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The lead fluoridooxidovanadates(V), Pb(V2O2F8) and Pb(VOF5), were synthesized from PbF2 and VOF3 in anhydrous HF. Their crystal structures were determined and Raman spectra recorded. Compound Pb3F(V4O3F18) with a novel mixed valent vanadium(IV, V) fluoridooxido anion, V4O3F185–, obtained as a by‐product, was also structurally characterized.
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