三(邻溴苄基)溴化锡和四(对溴苄基)锡的合成及结构研究

Study on Synthesis and Crystal Structure of Tri(o-bromobenzyl)tin Bromide and Tetra(p-bromobenzyl)tin

邻溴苄基溴或对溴苄基溴与锡反应合成三 (邻溴苄基 )溴化锡 ( 1)和四 (对溴苄基 )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属斜方六面体晶系 ,空间群为R 3 ,晶体学参数 :a =1 3 3 89( 3 )nm ,b =1 3 3 89( 3 )nm ,c =2 1896( 8)nm ,V =3 3 993 ( 16)nm3 ,Z =6,Dx=2 0 77Mg·m-3 ,μ(MoKα) =81 83cm-1,F( 0 0 0 ) =2 0 0 4,R1=0 0 477,wR2 =0 13 72 ;晶体结构 2属正交晶系 ,空间群为Fdd2 ,晶体学参数 :a =2 10 2 7( 7)nm ,b =2 3 0 3 4( 8)nm ,c =1 14 3 1( 4 )nm ,V =5 5 3 6( 3 )nm3 ,Z =8,Dx=1 917Mg·m-3 ,μ(MoKα) =67 11cm-1,F( 0 0 0 ) =3 0 5 6,R1=0 0 3 5 8,wR2 =0 0 65 9.化合物 1中Sn—C键长为 0 2 160 ( 8)nm ,Sn—Br键长为 0 2 491( 3 )nm ;化合物 2中Sn—C键长分别为 0 2 175和 0 2 178nm .中心锡与亚甲基碳 (或溴 )

The n-butyl alcohol solution of o-bromobenzyl bromide or p-bromobenzyl bromide and Sn was heated at reflux for 6 h to yield tri(o-bromobenzyl)tin bromide (1) and tetra(p-bromobenzyl)tin (2). The crystal and molecular structures of compounds 1 and 2 were determined by X-ray diffraction analysis. The crystal 1 is rhombohedral, space group R-3 with a=1.3389(3) nm, b=1.3389(3) nm, c=2.1896(8) nm, V=3.3993(16) nm 3, Z=6, D x=2.077 Mg·m -3, μ(Mo Kα)=81.83 cm -1, F(000)=2004, R 1=0.0477, wR 2=0.1372. The crystal 2 belongs to orthorhombic, space group Fdd2 with a=2.1027(7) nm, b=2.3034(8) nm, c=1.1431(4) nm, V=5.536(3) nm 3, Z=8, D x=1.917 Mg·m -3, μ(Mo Kα)=67.11 cm -1, F(000)=3056, R 1=0.0358, wR 2=0.0659. The bond lengths of Sn—C are 0.2160(8) nm and 0.2175～0.2178 nm, respectively. The length of Sn—Br is 0.2491(3) nm. The tin atom has a distorted tetrahedral geometry.