Two electron-rich, metal-metal bonded pentamolybdate hybrids, 2D-[MoIV3MoVI2OSr(HO)(CHO)py]·3.5HO (1) and 1D-[MoIV3MoVI2OSr(HO)(CHO)py]·py·2[NH(CH)]·2HO (2, py = pyridine), were prepared by the partial solvothermal oxidation of [MoIV3O(OCCH)(HO)]ZnCl·8HO and citric acid in py/HO (for 1) or py/HO/DMF (for 2). Both 1 and 2 feature a triangularly metal-metal bonded incomplete cuboidal [MoIV3O] unit. Redox-active 6-[MoIV3O] units can serve as an "electron sponge" to store/release six electrons reversibly Δ-bond breakage and re-formation during charging/discharging processes. 1 and 2 further form 3D and 2D supramolecular structures, respectively, through slipped π-π stacking interactions between the pyridine ligands. Both the incorporated 6-redox active [MoIV3O] unit and the 3D/2D supramolecular conductive networks in hybrid-POM 1/2 remarkably enhance the electronic conductivity and reversible multi-electron redox ability with the structural integrity retained. Consequently, 1 and 2 exhibited high discharge specific capacities of 236.0 and 277.0 mA h g at 50 mA g, respectively, and a good cycling performance at high current density (121.8 mA h g, 2 A g for 2), providing a new way for improving POM-based electrode materials.
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