摘要:
水热法合成~种新化合物[C10N2H10]2[H2P2Mo5O23]·2H2O,并通过红外光谱、元素分析、X线单晶衍射分析和电化学分析等手段进行表征.晶体数据结果表明,晶体属于三斜晶系,P-1空间群,晶胞参数分别为a=0.995 15(11) nm,b-1.123 67 (13) nm,c=1.758 1(2) nm,α=73.454(1)°,β=84.036(1)°,γ=68.002(1)°,V=1.747 3(3) nm3;Z=2;最后的一致性因子R1=0.030 5,wR2 =0.077 3.标题化合物由两个质子化的4,4'联吡啶和一个杂多阴离子[H2P2Mo5O23]4-组成.循环伏安法显示该化合物具有可逆的氧化还原性能,电子转移数为1,相关电对为Mo(Ⅵ)/Mo(Ⅴ).%A new compound [C10N2H10]2[H2P2Mo5 023]·2H2O, containing the heteropolyanion, [H2P2Mo5O23]4- , together with diprotonated 4,4 -bipyridine, had been synthesized by hydrothermal method and characterized by crystal X-ray structure analysis, IR spectrum and CV. The results of X-ray single crystal diffraction was shown that the compound crystallized in space group P-l of triclinic system with a = 0.995 15 (11) nm, 6=1. 123 67 (13) nm, c=1. 758 1(2) nm, α = 73. 454(1)°, β= 84.036(1)°, γ=68. 002(1)°, V=l. 747 3(3) nm3; Z=2;R1, =0. 030 5, wR2 =0. 077 3. The heteropolyanion was built up from five MoO6 distorted octahedral sharing four common edges and one common corner, capped by two PO4 distortion tetrahedron. Cyclic voltammetric measurement of the compound revealed that the molybdenum was reduced irreversibly. The electron transfer number in) involved in reduction processes could be calculated to be approximately 1, which corresponded to the Mo(Ⅵ) / Mo(Ⅴ)couple.