二茂铥苯并噻唑-2-烃硫基配合物的合成及其晶体结构  

Synthesis and X ray Crystal Structures of Biscyclopentadienyl thulium Benzothiazole-2-thiolate Cp_2Tm(SBT)(THF)

作　　者：张立新[1] 周锡庚[1] 黄祖恩[1] 蔡瑞芳[1] 张丽蓓[1] 吴锵金[2] 

机构地区：[1]复旦大学化学系,上海200433 [2]福建结构化学国家重点实验室,福州350002

出　　处：《Chinese Journal of Structural Chemistry》2001年第1期40-43,共4页结构化学（英文）

基　　金：国家自然科学基金;配位化学国家重点实验室资助课题 !(2 9872 0 0 9)

摘　　要：Cp3Tm和HSBT(HSBT =2 巯基苯并噻唑 )在THF中反应 ,生成Cp2 Tm (SBT) (THF)(TmS2 NOC2 1 H2 2 Mr=537.47) ,该晶体为正交晶系 ,空间点群为P2 1 2 1 2 1 ,晶胞参数a =1 4 734(7) ,b=1 0 .680 (1 ) ,c =1 2 .82 0 (4) ,V =2 0 1 7(3) 3,Z =4,Dc=1 .77g/cm3,F(0 0 0 ) =1 0 56,μ(MoKα) =46.53cm- 1 ,独立反射点数为 2 2 77,其中I >3σ(I)的可观测点为 1 854个 ,最终偏离因子R =0 .0 50 ,Rw=0 .0 67。晶体结构显示 ,该化合物为单体结构 ,中心铥原子分别与两个茂基、苯并噻唑 2 烃硫基上的硫原子和氮原子以及一个四氢呋喃分子配位 ,形成一个变形的三角双锥构型。(C5H5)(3) Tm reacted with equimolar of 2-mercapto-benzothiazole (HSBT) in THF at room temperature to give (C5H5)(2) Tm(SBT) (THF) (TmC21H22ONS2 M-r = 537. 47), which crystallized in the orthorhombic system space group P2(1)2(1)2(1) with unit cell dimensions a = 14.734(7), b = 10.680(1), c = 12.820(4) Angstrom, V = 2017(3) Angstrom (3), Z = 4, D-c = 1.77g/cm(3), F(000) = 1056, and mu = 46.53 cm(-1). Least-squares refinement of the model based on 1854 reflections with I > 3 sigma (I) converged to the final factor R = 0.050, R-w = 0.067. The crystal structure analysis showed that in the complex each thulium ion is coordinated by two eta (5)-cyclopentadienyl groups, one oxygen atom of THF, one sulfur and one nitrogen atoms from the chelating benzothiazole-2-thiolate ligand to form a distorted trigonal-bipyrimidal geometry.

关 键 词：2-巯基苯并噻唑 铥配合物 合成 晶体结构 

分 类 号：O627[理学—有机化学]