梯桥状有机锡氧杂环二聚体[(n-BuSn)_6(μ_3-O)_4(C_4H_3SCO_2)_8Cl_2]的合成及结构  

Synthesis and Crystal Structure of a Novel Iadder-Bridge-Shaped Heterometallacylic Organooxotin Dimer,[(n-BuSn)_6(μ_3-O)_4(C_4H_3SCO_2)_8Cl_2]

作　　者：邝代治[1] 冯泳兰[1] 张复兴[1] 王剑秋[1] 彭雁[1] 庾江喜[1] 蒋伍玖[1] 朱小明[1] 

机构地区：[1]功能金属有机材料湖南省高校重点实验室衡阳师范学院化学与材料科学系,湖南衡阳421008

出　　处：《衡阳师范学院学报》2015年第3期1-4,共4页Journal of Hengyang Normal University

基　　金：湖南省科技计划(2014NK3086);湖南省自然科学基金(13JJ3112);湖南省高校创新平台开放基金(13K105;13K01;14K014;GN14K01);湖南省十二五重点建设学科及学院协同创新中心培育项目(12XT02)

摘　　要：2-噻吩甲酸和正丁基锡酸反应后经三氯甲烷处理,获得一结构新颖的有机锡氧杂环二聚体化合物[(nBuSn)6(μ3-O)4(C4H3SCO2)8Cl2],经IR、1 HNMR和元素分析表征,并用X-射线晶体衍射测定了分子结构,该化合物晶体属于三斜晶系,空间群P-1,晶胞参数:a=1.2484(3)nm,b=1.3656(3)nm,c=1.5224(3)nm,α=67.94(3)°,β=65.99(3)°,γ=66.72(3)°,V=2.1053(7)nm3,Z=2,Dc=1.929g/cm3,μ(MoKa)=2.270mm-1,F(000)=1200,R1=0.0415and wR2=0.1160.晶体结构分析表明,化合物通过μ3-O与3个Sn原子配位和羧基氧桥联2个Sn原子,形成Sn-O键构筑的中心对称梯桥状[Sn4(μ3-O)4]结构和8个由羧基组装的锡氧六元杂环(-CO2Sn2O)支撑其梯桥的有机锡氧簇化合物。A Novel dimeric compound,[（n-BuSn）6 （μ3-O）4 （C4 H 3 SCO2 ）8 Cl2 ]has been obtained by the reaction of of n-BuSn（O） （OH）with 2-thiophenecarboxylic acid,and then treated with HCCl3 .The structures were characterized by IR,1 H NMR,ele-mental analysis and the molecular structure of compound was determined by X-ray analysis.The crystal belongs to triclinic sys-tem,space group P-1 with the cell parameters：a = 1.2484（3）nm,b = 1.3656（3）nm,c = 1.5224（3）nm,α = 67.94（3）°,β= 65.99（3）°,γ = 66.72（3）°,V = 2.1053（7）nm 3 ,Z = 2,Dc = 1.929g /cm 3 ,μ（MoKa）= 2.270mm-1 ,F（000）=1200, R1 = 0.041 5 and wR2 = 0.1 1 60.The compound is a cluster structure with Sn-O bond.The three tin atoms are held together by aμ3-oxygen atom,and the two tin atoms in each tritin are carboxyl-bridged.The compound having a centro-symmetric lad-der-bridge [Sn4 （μ3-O）4 ]and eight the six-membered （-CO2 Sn 2 O）ring,the compounds formed a like ladder-bridge-shaped structure.

关 键 词：锡氧杂环化合物 桥状结构 合成 晶体结构 

分 类 号：O614.432[理学—无机化学]