己二胺-12-钼磷酸电荷转移盐的光化学合成与晶体结构

采用光化学法合成一种有机-无机电荷转移盐，（HMDH2）H2PMo12O40]·AA·3H2O·DMF（HMD = 1,6-己二胺，AA = 乙醛，DMF = N,N-二甲基甲酰胺）超分子化合物。用元素分析，IR，固体漫反射电子光谱，ESR进行了表征。X-射线四圆衍射测定其晶体结构属三斜晶系，空间群Pī，Mr=2081.68，晶胞参数a = 14.092(3)，b =14.347(3)，c =14.358(3)?，α=75.10(3)，β=80.70(3)，γ=80.73(3)°,V=2746.6(10)?3，Z=2，Dc=2.517g/cm3，F(000)=1970，μ(MoKα)=2.766mm-1，全矩阵最小二乘法修正至R=0.0832，wR=0.2638。标题化合物是由1个质子化的1,6-己二胺、12-钼磷混合价杂多阴离子PMo12O40]4ˉ、3个水分子、2个乙醛分子和1个二甲基甲酰胺分子构成。

Photochemical Synthesis and Crystal Structure of a Charge Transfer Salt [HMDH2][H2PMovMo11O40]·2AA·3H2O·DMF

The title supramolecular compound, HMDH2]H2PMoVMo11O40]·2AA·3H2O·DMF ( HMD = hexamethylene diamine; AA=acetaldehyde; DMF=N,N-dimethyl formamide), has been photochemically synthesized by using elemental analysis, IR, solid diffusion reflectance electronic spectra, ESR spectra and X-ray single-crystal analysis. The crystallographic data: triclinic, Pī, a=14.092(2)，b=14.347(3)，c= 14.358(3)?，α = 75.10(3)，β = 80.70(3)，γ = 80.73(3)°，V = 2746.6(10)?3，Z = 2，Mr = 2081.68， Dc=2.517g/cm3，F(000) =1970，μ(MoKα) =2.766mm-1. The structure has been refined to R =0.0832 and wR=0.2638, by full-matrix least-squares method. The title compound is composed of hexamethylene diamine, two acetaldehyde molecules, three water molecules, one N,N-dimethylformamide and H2PMoVMo11O40]2ˉ heteropoly anion.