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The first polyoxometalates (POMs) composed of MoIV, MoV2, discrete d1‐MoV and MoVI, [MoIV3MoV6MoVI4O32(μ2‐OH)(μ3‐OH)py9] (1), was prepared from the solvothermal partial oxidation of [MoIV3O2(O2CCH3)6(H2O)3]ZnCl4 in a mixture of pyridine and water. The MoV=O adduct‐free unit [H2Mo12O33py9] presents the 11e‐reduced Mo derivative of the paratungtic archetype. The use of methanol, ethanol, n‐propyl alcohol...