Oxidation of the molybdate-linked pair having two quadruply bonded Mo24+ units, [Mo2(DAniF)3]2(µ2-MoO4), (DAniF = N,N′-di-(p-anisyl)formamidinate) leads to the formation of a species consisting of three oxidized Mo25+ units connected by two µ3-MoO42− dianions, {[Mo2(DAniF)3]3(µ3-MoO4)2}2+. This cation displays overall D3 point group symmetry due to a slight twisting of the three Mo25+ units about the threefold symmetry axis. This distortion removes all mirror symmetry but preserves all C2 axes orthogonal to the unique C3 axis. Cyclic voltammetry of {[Mo2(DAniF)3]3(µ3-MoO4)2}2+ in CH2Cl2 reveals three reversible one-electron redox processes, corresponding to successive reduction of each of the three Mo25+ units, with ΔE1/2 separations of 0.36 V and 0.41 V.
