PREPARATION AND SPECTROSCOPIC CHARACTERIZATION OF THE PERSULFONIUM SALTS (CH3)(CF3)SF3+SBF6- AND (CH3)(CF3)2SF2+SBF6- AND CRYSTAL-STRUCTURE OF CF3SF2+SBF6-

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, H-1, C-13, and F-19 NMR spectroscopy. CF3SF2+SbF6- crystallizes in the space group C2/c with a = 16.889(8) angstrom, b = 7.261(4) angstrom, c = t3.416(7) angstrom, beta = 91.08-degrees with 8 formula units per unit cell at 167 K. Cations and anions are connected via short SF contacts forming a V-octahedral surrounding of the central S atom which is in close analogy to the already known CF3SF2+AsF6-.