12-钼磷酸四丁基铵杂多蓝的光化学合成表征与晶体结构

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用450W高压汞灯照射H3PMo12O40·5H2O和(Bu4N)Br(TBA)的DMF(N,N-二甲基甲酰胺)溶液,合成了12-钼磷酸四丁基铵杂多蓝(Bu4N)4[PMo12O40]·2DMF·H2O,用元素分析,IR,固体漫反射电子光谱,ESR,XPS和CV等进行了表征。晶体结构分析表明,标题化合物属单斜晶系,空间群P21/c,晶胞参数a=14.124(3),b=17.481(4),c=22.744(5)A,β=101.66(3)°,V=5500(2)A3,C70H160Mo12N6O43P,Mr=2956.29,Z=2,Dc=1.785g/cm3,F(000)=2970,μ(MoKα)=1.412mm-1,R=0.0638,wR=0.1975。标题化合物是由4个四丁基铵阳离子、1个12-钼磷混合价杂多阴离子[PMo12O40]4-、2个DMF分子和1个水分子构成。 A solution of H3PMo12O40.5H2O and (Bu4N) Br (TBA) in DMF (N, N-dimethylformamide) was irradiated with a 450W high pressure mercury lamp to synthesize tetrabutylammonium tetosulfonate (Bu4N) 4 [ PMo12O40] · 2DMF · H2O, characterized by elemental analysis, IR, solid-state diffuse reflectance electron spectroscopy, ESR, XPS and CV. The crystal structure analysis showed that the title compound belongs to the monoclinic system with space group P21 / c. The unit cell parameters a = 14.124 (3), b = 17.481 (4), c = 22.744 °, V = 5500 (2) A3, C70H160Mo12N6O43P, Mr = 2956.29, Z = 2, Dc = 1.785g / cm3, F (000) = 2970, μ (MoKα) = 1.412mm-1, R = 0.1975. The title compound consists of four tetrabutyl ammonium cations, one 12-molybdophosphoric mixed heteropolyanion [PMo12O40] 4-, two DMF molecules and one water molecule.
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