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  • preparation  (19)
  • Vibrational Spectra  (5)
  • (difluoro)methylphosphine  (1)
  • (μ-thio)bisnitriliumhexafluoro metallates  (1)
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  • 11
    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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  • 12
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 605 (1991), S. 109-116 
    ISSN: 0044-2313
    Keywords: Antimony(III)fluoride,(Sb2F5+)(Sb3F72+)(SbF6-)3 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of a new Modification of Sb8F30The modification of Sb8F30, described here, crystallizes in the orthorhombic space group Pca21 (No. 29) with a = 1115.7(1), b = 1100.2(1), c = 1917.8(3) pm and Z = 4. Within this complex molecule, the Sb3F72+-cation was identified besides a heavily distorted form of the mixed valent Sb4F17--anion.
    Notes: Die hier beschriebene Modifikation von Sb8F30 kristallisiert in der orthorhombischen Raumgruppe Pca21 (Nr. 29) mit a = 1115,7(1), b = 1100,2(1), c = 1917,8(3) pm und Z = 4. Innerhalb dieses komplexen Moleküls werden ein Sb3F72+-Kation und eine stark verzerrte Form des gemischt valenten Sb4F17--Anions identifiziert.
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  • 13
    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.
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  • 14
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 514-518 
    ISSN: 0044-2313
    Keywords: N-Trifluormethyl-difluormethyleneiminium salts ; preparation ; n.m.r., i.r. spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of the Iminium Salts CF3—NX=CF2+MF6- (X = CH3, F and M = As, Sb) and CF3—NCl=CF2+ AsF6-The preparation of the iminiumsalts CF3—NX=CF2+ MF6- (X = CH3, F and M = As, Sb) and CF3—NCl=CF2+ AsF6- is reported. The salts were characterized by NMR and infrared spectroscopy. CF3—NCH3=CF2+MF6- decompose into MF5 and (CF3)2NCH3.
    Notes: Es wird über die Darstellung der Iminiumsalze CF3—NX=CF2+ MF6- (X = CH3, F und M = As, Sb) und CF3—NCl=CF2+AsF6- berichtet. Die Salze werden durch NMR- und IR-Spektroskopie charakterisiert. CF3—NCH3=CF2+MF6- zerfällt in MF5 und (CF3)2NCH3.
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  • 15
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 2066-2070 
    ISSN: 0044-2313
    Keywords: Dichlorine(trifluoromethyl)amine ; dichlorine-fluorine(trifluoromethyl)ammonium hexafluoroarsenate,-antimonate ; Chlorine(difluoromethylene)fluorineammonium hexafluoroantimonate ; preparation ; gas phase structure of CF3NCl2 ; i.r. spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Gas Phase Structure of CF3NCl2 and Preparation of CF3NCl2F+MF6- (M = As, Sb) and CF2 = NCl2F+SbF6-The gas phase structure of CF3NCl2 is reported. The following skeletal parameters are derived (ra-values, error limits are 3σ values): N—C = 1.470(6) Å, N—Cl = 1.733(3) Å, ClNCl = 111.5(4)° and ClNC = 107.6(5)°. CF3NCl2F+MF6- is prepared by fluorination of CF3NCl2 with XeF+MF6-. The same educt CF3NCl2 reacts with XeF+SbF6- at -40°C to CF2 = NClF+SbF6- under elimination of ClF.
    Notes: Es wird über die Gasphasenstruktur von CF3NCl2 berichtet. Der N—C-Bindungsabstand (ra-Wert, Fehlergrenze 3σ-Wert) beträgt 1,470(6) Å, der N—Cl-Abstand 1,733(3) Å und die Bindungswinkel am Stickstoff ClNCl = 111,5(4)° und ClNC = 107,6(5)°.Durch Fluorierung des Amins mit XeF+MF6- (M = As, Sb) können die bis -50°C stabilen Fluorammoniumsalze CF3NCl2F+MF6- synthetisiert werden. Mit dem gleichen Edukt CF3NCl2 reagiert XeF+SbF6- bei -40°C unter ClF-Abspaltung zu CF2 = NClF+SbF6-.
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  • 16
    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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  • 17
    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.
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  • 18
    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.
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  • 19
    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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  • 20
    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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