Non‐Aqueous Microwave‐Assisted Syntheses of Deca‐ and Hexa‐Molybdovanadates

We report a new approach for the synthesis of heterohexa‐ and heterodecametalates via the use of non‐aqueous, microwave‐assisted reaction conditions. The two novel molybdovanadates have been isolated and characterized in the solid and solution states using single‐crystal X‐ray diffraction, FT‐IR, UV/Vis, multinuclear NMR spectroscopy, and ESI‐MS. The relative stabilities of the possible structural isomers were probed using dispersion‐corrected DFT calculations for both polyoxometalate systems. Six of one, ten of another: Two molybdovanadates are prepared by microwave reaction of a polymolybdate with a polyvanadate. Both heteropolyoxometallates were isolated and characterized in the solid and solution state. The relative stabilities of their structural isomers were determined theoretically.