methoxy(oxy)sulfonium hexafluoroarsenate CH3OSO+ AsF6- crystallizes in the monoclinic space group P21/n with a = 547,0(4) pm, b = 1 728.1(5) pm, c = 767.8(4) pm, β = 106.69(4)°, Z = 4. The cation is planar with bond distances d(CO) = 150.2(9) pm, d(SO) = 150.5(5) pm, d(SO) = 139.7(5) pm and angles ∢ (COS) = 125.8(4)°, ∢ (OSO) = 114.9(3)°.The vibrational frequencies of the cation are discussed with correspondence to the values of 34S and 18O labelled substituted species. A force field calculation equates f(CO) = 3.75 Ncm-1, f(SO) = 6.91 Ncm-1, f(SO) = 10.81 Ncm-1.
    Notes: Methoxy(oxy)sulfonium-hexafluoroarsenat CH3OSO+ AsF6- kristallisiert in der monoklinen Raumgruppe P21/n mit a = 547,0(4) pm, b = 1 728,1(5) pm, c = 767,8(4) pm, β = 106,69(4)°, Z = 4. Das Kation ist planar mit Bindungsabständen von d(CO) = 150,2(9) pm, d(SO) = 150,5(5) pm, d(SO) = 139,7(5) pm und Winkeln ∢ (COS) = 125,8(4)°, ∢ (OSO) = 114,9(3)°.Die Schwingungsfrequenzen des Kations werden unter Einbeziehung der 34S und 18O markierten Spezies diskutiert. Eine Kraftfeldberechnung ergibt f(CO) = 3,75 Ncm-1, f(SO) = 6,91 Ncm-1, f(SO) = 10,81 Ncm-1.
    Additional Material: 3 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 617 (1992), S. 143-147 
    ISSN: 0044-2313
    Keywords: Nitrilium salts ; preparation ; vibrational spectra ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of the Halogenonitrilium Salts XCNH+MF6- (X = CI, Br, I; M = As, Sb) and the Trifluoroacetonitrilium Salts CF3CNH+MF6-The halogenonitrilium salts XCNH+MF6- (X = CI, Br, I; M = As, Sb) are synthesized by protonation of cyanogen halides in the superacide system HF/MF5 at low temperature. The synthesis of trifluoroacetonitrilium salts CF3CNH+MF6- (M = As, Sb) is proceeded analogous with trifluoroacetonitrile. All salts are characterized by vibrational and NMR spectroscopy.
    Notes: Die Halogennitrilium-Salze XCNH+MF6- (X = Cl, Br, I; M = As, Sb) werden aus Halogencyanen durch Protonierung mit dem supersauren System HF/MF5 bei tiefer Temperatur dargestellt. Die Synthese der Trifluoracetonitrilium-Salze CF3CNH+MF6- (M = As, Sb) erfolgt analog aus Trifluoracetonitril. Alle Salze werden durch Schwingungs und NMR-Spektren charakterisiert.
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  • 7
    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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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 604 (1991), S. 105-112 
    ISSN: 0044-2313
    Keywords: Methylthio(trihalogeno)phosphonium salts ; preparation ; vibrational spectra ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Preparation of Methylthio(trihalogeno)phosphonium Salts ClnBr3-nPSCH3+MF6-(n = 0-3; M = As, Sb) and Hal3PSCH3+SbCl6-(Hal = Br, Cl)The methylthio(trihalogeno) phosphonium salts BrnCl3-nPSCH3+MF6- (n = 0-3; M = As, Sb) are prepared by methylation of the corresponding thiophosphorylhalides BrnCl3-nPS in the system SO2/CH3F/MF5. The hexachloroantimonates Hal3PSCH3+SbCl6-(Hal = Br, Cl) are synthesized by thiomethylation of PBr3 and PCl3 with CH3SCl/SbCl5. All salts are characterized by vibrational and NMR spectroscopy.
    Notes: Die Methylthio(trihalogen)phosphonium-Salze BrnCl3-nPSCH3+MF6-(n = 0-3; M = As, Sb) werden durch Methylierung der Thiophosphorylhalogenide BrnCl3-nPS mit CH3OSO+MF6- in flüssigem SO2 dargestellt. Die Hexachloroantimonate Hal3PSCH3+SbCl6-(Hal = Br, Cl) werden durch Thiomethylierung von PBr3 und PCl3 mit CH3SCl/SbCl5 erhalten. Alle Verbindungen werden durch ihre Schwingungs- und NMR-Spektren charakterisiert.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 114-116 
    ISSN: 0044-2313
    Keywords: Bromosulfenyl(trihalogeno)phosphonium salts ; preparation ; vibrational spectra ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bromosulfenyl(trihalogeno)phosphonium Salts Cl3-nBrnPSBr+AsF6- (n = 0 - 3) and Cl3PSBr+SbF6-  -  Oxidative Bromination of ThiophosphorylhalidesThe bromosulfenyl(trihalogeno)phosphonium salts Cl3-nBrnPSBr+AsF6- (n = 0 - 3) and Cl3PSBr+SbF6- are prepared by oxidative bromination of the corresponding thiophosphorylhalides with Br2/MF5 (M = As, Sb) and characterized by vibrational and NMR spectroscopy.
    Notes: Die Bromsulfenyl(trihalogen)phosphonium Salze Cl3-nBrnPSBr+AsF6- (n = 0 - 3) und Cl3PSBr+SbF6- werden durch oxidative Bromierung der entsprechenden Thiophosphorylhalogenide mit Br2/MF5 (M = As, Sb) dargestellt und schwingungs- sowie NMR-spektroskopisch untersucht.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 93-97 
    ISSN: 0044-2313
    Keywords: Methylnitrilium salts ; preparation ; vibrational spectra ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of N-Methylhalidonitrilium Salts XCNCH3+MF6- (X = Cl, Br, I; M = As, Sb) and the N-Methyl-trifluoroacetonitrilium Salts CF3CNCH3+MF6-The N-methyl-halidonitrilium salts XCNCH3+MF6- (X = Cl, Br, I; M = As, Sb) are synthesized by methylation of cyanogen halides with CH3F/MF5 in SO2 at low temperatures.The N-methyl-trifluoroacetonitrilium salts CF3CNCH3+MF6- (M = As, Sb) are formed analogous with trifluoroacetonitrile. All salts are characterized by vibrational and NMR spectroscopy.
    Notes: Die N-Methyl-halogennitrilium-Salze XCNCH3+MF6- (X = Cl, Br, I; M = As, Sb) werden aus Halogenocyanen durch Methylierung mit CH3F/MF5 in SO2 bei tiefer Temperatur synthetisiert. Die Darstellung der N-Methyl-trifluoracetonitrilium-Salze CF3CNCH3+MF6- (M = As, Sb) erfolgt analog ausgehend von Trifluoracetonitril. Alle Salze werden durch Schwingungs- und NMR-Spektren charakterisiert.
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