高等学校化学学报

高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (4): 521.

• 研究论文 • 上一篇    下一篇

超分子化合物(bipyH2)2(H2P2Mo5O23)·H2O的水热合成、晶体结构和性质

赵士龙1, 黄长沧1,2, 张汉辉1   

  1. 1. 福州大学化学系, 福州 350002;
    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
  • 收稿日期:2001-07-27 出版日期:2002-04-24 发布日期:2002-04-24
  • 通讯作者: 张汉辉(1947年出生),男,教授,博士生导师,主要从事簇合物的结构化学研究.
  • 基金资助:

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

Hydrothermal Synthesis, Crystal Structure and Properties ofSupermolecular Compound (bipyH2)2(H2P2Mo5O23)·H2O

ZHAO Shi-Long1, ZHANG Han-Hui1,2, HUANG Chang-Cang1   

  1. 1. Department of Chemistry, Fuzhou University, Fushou 350002, China;
    2. State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002, China
  • Received:2001-07-27 Online:2002-04-24 Published:2002-04-24

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摘要： 在水热条件下合成了新型超分子化合物(bipyH2)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=1.67951(7)nm,b=1.15193(4)nm,c=1.88908(8)nm,β=108.335(1)°,V=3.4692(2)nm3,Z=4,Dc=2.382g/cm3.F(000)=2408,μ=1.951mm-1,R=0.0244,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。

关键词: 水热合成, 磷钼酸盐, 超分子化合物, 晶体结构

Abstract: Anovel 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.67951(7) nm, b=1.15193(4) nm, c=1.88908(8) nm, β= 108.335(1)°,V=3.4692(2) nm3, Z = 4, Dc = 2.382 g/cm3, F(000) =2408, μ=1.951mm-1, R=0.0244, Rw = 0.0721.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, Patoms show a distorted pentagonal bipyramidal configuration, and the heteropoly anions are connected to a infinite planar structure with the protonated 4,4'-bipy.

Key words: Hydrothermal synthesis, Molybdophosphate, Supermolecular compound, Crystal structure

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