三(邻氟苄基)氯化锡和四(对氟苄基)锡的合成及结构研究  

Study on the Synthesis and Crystal Structures of Tri(o-fluorobenzyl)tin Chloride and Tetra(p-fluorobenzyl)tin

作　　者：张复兴[1] 邝代治[1] 冯泳兰[1] 王剑秋[1] 许志锋[1] 

机构地区：[1]衡阳师范学院化学系,衡阳421008

出　　处：《有机化学》2003年第4期368-371,共4页Chinese Journal of Organic Chemistry

基　　金：湖南省自然科学基金 (No.0 0JJY2 0 1 0 );湖南省教育厅重点 (No.0 0A0 0 4 )资助项目

摘　　要：邻氟苄基氯或对氟苄基氯分别与锡反应合成三 (邻氟苄基 )氯化锡 ( 1)和四 (对氟苄基 )锡 ( 2 ) .经X射线方法测定了新化合物的晶体结构 .晶体结构 1属单斜晶系 ,空间群为P2 ( 1) /n ,晶体学参数 :a =0 5 896( 9)nm ,b =1 2 62 ( 2 )nm ,c =2 63 4( 4 )nm ,V =1 95 9( 5 )nm3 ,Z =4,Dx=1 63 2g/cm3 ,μ(MoKα) =14 69cm-1,F( 0 0 0 ) =95 2 ,R1=0 0 5 41,wR2 =0 12 80 ;晶体结构 2属单斜晶系 ,空间群为Cc,晶体学参数 :a =1 0 778( 6)nm ,b =2 3 3 12 ( 14 )nm ,c =1 0 888( 7)nm ,V =2 460 ( 3 )nm3 ,Z =4,Dx=1 499g/cm3 ,μ(MoKα) =10 82cm-1,F( 0 0 0 ) =1112 ,R1=0 0 3 0 2 ,wR2 =0 0 5 90 .在化合物 1和2中Sn—C键长分别为 0 2 13 6～ 0 2 14 8和 0 2 13 8～ 0 2 180nm ,Sn—Cl键长为 0 2 3 78( 4 )nm ,中心锡与亚甲基碳 (氯 )原子构成畸型四面体 .The n-butyl alcohol solution of o-fluorobenzyl chloride or p-fluorobenzyl chloride mid Sn was heated at reflux for 5 h to yield tri( o-fluorobenzyl) tin chloride (1) and tetra(p-fluorobenzyl) tin (2), respectively. The crystal,and molecular structures of compounds 1 and 2 were determined by X-ray diffraction study. The crystal 1 are monoclinic, space group P2(1)/n with a = 0.5896(9) nm, b = 1.262(2) nm, c = 2.634(4) nm, V = 1.959(5) nm(3), Z = 4, D-x = 1. 632 g/cm(3), mu (Mo Kalpha) = 14.69 cm(-1), F (000) = 952, R-1 = 0. 0541, omegaR(2) = 0.1280. The crystal 2 belongs to monoclinic, space group Cc,with a = 1.0778(6) nm, b = 2.3312(14) nm, c = 1.0888(7) nm, V=2.460(3)nm(3), Z=4, D-x = 1.499g/cm(3), mu(Mo Kalpha)= 10.82 cm(-1), F(000)=1112, R-1=0.0302, omegaR(2) = 0.0590. The bond lengths of Sn---C are 0.2136similar to0.2148 and 0.2138similar to0.2180 nm, respectively. The bond length of Sn--Cl is 0.2378 nm. The tin atom adopts a distorted tetrahedral geometry.

关 键 词：三(邻氟苄基)氯化锡 四(对氟苄基)锡 合成 结构 有机锡化合物 

分 类 号：O627[理学—有机化学]