Co(μ_2-bpy)V_2O_6(bpy=4,4'-联吡啶)的水热合成和晶体结构  

Synthesis and Crystal Structure of an Inorganic Organic Hybrid Compound Co(μ_2-bpy)V_2O_6 (bpy=4,4′-bipyridine)

作　　者：李增和[1] 银陈[1] 王如骥[2] 王平[1] 郭洪猷[1] 

机构地区：[1]北京化工大学化学系,北京100029 [2]清华大学化学系,北京100084

出　　处：《物理化学学报》2003年第12期1133-1137,共5页Acta Physico-Chimica Sinica

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,犤Co2V4O12犦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0.5nm×0.7nm.漫反射光谱研究表明,此晶体具有约2.0eV的光学能隙,属于半导体,在420℃以下是热稳定的.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,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.

关 键 词：Co(μ2^-bpy)V206 4 4′联吡啶 水热合成 晶体结构 热稳定性 漫反射光谱 钴 钒 杂多酸 

分 类 号：O626[理学—有机化学]