Recent achievements in the synthesis and characterization of metal hexafluorantimonates and hexafluoroaurates

The efforts to prepare new MSbF6/MSb2F11 (A = In, Cu, Au, Hg) compounds were partly successful. Reaction between InBF4 and excess SbF5 in anhydrous hydrogen fluoride (aHF) yields a mixture of InF3·3SbF5 and unidentified SbF3·xSbF5. The attempts to synthesize MSbF6/MSb2F11 salts (A = Au, Hg) by controlled reduction of Au(SbF6)2 or Hg(SbF6)2 solutions in aHF/SbF5 by elemental hydrogen, resulted in the precipitation of metallic Au or Hg2(Sb2F11)2. In the reaction of metallic Cu and deficit SbF5, the synthesis of CuSbF6 was achieved. CuSbF6, like CuAsF6, is a rare example of a Cu(I) compound in a pure fluorine environment. ional spectra of M(II) hexafluoroantimonates (M = Ni, Fe, Co, Cu, Cr, Pd, Ag) were reinvestigated. It was found that many of them originally assigned to M(SbF6)2 compounds, belong to their mixtures with oxonium salts H3OM(SbF6)3, H3OSbF6, and/or H3OSb2F11. ons were studied between MF2/2AuF3 (M = Ni, Cu, Ag, Zn, Cd and Hg) and KrF2 or UV-irradiated elemental fluorine in aHF as solvent at room temperature. On the basis of mass balances, Raman spectroscopy and X-ray powder diffraction analysis it can be concluded that the isolated solids have structures that can be considered in terms of an M(AuF6)2 formulation. Previously reported syntheses and characterization of M(AuF6)2 (M = Mg, Ca, Sr, Ba) were reinvestigated. In the case of M = Ba two different Au F 6 − salts were isolated. spectra of the majority of synthesized metal hexafluoroaurates (M = Ni, Cu, Ag, Zn, Cd, Hg, Mg and Ca) show more bands than expected for regular Au F 6 − anion, indicating that the salts obtained exhibit relatively strong cation–anion interactions. The Raman spectra of the remaining Sr and Ba salts show the presence of more regular Au F 6 − octahedra, indicating weak cation–anion interactions.