12-钼磷酸四丁基铵杂多蓝的光化学合成表征与晶体结构

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）4PMo12O40]·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。

Photochemical Synthesis, Characterization and X-ray Crystal Structure of Dodecamolybdophosphate Tetrabutylammonium Heteropoly Blue (Bu4N)4[PMo12O40]·2DMF·H2O

In this paper, we will report the preparation of a mixed-valence polyoxometalate compound (Bu4N)4PMo12O40]·2DMF·H2O (TBA = tetrabutylammonium; DMF = N,N-dimethyl formamide). The title compound has been photochemically synthesized and characterized by using elemental analysis, IR, solid diffusion reflectance electronic spectra, ESR spectra, XPS, CV and X-ray single-crystal analysis. The crystallographic data are as follows: monoclinic, P21/c, 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= 1.785 g/cm3, F(000) = 2970 and μ(MoKα) = 1.412 mm-1. The structure has been refined to R = 0.0638 and wR = 0.1975 by full-matrix least-squares methods. The title compound is composed of four tetrabutylammonium cations, one PMovMo11O40]4- heteropoly anion, two N,N-dimethyl formamide and one H2O molecule.