SYNTHESIS AND CHARACTERIZATION OF CHLOROFLUOROANTIMONATES(V)

Five of the eight possible chlorofluoroantimonate(V) anions have been characterised in solution by Sb-121 and F-19 NMR spectroscopy; of these three have been isolated in at least 90% purity as their tetraalkylammonium salts and their infrared and Raman spectra have been assigned. None of the three trans isomers was detected either in solution or in the solid state. Factors influencing the appearance of the antimony NMR spectra of the octahedral anions are discussed. The course of the solvolysis of the SbCl6-ion by anhydrous HF has been shown to be irreversible and to generate all possible stoichiometries of the chlorofluoro-anions in succession.