摘要
以NH4VO3,Zn(AC)2和5,5’-mbpy(5,5’-dimethyl-2,2’-bipyridyl)为原料,水热法合成了一个新的钒酸盐化合物[Zn(5,5’-mbpy)(H2O)V2O6]。通过元素分析、红外光谱对其结构进行了表征,利用热重法测定了化合物的稳定性。用X射线单晶衍射法测定了化合物的晶体结构,结果分析表明:晶体属于三斜晶系,P-1空间群,a=0. 8635(9) nm,b=0. 9506(10) nm,c=1. 0781(11) nm,α=93. 817(14)°,β=100. 607(13)°,γ=109. 129(15)°,V=0. 8141(15) nm^3,F000=464,Z=2,R1=0. 0273,wR2=0. 0725。该晶体结构的特点是由[V4O12]4-阴离子簇和[Zn(5,5’-mbpy)(H2O)]2+阳离子形成的一维链状结构,链与链之间进一步通过分子间弱作用力堆积成三维超分子结构。热重分析表明,化合物晶体结构在温度升至155℃时开始分解,该化合物具有一定的稳定性。
A new polyvanadate[Zn( 5,5’-mbpy)( H2 O) V2O6]had been synthesized under hydrothermal conditions by using NH4 VO3,Zn( AC)2 and 5,5’-mbpy( 5,5’-dimethyl-2,2’-bipyridyl) as raw materials.The complex was characterized by elemental analysis,infrared spectrum( IR),and thermogravimetric analysis. X-ray single crystal diffraction analysis revealed that the complex crystallizes in the space group P-1 of Triclinic system with a = 0. 8635( 9) nm,b = 0. 9506( 10) nm,c = 1. 0781( 11) nm,α= 93. 817( 14)°,β= 100. 607( 13)°,γ= 109. 129( 15)°,V = 0. 8141( 15) nm^3,F( 000)= 464,Z = 2,R1= 0. 0273,wR2= 0. 0725. The crystal features a one-dimensional chain-like structure constructed by[V4 O12]4-anionic clusters and[Zn( 5,5’-mbpy)( H2 O)]2+cations.These chains further extend into a 3 D supramolecular structure by weak intermolecular forces.The thermal analysis showed that the title compound is stable under the temperature of 155 ℃.
作者
郑新芳
何学丽
韩占刚
李俊峰
韩晓
ZHENG Xin-fang;HE Xue-li;HAN Zhan-gang;LI Jun-feng;HAN Xiao(College of Chemistry and Chemical Engineering and Material Science,Handan College,Handan 056005,China;College of Chemistry & Material Science,Hebei Normal University,Shijiazhuang 050024,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2019年第8期1416-1421,共6页
Chemical Research and Application
基金
国家自然科学基金青年科学基金项目(21803016)资助
邯郸学院校级项目(16106
2017310)
关键词
水热合成
晶体结构
有机-无机杂化钒酸盐
hydrothermal synthesis
crystal structure
organic-inorganic hybrid vanadate
