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室温条件下,H3PMo12O40.xH2O和水杨醛缩氨基硫脲在95%乙醇溶液中进行原位反应,得到一维链状化合物[C2H8N]3[PMo12O40],对其进行元素分析、ICP、IR、TG-DSC和单晶X射线衍射表征。结果表明,化合物属于菱形晶系,R-3 m空间群,晶胞参数:a=1.652 25(8)nm,b=1.652 25(8)nm,c=2.516 69(14)nm,α=90°,β=90(10)°,γ=120°,V=5.949 9(5)nm3,Z=6,Dc=3.283g/cm3,R1=0.029 7,wR2=0.072 5。化合物分子结构单元由1个[PMo12O40]3-阴离子和3个[(CH3)2NH2]+阳离子构成。化合物分子通过氢键形成二维超分子体系。电化学研究表明,化合物存在两步氧化还原过程。
At room temperature, H3PMo12O40.xH2O and salicylaldehyde thiosemicarbazone were reacted in situ in 95% ethanol solution to obtain one-dimensional chain compound [C2H8N] 3 [PMo12O40], which was subjected to elemental analysis, ICP, IR, TG-DSC and single crystal X-ray diffraction characterization. The results showed that the compounds belong to the rhombohedral system with R-3 m space group with a = 1.652 25 (8) nm, b = 1.652 25 (8) nm and c = 2.516 69 °, β = 90 (10) °, γ = 120 °, V = 5.949 9 (5) nm3, Z = 6, Dc = 3.283 g / cm3, R1 = 0.0297, wR2 = 0.072 5. The compound molecular structure unit consists of one [PMo12O40] 3-anion and three [(CH3) 2NH2] + cations. Compound molecules form a two-dimensional supramolecular system by hydrogen bonding. Electrochemical studies show that compounds exist two-step redox process.