The preparation and characterization of SeCl3SbF6, improved syntheses of MCl3(As/Sb)F6 (M = S, Se), and the X-ray crystal structure determination of SeCl3AsF6 and a new phase of SBr3SbF6

Article abstract of DOI:10.1139/v96-184

Alternative and, in some cases, improved syntheses of the salts MX₃(As/Sb)F₆ (M = S, Se) and SCl₃(SbCl₆/AlCl₄) are described. In addition, the synthesis of SeCl₃SbF₆ is reported. The compounds were characterized by FT-Raman spectroscopy and the X-ray crystal structures of SeCl₃AsF₆ (also ⁷⁷Se NMR)and a new phase of SBr₃SbF₆ were determined. Crystals of SeCl₃AsF₆ and SBr₃SbF₆ are monoclinic, space group P2₁/c with [values for SBr₃SbF₆ in brackets] a = 7.678(1) [8.137(1)] A, b = 9.380(3) [9.583(2)] A, c = 11.920(3) [12.447(2)] A, β = 98.19(2)° [97.36(1)]°, V = 849.72(3) [962.6(3)] A³, z = 4, D_x = 2.925 [3.502] Mg m^-3, R = 0.0525 [0.055], and R_w = 0.0554 [0.060] for 1151 [1472] observed reflections.