Silver(I) Undecafluorodiantimonate(V)

The reaction between AgBF4 and excess of SbF5 in anhydrous hydrogen fluoride (aHF) yields the white solid AgSb2F11 after the solvent and the excess of SbF5 have been pumped off. Reaction between equimolar amounts of AgSb2F11 and AgBF4 yields AgSbF6. Meanwhile, oxidation of solvolyzed AgSb2F11 in aHF by elemental fluorine yields a clear blue solution of solvated Ag(II) cations and SbF6 - anions. AgSb2F11 is orthorhombic, at 250 K, Pbca, with a = 1091.80(7) pm, b = 1246.28(8) pm, c = 3880.2(3) pm, V = 5.2797(6) nm3, and Z = 24. The crystal structure of AgSb2F11 is related to the already known crystal structure of H3OSb2F11. Vibrational spectra of AgSb2F11 entirely match the literature-reported vibrational spectra of β-Ag(SbF6)2, for which a formulation of a mixed-valence Ag(I)/Ag(III) compound was suggested (AgIAgIII(SbF6)4). On the basis of obtained results it can be concluded that previously reported β-Ag(SbF6)2 is in fact Ag(I) compound with composition AgSb2F11.