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化学学报
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化学学报 ›› 2002, Vol. 60 ›› Issue (5): 897-903. 上一篇    下一篇

研究论文

双核有机锡（IV）配合物[Ph_3Sn(CH_3OH)O_2CC_6H_4CO_2(CH_3OH)-SnPh_3]·2CH_3OH和[Ph_3SnS_2CN(CH_2CH_2)_2NCS_2SnPh_3]·2CH_3OH的合成、表征和晶体结构

尹汉东;马春林;王勇;房海霞;邵建新   

  1. 聊城师范学院化学系,聊城(252059);潍坊医学院生化教研室,潍坊(261000)
  • 发布日期:2002-05-15

Synthesis and Crystal Structure of Binuclear Organotin (IV) Complexes [Ph_3Sn(CH_3OH)O_2CC_6H_4CO_2(CH_3OH)-SnPh_3]·2CH_3OH and [Ph_3SnS_2CN(CH_2CH_2)_2NCS_2SnPh_3]·2CH_3OH

Yin Handong;Ma Chunlin;Wang Yong;Fang Haixia;Shao Jianxin   

  1. Department of chemistry, Liaocheng Teachers University,Liaocheng (252059);Department of Chemistry, Weifang Medical College,Weifang (261000)
  • Published:2002-05-15

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利用三苯基氯化锡和对苯二甲酸二钠、哌嗪荒酸二钠在甲醇中反应，合成了双 核有机锡（IV）配合物[Ph_3Sn(CH_3OH)O_2CC_6H_4CO_2(CH_3OH)SnPh_3]· 2CH_3OH和[Ph_3SnS_2CN(CH_2CH_2)_2NCS_2SnPh_3]·2CH_3OH（2）。通过元素分 析、红外光谱和核磁共振氢谱对其结构进行了表征。用X射线单晶衍测定了这两个 化合物的晶体结构。化合物质1为单斜晶系，空间群P2_1/n，a = 1.5199(5) nm， b = 0.9000(3) nm，c = 1.8206(6) nm，β=113.970(5)°，Z = 2，V = 2.2755 (13) nm~3，D_c = 1.413 g/cm~3，μ = 1.146 mm~(-1)，F(000) = 980，R_1 = 0.0353，wR_2 = 0.0606。化合物2为单斜晶系，空间群P2_1/c，a = 1.5066(5) nm，b = 1.0875(4) nm，c = 1.3542(5) nm，β=91.614(5)°，Z = 2，V = 2. 2178(14) nm~3，D_c = 1.498 g/cm~3，μ=1.351 mm~(-1)，F(000) = 1008，R_1 = 0.0401，wR_2 = 0.1148。在1和2的晶体中，锡原子呈五配位畸变三角双锥构型 。配合物1由未配位的甲醇分子通过氢键作用形成二维网状结构。

关键词: 锡络合物, 苯二甲酸, 哌嗪 P, 晶体结构

Binuclear organotin (IV) complexes [Ph_3Sn(CH_3OH)O_2CC_6H_4CO_2 (CH_3OH)-SnPh_3]·2CH_3OH and [Ph_3SnS_2CN(CH_2CH_2)_2NCS_2SnPh_3]· 2CH_3OH (2) were synthesized by the reaction of Ph_3SnCl with terephthalate of piperazinylbisdithiocarbamate in 2: 1 molar ratio in methanol solution. their structure were characterized by elementary analysis, IR and ~1H NMR and the crystal structures were determined by X-ray single crystal diffraction. The crystal 1 belongs to monoclinic with space group P2_1/n, a = 1.5199(5) nm, b = 0.9000(3) nm, c = 1. 8206(6) nm, β=113.970(5)°, Z = 2, Z = 2, V = 2.2755(13) nm~3, D_c = 1. 413 g/cm~3, μ=1.146 mm~(-1), F(000) = 980, R_1 = 0.0353, wR_2 = 0.0606. The crystal 2 belongs to monoclinic with space group P2_1/c, a = 1. 5066(5) nm, b = 1.0875(4) nm, c = 1.3542(5) nm, β=91.614(5)°,Z = 2, V = 2.2178(14) nm~3, D_c = 1.498 g/cm~3, μ=1.351 mm~(-1), F(000) = 1008, R_1 = 0.0401, wR_2 = 0.1148. In the crystals of complexes 1 and 2, the tin atoms rendered five-coordinate in a distorted trigonal bipyramidal configurations. The complex 1 is formed 2-D network structure by packing along the a-axis through hydrogen bonding.

Key words: TIN COMPLEX, BENZENEDICARBOXYLIC ACID, PIPERAZINE P, CRYSTAL STRUCTURE

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