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Two molybdophosphate compounds,[Ni(bim)3]2[H2P2Mo5O23]·2H2O 1 and 2,2-dipyridyl),have been synthesized under hydrothermal conditions and structurally characterized by elemental analysis,TG.and IR.The single-crystal X-ray analysis exhibits that 1 consists of one [H2P2Mo5O23]4-,two[Ni(bim)3]2+ cations and two lattice water molecules,while 2 is constructed from one sandwich-type[ZnP4Mo6]anion modified by four Zn-bpy complexes and nine lattice water molecules.The electrochemical behaviors of compounds 1 and 2 have been studied in detail based on solid bulk modified carbon paste electrodes of compound(CPEs).