The Mo(V) di-μ-oxo type [Mo2O4(H2O)2L]Cl2 complexes(L: 4,4'-Diphenyl-2,2'-dipyridyl, 4,4'-Dimethyl-2,2'-dipyridyl, 4,7-Diphenyl-1,10-phenanthroline) have been prepared by the reaction of [Mo2O4(H2O)6]2+ with a series of chelate ligands. These complexes are completed by two terminal oxygens arranged trans to one another and each ligand forms a chelate types. In Mo2O4(H2O)2L two H2O coordinated at trans site of terminal oxgens. The prepared complexes have been characterized by elemental analysis, infrared spectra, electronic spectra, 1H nuclear magnetic resonance spectra, and thermal analysis(TG-DTA). In the potential range -0.00V to -1.00V at scan rate of 50mVs-1, a cathodic peak at -0.83V ~ -0.88V (vs SCE) and an anodic peak at -0.54V ~ -0.88V (vs SCE) have been observed in aquous solution. The ratio of the cathodic to anodic current(Ipc/Ipa) is almost 2, we infer that redox is irreversible as dimer forms broken.