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  • 1
    ISSN: 0044-2313
    Keywords: Persulfonium salts ; preparation ; vibrational spectra ; NMR spectra ; crystal structure of CF3SF2+SbF6- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Spectroscopic Characterization of the Persulfonium Salts (CH3)(CF3)SF3+SbF6- and (CH3)(CF3)2SF2+SbF6- and Crystal Structure of CF3SF2+SbF6- [1].The preparation of the persulfonium salts (CH3)(CF3)SF3+SbF6- and (CH3)(CF3)2SF2+SbF6- by methylation of the sulfuranes CF3SF3 and (CF3)2SF2 with CH3OSO+SbF6- in liquid SO2 is reported. The thermolabile compounds are characterized by IR, Raman, 1H, 13C, and 19F NMR spectroscopy.CF3SF2+SbF6- crystallizes in the space group C2/c with a=16.889(8) Å, b=7.261(4) Å, c=13.416(7) Å, β=91.08° with 8 formula units per unit cell at 167 K. Cations and anions are connected via short SF contacts forming a Ψ-octahedral surrounding of the central S atom which is in close analogy to the already known CF3SF2+AsF6-.
    Notes: Es wird über die Darstellung der Persulfoniumsalze (CH3)(CF3)SF3+SbF6- und (CH3)(CF3)2SF2+SbF6- durch Methylierung der Sulfurane CF3SF3 und (CF3)2SF2 mit CH3OSO+SbF6- in flüssigem SO2 berichtet. Die thermolabilen Verbindungen werden durch IR-, Raman-, 1H-, 13C- und 19F-NMR-Spektroskopie charakterisiert. CF3SF2+SbF6- kristallisiert in der Raumgruppe C2/c mit a=16,889(8) Å, b=7,261(4) Å, c=13,416(7) Å, β=91,08° und 8 Formeleinheiten pro Einheitszelle bei 167 K. Kationen und Anionen sind über kurze SF-Kontakte verbunden und bilden eine Ψ-oktaedrische Umgebung des zentralen S-Atoms. Diese Struktur stimmt gut mit der des bereits bekannten CF3SF2+AsF6- überein.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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