高等学校化学学报

高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (7): 1231.

• 研究论文 • 上一篇    下一篇

[2-(2-羟基苯基)亚氨甲基苯硫酚根(2-)-N,O,S](2-甲氧羰基乙基-C,O)氯化锡的合成及性质

田来进1,2, 周正宇1,2,3   

  1. 1. 曲阜师范大学化学系, 曲阜 273165;
    2. 浙江大学化学系, 杭州 310027;
    3. 山东大学晶体材料国家重点实验室, 济南 250100
  • 收稿日期:2001-08-29 出版日期:2002-07-24 发布日期:2002-07-24
  • 通讯作者: 周正宇(1941年出生),男,教授,博士生导师,从事量子化学和功能配合物化学研究.E-mail:zhengyu@qfnu.edu.cn E-mail:zhengyu@qfnu.edu.cn
  • 基金资助:

    国家自然科学基金(批准号:20075016);晶体材料国家重点实验室开放基金;曲阜师范大学科研基金资助

Synthesis and Properties of [2-(2-Hydroxyphenyl)iminomethyl- [JZ]benzenethiolato(2-)-N,O,S](2-methoxy-(2-methoxy-carbonylethyl-C,O)tin Chloride

TIAN Lai-Jin1,2, ZHOU Zheng-Yu1,2,3   

  1. 1. Department of Chemistry, Qufu Normal University, Qufu 273165, China;
    2. Department of Chemistry, Zhejiang University, Hangzhou 310027, China;
    3. The State Key Laboratory of Crystal Materials, Shandong University, Jinan 250100, China
  • Received:2001-08-29 Online:2002-07-24 Published:2002-07-24

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摘要： 利用2-甲氧羰基乙基三氯化锡与硫代水杨醛缩邻氨基苯酚(H2L)进行反应合成了标题配合物[2-(2-羟基苯基)亚氨甲基苯硫酚根(2-)-N,O,S](2-甲氧羰基乙基-C,O)氯化锡CH3OCOCH2CH2SnClL(L=2-SC6H4CHNC6H4O-2),该配合物与二甲基亚砜(DMSO)、六甲基磷酰胺(HMPA)等单齿配体反应生成混配配合物CH3OCOCH2CH2SnClLL′(L′=DMSO,HMPA),与醇(ROH)反应生成相应的2-烷氧羰基乙基锡配合物ROCOCH2CH2SnClL.通过元素分析、红外光谱、核磁共振谱等对配合物的结构进行了表征.用X射线单晶衍射测定了标题配合物的晶体结构,晶体属三斜晶系,P1空间群,Z=2,晶胞参数a=0.8704(2)nm,b=0.9393(3)nm,c=1.4511(3)nm,α=98.05(3)°,β=103.03(3)°,γ=96.99(3)°.该配合物具有分子内羰基氧原子和配体L的硫、氮、氧原子对锡原子配位的畸变八面体结构.

关键词: 锡()配合物, 硫代水杨醛缩邻氨基苯酚, 2-甲氧羰基乙基三氯化锡, 晶体结构

Abstract: The title complex, [2-(2-hydroxyphenyl)iminomethyl benzenethiolato(2-)-N, O, S] (2-methoxycarbonylethyl-C, O) tin chloride, CH3OCOCH2CH2SnClL(L=2-SC6H4CHN=C6H4O2), was synthesized by the reaction of 2 methoxycarbonylethyltin trichloride with N (2 hydroxy phenyl)thiosalicylideneimine. This complex reacted with neutral monodentate ligands such as dimethylsulfoxide(DMSO) and hexamethylphosphoramide(HMPA) to form the mixed ligand complexes, CH3OCOCH2CH2SnClLL′(L′=DMSO, HMPA), and also readily underwent transesterification with alcohols to produce the corresponding2alkoxycarbonylethyltin analogues, ROCOCH2CH2SnClL. These complexes were characterized by means of elemental analysis, IRand 1H NMRspectra. The crystal structure for the title complex was determined by X-ray diffraction analysis. The crystal belongs to triclinic system, space group P1with cell parameters α=0.8704(2) nm, b=0.9393(3) nm, c=1.4511(3) nm, α=98.05(3)°, β=103.03(3)°, γ=6.99(3)°, V=1.1299(4) nm3, Z=2, Dc=1.378 g/cm3, F (000)=524. In this compound, the tin atom adopts a distorted octahedral geometry via intramolecular carbonyl oxygen atom and the sulfur, nitrogen and oxygen atoms of the chelating ligand Lto tin coordination.

Key words: Tin(Ⅳ) complex, N (2 Hydroxyphenyl)thiosalicylideneimine, 2 Methoxycarbonylethyltin trichloride, Crystal structure

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