超分子化合物(bipyH_2)_2(H_2P_2Mo_5O_(23))·H_2O的水热合成、晶体结构和性质  

Hydrothermal Synthesis, Crystal Structure and Properties ofSupermolecular Compound (bipyH_2)_2(H_2P_2Mo_5O_(23))·H_2O

作　　者：赵士龙[1] 黄长沧[1] 张汉辉[1,2] 

机构地区：[1]福州大学化学系 [2]中国科学院福建物质结构研究所结构化学国家重点实验室,福州350002

出　　处：《高等学校化学学报》2002年第4期521-525,共5页Chemical Journal of Chinese Universities

基　　金：福建省自然科学基金(E0110013);福建省教育委员会基金(JA00137)资助.

摘　　要：在水热条件下合成了新型超分子化合物(ｂｉｙｙＨ２)２(Ｈ２Ｐ２Ｍｏ５Ｏ２３)·Ｈ２Ｏ,对其进行了红外光谱、拉曼光谱、紫外－可见漫反射光谱、荧光光谱和循环伏安等分析表征,Ｘ射线单晶结构分析表明,标题化合物属单斜晶系,Ｐ２１/ｃ空间群,晶胞参数α＝１．６７９ ５１(７)ｎｍ,ｂ＝１．１５１ ９３(４)ｎｍ,ｃ＝１．８８９ ０８(８)ｎｍ,β＝１０８．３３５(１)°,Ｖ＝３．４６９ ２(２)ｎｍ３,Ｚ＝４,Ｄｃ＝２．３８２ｇ/ｃｍ３．Ｆ(０００)＝２ ４０８,μ＝１．９５１ｍｍ－１,Ｒ＝０．０２４ ４,Ｒｗ＝０．０７２１．标题化合物的杂多阴离子[Ｐ２Ｍｏ５Ｏ２３]４－由５个ＭｏＯ６畸变的八面体和２个ＰＯ４畸变四面体通过共顶点或共边组成;５个Ｍｏ原子近似处于同一平面,它们和２个Ｐ原子组成了一个畸变的五角双锥构型;杂多阴离子与质子化的４,４'－ｂｉｐｙ和水分子通过氢键连成无限二维网状结构,形成超分子化合物．A novel molybdophosphate supermolecular compound (bipyH2)2(H2P2Mo5O23). H2O has been synthesized by hydrothermal method and characterized by crystal X-ray structure analysis, IR spectrum, Raman spectrum, UV-Vis DRIS spectrum, fluorescence spectrum and CV. The crystal belongs to mono-clinic system with a space group P21/c, a=l. 679 51(7) nm, b=1. 151 93(4) nm, c=1. 889 08(8) nm, β= 108. 335(1)°,V=3. 469 2(2) nm3, Z = 4, Dc = 2. 382 g/cm3, F(000) =2408, μ=1.951mm-1, R=0.024 4, Rw = 0. 072 1. The heteropoly anion[H2P2Mo5O23]4- and protonated 4,4'-bipy are connected to a supermolecular compound by hydrogen bonds; and the anions contain five MoO6 octahedra and two PO4 tetrahedron; Mo, P atoms show a distorted pentagonal bipyramidal configuration, and the heteropoly anions are connected to a infinite planar structure with the protonated 4,4'-bipy.

关 键 词：水热合成 磷钼酸盐 超分子化合物 晶体结构 杂多化合物 

分 类 号：O641.3[理学—物理化学]