物理化学学报 >> 2003, Vol. 19 >> Issue (12): 1133-1137.doi: 10.3866/PKU.WHXB20031208

研究论文 上一篇    下一篇

Co(μ2-bpy)V2O6 (bpy =4,4′-联吡啶)的水热合成和晶体结构

李增和;银陈;王如骥;王平;郭洪猷   

  1. 北京化工大学化学系,北京 100029;清华大学化学系,北京 100084
  • 收稿日期:2003-05-16 修回日期:2003-08-11 发布日期:2003-12-15
  • 通讯作者: 郭洪猷 E-mail:guohy@public.fhnet.cn.net

Synthesis and Crystal Structure of an Inorganic-Organic Hybrid CompoundCo(μ2-bpy)V2O6 (bpy=4,4’-bipyridine)

Li Zeng-He;Yin Chen;Wang Ru-Ji;Wang Ping;Guo Hong-You   

  1. Department of Chemistry, Beijing University of Chemical Technology, Beijing 100029;Department of Chemistry, Tsinghua University, Beijing 100084
  • Received:2003-05-16 Revised:2003-08-11 Published:2003-12-15
  • Contact: Guo Hong-You E-mail:guohy@public.fhnet.cn.net

摘要: 采用CoCl2•6H2O、4,4′-联吡啶和NH4VO3,以H2O作溶剂(摩尔比1∶2∶2∶1950)在170 ℃下水热反应合成无机-有机杂化化合物Co(μ2-bpy)V2O6 (bpy=4,4′-联吡啶), 经单晶X射线衍射测定其晶体结构.此晶体属三斜晶系,空间群为Pī,晶胞常数a=0.81599(7) nm,b=0.85826(7) nm, c=1.02031(8) nm,α=87.111(2)°, β=75.305(2)°,γ=74.784(2)°, Z=2. Co(μ2-bpy)V2O6是无机的双金属氧化物层,[Co2V4O12]n通过有机的桥式配体μ2-bpy以N-Co配位键桥联而成.晶体的三维共价结构含有多种开放式孔道,其中最大孔道的尺寸为0.5 nm×0.7 nm.漫反射光谱研究表明,此晶体具有约2.0 eV的光学能隙,属于半导体,在420 ℃以下是热稳定的.

关键词: Co(μ2-bpy)V2O6, 水热合成, 晶体结构,  热稳定性, 漫反射光谱

Abstract: A novel inorganic/organic hybrid compound Co(μ2-bpy)V2O6 was synthesized by hydrothermal reaction of CoCl2•6H2O, 4,4′-bipyridine,NH4VO3,and H2O in a molar ratio of 1∶2∶2∶1950 at 170 ℃ for 72 h. The compound crystallized in triclinic space group Pī,with the cell parameters a=0.81599(7) nm, b=0.85826(7) nm, c=1.02031(8) nm, α=87.111(2)°, β=75.305(2)° and γ=74.782(2). As showed by single crystal X-ray diffraction, The crystal structure is constructed with inorganic bimetallic oxide layers, [Co2V4O12]n, and organic 4,4′-bipyridine μ2-ligands.The 4,4′-bipyridine ligands bridge the inorganic layers through N-Co coordination bonds to build up a three dimensional covalent framework with various open micropores. UV-Vis-NIR reflectance spectrum study revealed the nature of a semiconductor with an energy gap of ca.2.0 eV and thermal analysis showed thermal stability below 420 ℃ for the title compound.

Key words: Co(μ2-bpy)V2O6, Hydrothermal synthesis, Crystal structure, Thermal stability, Diffuse reflectance spectra