Synthesis, crystal structure and characterization of ［N(CH3)4］4［Mo10O18(OH)4(O2)10(O2)2］·6H2O

doi:10.3969/j.issn.1000-1565.2021.01.005

Abstract

Abstract: 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, D_c=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.

Key words: peroxo, superoxo, molybdate, synthesis, crystal structure

CLC Number:

O611.2

LIU Xuemei, LI Huimin, DING Liqin, GUO Kexin, LI Jinhuan. Synthesis, crystal structure and characterization of ［N(CH₃)₄］₄［Mo₁₀O₁₈(OH)₄(O₂)₁₀(O₂)₂］·6H₂O[J]. Journal of Hebei University(Natural Science Edition), 2021, 41(1): 32-39.

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Synthesis, crystal structure and characterization of ［N(CH₃)₄］₄［Mo₁₀O₁₈(OH)₄(O₂)₁₀(O₂)₂］·6H₂O

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