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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 102-108 
    ISSN: 0044-2313
    Keywords: Trimethylphosphonium Salts ; Preparation ; Vibrational Spectra ; NMR Spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Vibrational Spectra of Trimethylphosphonium Cations (CH3)3PX+ (X = H, D) and Crystal Structures of (CH3)3PD+SbCl6- and (CH3)3PCl+SbCl6-The trimethylphosphonium salts (CH3)3PX+SbCl6- (X = H, D) and (CH3)3PH+MF6- (M = As, Sb) are prepared and characterized by vibrational and NMR spectroscopy (1H, 31P, 13C).In addition the crystal structures of (CH3)3PD+SbCl6- and (CH3)3PCl+SbCl6- are reported. (CH3)3PD+SbCl6- crystallizes in the orthorhombic space group Pnma with a = 1555(1) pm, b = 753.1(8) pm, c = 1166(1) pm Z = 4. (CH3)3PCl+SbCl6- crystallizes triclinic in the space group P1 with a = 704.6(4) pm, b = 729.5(3) pm, c = 1391.1(7) pm, α = 89.57(4)°, b̃ = 88.04(4)°, γ = 74.98(4)° and Z = 2.
    Notes: Die Trimethylphosphonium-Salze (CH3)3PX+SbCl6- (X = H, D) und (CH3)3PH+MF6- (M = As, Sb) werden dargestellt und schwingungs- sowie NMR-spektroskopisch (1H, 31P, 13C) untersucht.Zusätzlich wird über die Kristallstrukturen von (CH3)3PD+SbCl6- und (CH3)3PCl+SbCl6- berichtet. (CH3)3PD+SbCl6- kristallisiert in der orthorhombischen Raumgruppe Pnma mit a = 1 555(1) pm, b = 753,1(8) pm, c = 1166(1) pm und Z = 4. (CH3)3PCl+SbCl6- kristallisiert triklin in der Raumgruppe P1 mit a = 704,6(4) pm, b = 729,5(3) pm, c = 1391,1(7) pm, α = 89,57(4)°, b̃ = 88,04(4)°, γ = 74,98(4)° und Z = 2.
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  • 2
    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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  • 3
    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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  • 4
    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.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 611 (1992), S. 23-27 
    ISSN: 0044-2313
    Keywords: (C6F5)2SF+SbF6- ; Preparation ; Crystal Structure ; Spectroscopic Data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of (C6F5)2SF+MF6- (M = As, Sb) and Crystal Structure of (C6F5)2SF+SbF6-XeF+MF6- (M = As, Sb) reacts with (C6F5)2S in HF to form (C6F5)2SF+MF6-. The deeply violet sulfonium salts can be kept without decomposition up to 24 h at room temperature.The hexafluoroantimonate salt crystallizes in the monoclinic space group P21/n with a = 1056.4(7) pm, b = 1446.3(10) pm, c = 1102.9(8) pm, β = 91.29(6)° und Z = 4. The SF-bond distance with 158.4(3) pm is of unusual length. Cations and anions are connected via interionic fluorine contacts to an infinite chain, in which cations and anions form to ABAB sequence along the chain.
    Notes: XeF+MF6- (M = As, Sb) reagiert mit (C6F5)2S in HF zu (C6F5)2SF+MF6-/. Die beiden tiefvioletten Sulfoniumsalze sind bei Raumtemperatur bis zu 24 Stunden unzersetzt haltbar.Das Hexafluoroantimonat kristallisiert in der monoklinen Raumgruppe P21/n mit a = 1056,4(7) pm, b = 1446,3(10) pm, c = 1102,9(8) pm, β = 91,29(6)° und Z = 4. Der SF-Bindungsabstand ist mit 158,4(3) pm außergewöhnlich lang. Kationen und Anionen werden durch interionische Fluor-Kontakte zu einer unendlichen Kette verknüpft, in der Kationen und Anionen in einer ABAB-Folge angeordnet sind.
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  • 6
    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.
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  • 7
    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.
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  • 8
    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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  • 9
    ISSN: 0044-2313
    Keywords: Dichloromethyleneiminum Salts ; Preparation ; Vibrational Spectra ; NMR-Spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis of the Dichloromethyleneiminium Salts Cl2C=NClH+MF6- and Cl2C=NClCH3+ MF6- (M = As, Sb) and Crystal Structure of Dichloromethyleneiminium-hyxachloroantimonate Cl2C=NH2+SbCl6-The N-chloro-dichloromethyleneiminium salts Cl2C=NCIH+MF6- (M = As, Sb) are prepared by protonationof trichloromethyleneimine in the superacide system HF/MF5 at 195 K. The synthesis of the N-chloro-N-methyl-dichloromethyleneiminium salts Cl2C=NClCH3+MF6- (M = As, Sb) is proceeded by methylation of perchloromethylenimine by CH3OSO+MF6- in SO2 also at low temperature. All salts are characterized by vibrational and NMR spectra. The dichloromethyleneiminiumhexachloroantimonate crystallizes in the space group P21/c with a = 971.3(4)pm, b = 1134.0(4)pm, c = 2154.2(7)pm β = 102.04(3)° and Z = 8.
    Notes: Die N-Chlor-dichlormethyleniminium-Salze Cl2C=NClH+MF6- (M = As, Sb) werden aus Trichlormethylenimin durch Protonierung mit dem supersauren System HF/MF5 bei 195 K dargestellt. Die Synthese der N-Chlor-N-methyl-dichlormethylen-iminium-Salze Cl2C=NClCH3+MF6- (M = As, Sb) erfolgt durch Methylierung von Perchlormethylenimin mit CH3OSO+MF6- in SO2 ebenfalls bei tiefer Temperatur. Alle Salze werden schwingungs- und NMR-spektroskopisch charakterisiert. Dichlormethyleniminiumhexachloroantimonat kristallisiert monoklin in der Raumgruppe P21/c mit a = 971,3(4)pm, b = 1134,0(4)pm, c = 2154,2(7) pm, β = 102,04(3)° und Z = 8.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 139-143 
    ISSN: 0044-2313
    Keywords: Cyanonitrilium Salts ; Preparation ; Vibrational Spectra ; NMR Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Spectroscopic Characterization of the Cyanonitrilium Salts NCCNH+MF-6 and the N-Methyl-cyanonitrilium Salts NCCNCH3+MF6- (M = As, Sb)The cyanonitrilium salts NCCNH+MF-6 (M = As, Sb) are prepared by protonation of cyanogene (CN)2 in the superacid HF/MF5 at 195 K. The synthesis of the N-methyl-cyanonitrilium salts NCCNCH3+MF6- (M = As, Sb) is proceeded by methylation of cyanogene by CH3OSO+MF6- in SO2 also at low temperature. All salts are characterized by vibrational and NMR spectra.
    Notes: Die Cyannitrilium-Salze NCCNCH+MF6- (M = As, Sb) werden aus Dicyan (CN)2 durch Protonierung in der Supersäure HF/MF5 bei 195 K dargestellt. Die Synthese der N-Methylcyannitriliumsalze NCCNCH3+MF6- (M = As, Sb) erfolgt durch Methylierung von Dicyan mit CH3OSO+MF6- in SO2 ebenfalls bei tiefer Temperatur. Alle Salze werden schwingungs- und NMR-spektroskopisch charakterisiert.
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