A new tetramethyl ammonium decamolybdate ［N(CH3)4］4［Mo10O18(OH)4(O2)10(O2)2］·6H2O with peroxo and superoxo groups was synthesized by reacting of 30% hydrogen peroxide as the oxidant, ammonium molybdate and tetramethyl ammonium chloride in aqueous solution at room temperature. The compound was characterized by elemental analysis, IR, UV spectroscopy and Its structure was determined by single crystal Xray diffraction. The compound belongs to monoclinic system with space group P21/c, a=1.443(16)nm, b= 1.168(12)nm, c= 1.693(17)nm, β= 99.32(3)°, V=2.814(5)nm3, Z=2, Dc=2.441 g/cm3, R1 = 0.035 6, wR2 = 0.105 0(I>2, GOF=1.087. The compound anions exhibit a centrosymmetric structure containing two superoxo groups with a bond length of 0.114 5 nm and ten classical peroxo groups with a bond length range of 0.143 5~0.148 1 nm. The compound is unstable in water, but stable in solid state at room temperature, and can rapidly oxidize I- into I2 with the yield of iodine reaching 91.2%, indicating the compound has strong oxidizing properties due to peroxo and superoxo groups in the structure.
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