The complex of molybdenum(Ⅵ) peroxo glycine was synthesized by solid-liquid state reaction with molybdenum trioxide and glycine as starting materials. The composition and structure of the complex was characterized by elemental analysis, UV spectra, infrared spectra, thermogravimetry- differential scanning calorimetry (TG-DSC) and X-ray powder diffraction. The results demonstrate that the structural formula of the complex is [MoO(O2)2(C2H5NO2)]?H2O, and the glycine is coordinated as azwitterion via one oxygen. The molybdenum(Ⅵ) atom is six coordinated by one O atom of oxo group, four O atoms from two bidentate peroxo groups and one O atom from the carboxyl of glycine, respectively. The results of indexes to the X-ray powder diffraction data indicate that the crystal structure of the complex belongs to monoclinic system. The lattice parameters are: a = 1.7763 nm, b = 1.5972 nm, c = 1.9670 nm, β = 89.15?