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有机化学 ›› 2004, Vol. 24 ›› Issue (1): 80-84. 上一篇    下一篇

研究简报

三(邻溴苄基)溴化锡和四(对溴苄基)锡的合成及结构研究

王剑秋, 邝代治*, 张复兴, 冯泳兰, 许志锋   

  1. 衡阳师范学院化学与材料科学系 衡阳 421008
  • 收稿日期:2003-01-16 修回日期:2003-06-10 接受日期:2003-07-07 发布日期:2022-09-21
  • 基金资助:
    湖南省自然科学基金(Nos. 00JJY2010, 02JJY3005)和湖南省教育厅(Nos. 02C135, 02C137)资助项目.

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

WANG Jian-Qiu, KUANG Dai-Zhi*, ZHANG Fu-Xing, FENG Yong-Lan, XU Zhi-Feng   

  1. Department of Chemistry and Material Science, Hengyang Normal University, Hengyang 421008
  • Received:2003-01-16 Revised:2003-06-10 Accepted:2003-07-07 Published:2022-09-21
  • Contact: *E-mail: hnkdz@yahoo.com.cn

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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=1.3389(3) nm, b=1.3389(3) nm, c=2.1896(8) nm, V=3.3993(16) nm3, Z=6, Dx=2.077 Mg·m－3, μ(Mo Kα)=81.83 cm－1, F(000)=2004, R1=0.0477, wR2=0.1372;晶体结构2属正交晶系,空间群为Fdd2,晶体学参数:a=2.1027(7) nm, b=2.3034(8) nm, c=1.1431(4) nm, V=5. 536(3) nm3, Z=8, Dx=1.917 Mg·m－3, μ(Mo Kα)=67.11 cm－1, F(000)=3056, R1=0.0358, wR2=0.0659.化合物1中Sn—C键长为0.2160(8) nm, Sn—Br键长为0.2491(3) nm;化合物2中Sn—C键长分别为0.2175和0.2178 nm.中心锡与亚甲基碳(或溴)原子构成畸型四面体.

关键词: 三(邻溴苄基)溴化锡, 四(对溴苄基)锡, 晶体结构

The n-butyl alcohol solution of o-bromobenzyl bromide or p-bromobenzyl bromide and Sn was heated at reflux for 6 h toyield tri(o-bromobenzyl)tin bromide (1) and tetra(p-bromobenzyl)tin (2). The crystal and molecular structures of compounds 1 and 2 weredetermined 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) nm3, Z=6, Dx=2.077 Mg·m－3, μ(Mo Kα)=81.83 cm－1, F(000)=2004, R1=0.0477, wR2=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) nm3, Z=8, Dx=1.917 Mg·m－3, μ(Mo Kα)=67.11 cm－1, F(000)=3056, R1=0.0358, wR2=0.0659. The bondlengths 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.

Key words: tri(o-bromobenzyl)tin bromide, tetra(p-bromobenzyl)tin, crystal structure