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The mixed-valence heteropolyanion VMo12O40 n-(where n=4,5,6) in aprotic media wasinvestigated by cyclic voltammatry and in-situ FTIR and UV-visible-near-lRspectroelectrochemical methods. The results indicate that the heteropolyanion VMo12O403-undergoes three reversible one electron transfer reductions and the mixed-valenceheteropolyanion VMo12O40n-(where n=4,5,6) was formed after electroreduction. The spectraof the aforementioned mixed-valence compounds were characterized by in-situspectroelectrochemical mathods