高等学校化学学报

高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (2): 238.

• 研究论文 • 上一篇    下一篇

β-三氯化锡基丙烯酸甲酯与Schiff碱配合物分解反应及产物结构表征

李忠芳1,2, 王素文1, 王宇新2, 傅芳信3   

  1. 1. 山东理工大学科技研究学院, 淄博 255012;
    2. 天津大学化工学院, 天津 300072;
    3. 东北师范大学化学系, 长春 130024
  • 收稿日期:2000-11-17 出版日期:2002-02-24 发布日期:2002-02-24
  • 通讯作者: 李忠芳(1962年出生),男,博士研究生,教授,主要从事金属有机化学及燃料电池研究.E-mail:Lizhf@eyou.com E-mail:Lizhf@eyou.com
  • 基金资助:

    国家自然科学基金(批准号:29170084);山东省科委基金(批准号:983000001)资助

Decomposition of Complex of Estertin with Schiff Base and Characterization of Crystal Structure of Products

LI Zhong-Fang1,2, WANG Su-Wen1, WANG Yu-Xin2, FU Fang-Xin3   

  1. 1. Research Center of Scienceand Technology, Shandong University of Scienceand Engineering, Zibo 255012, China;
    2. School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China;
    3. Department of Chemistry, Northeast Normal University, Changchun 130024, China
  • Received:2000-11-17 Online:2002-02-24 Published:2002-02-24

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摘要： 将酯基锡MeO2CCH2CH2SnCl3(1)与Schiff碱(2-HOC6H4CH＝NC6H5)(2)反应合成配合物MeO2CCH2CH2SnCl3·(2-HOC6H4CH＝NC6H5)(3),在其反应混合液放置过程中发生分解生成酯基锡与无机氯离子形成的配合物MeO2CCH2CH2SnCl4-·H+(4)和酯基锡与Schiff碱的酚氧负离子取代生成的配合物MeO2CCH2CH2SnCl2·(2-OC6H4CH＝NC6H5)(5).用元素分析、IR及NMR对配合物3,4,5进行了表征,并对配合物4的晶体结构进行了解析.配合物4为正交晶系,空间群P2cn,a=0.7852(2)nm,b=1.2236(10)nm,c=1.6952(4)nm,α=β=γ=90°,V=1.6287nm3,Z=4,Dc=1.79g/cm3,F(000)=860,μ=22.2cm-1(Mo),R=0.0449,ωR=0.0382.配合物4的空间构型为畸变的八面体构型,中心锡原子的配位数为6.配合物5为Schiff碱中的酚氧负离子取代配合物1中的一个氯离子形成的配合物,锡原子的配位数为5.

关键词: 酯基锡, Schiff碱, 配合物, 分解, 晶体结构

Abstract: Complex MeO2CCH2CH2SnCl4-·H+(4) and MeO2CCH2CH2SnCl2·(2-OC6H4-CH＝NC6H5)(5) were obtained by decomposing the yellow reaction solution of MeO2CCH2CH2SnCl3· (2-HOC6H4CH＝NC6H5) (3), which is the product of β-methoxycarbonylethyltin trichlorides(1) with Schiff base (2-HOC6H4CH＝NC6H5)(2), after standing for 15 d. Complexes 4 & 5 were characterized by elemental analysis, IR　and NMR. The crystal structure of complex 4 was determined by X-ray diffraction analysis. The crystal belongs to orthorhombic system, space group P2cn, a =0.7852(2) nm, b = 1.2236(10) nm , c =1.6952(4) nm, α= β =γ =90°, V = 1.6287 nm3, Z =4, Dc =1.79 g/cm3, F (000) = 860, μ =22.2 cm-1 , R=0.0449, wR =0.0382 . Complex 4 exists as a discrete molecule, and the tin atom attains a distorted octahedral geometry via the coordination of intramolecular carbonyl oxygen and chloride ion. The coordination number of tin atom is 6. In complex 5, one chloride ion is replaced by the phenolic oxygen anion. Coordination of carbonyl oxygen atom to tin atom still exists, The coordination number of tin atom is 5.

Key words: Estertin, Schiff base, Complexes, Decompose, Crystal structure

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