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.