Hydrothermal Synthesis of the First Vanadomolybdenum Polyoxocation with a “Metal-Bonded” Spherical Framework

The heteropoly compound [(V(V)O(4))Mo(VI)(12)O(36)(V(IV)O)(6)][(OH)(9)].11H(2)O (1), synthesized by hydrothermal method under weak basic conditions, represents the first mixed Mo/V six-capped Keggin structural derivative with a spherical skeleton, and the first transition metal polyoxocation. The successful synthesis of 1 demonstrates that basic hydrothermal synthesis might be a power synthetic route to the isolation of more new polycationic metal-oxo clusters.