溶剂热合成5-氯-8-羟基喹啉-锑(Ⅲ)配合物  

Solvothermal synthesis of antimony(Ⅲ) complex based on 5-chloro-8-hydroxyquinoline

作　　者：赵腾[1] 宋瑞峰[1] 王玉红[1,2] 

机构地区：[1]苏州科技大学化学生物与材料工程学院,江苏苏州215009 [2]江苏省有机合成重点实验室,江苏苏州215123

出　　处：《苏州科技学院学报（自然科学版）》2016年第3期38-43,共6页Journal of Suzhou University of Science and Technology （Natural Science Edition）

基　　金：江苏省有机合成重点实验室资助项目(KJS1308)

摘　　要：采用溶剂热法,在甲醇-水体系中,单质锑与5-氯-8-羟基喹啉(HL)反应生成了一个基于芳氧化合物的新二核锑(Ⅲ)配合物[(SbL_2)_2(μ_2-O)]1,水在合成中起到了重要的作用。利用红外光谱、元素分析、热失重分析、X射线粉末衍射和单晶衍射等给予表征。配合物1属于单斜晶系,P21/c空间群,晶胞参数a=7.402 2(4),b=7.672 1(5),c=28.898(2),茁=94.217(7)°,V=1 636.68(19)3,Z=2。锑(Ⅲ)离子为五配位的四方锥形配位几何构型,两个锑(III)离子通过氧原子桥连形成二核分子。通过分子间的π-π、Sb···Sb相互作用与Sb···O弱作用,沿a方向形成准一维链结构;借助与分子间弱的C-H···Cl氢键将准一维链堆积为准三维结构。配合物1的热稳定性高,在409℃前是稳定的。固体Uv-Vis-Nir漫反射光谱结果显示它的光学能隙约为2.7 e V,表明配合物具有潜在的半导体性质。CCDC:1444057。The new dinuclear antimony complex 1 that features aryloxide ligand, namely [（SbL2）2（μ2-O）] （L=5- chloro-8-hydroxyquinoline anion） was synthesized hydrothermally from metal antimony and 5-chloro-8-hydrox- yquinoline （HL） in methanol/water system. Water played a very important role in the synthesis of complex 1. Its structure was characterized by IR,elemental analysis and single crystal X-ray diffraction analysis. Complex 1 belongs to monoclinie system and space group P2 1/c with unit cell parameters a=7.402 2（4） A,b=7.672 1（5） A,c= 28.898（2） A, β=94.217（7）°, V=I 636.68（19） A3,z=2. Antimony（Ⅲ） ion is five coordinate and square pyramidal coordination geometry,and two antimony （Ⅲ） ions are bridged by the oxygen atom to form a dinuclear molecule. A quasi-one-dimensional chain structure along the a direction was formed through intermolecular π- π, Sb...Sb and Sb... O interactions. These quasi-one-dimensional chains were joined to a quasi-three-dimen- sional structure by the intermolecular C-H… Cl hydrogen bonds. The thermal stability of compound 1 is stable at 409 ℃. The solid Uv-Vis-Nir diffuse reflectance spectra show that the optical energy gap of the solid is about 2.7 eV, which indicates that the complex 1 has the potential semiconductor property.

关 键 词：溶剂热合成 晶体结构 锑(Ⅲ)配合物 5-氯-8-羟基喹啉 

分 类 号：O614.531[理学—无机化学]