2-甲酯基丙基合锡(Ⅳ)配合物的固相合成 |
Synthesis of the Tin (Ⅳ) Complexes of 2-Methoxycarbonylpropyl in Solid State |
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摘要: 利用2-甲酯基丙基三氯化锡与六甲基磷酰三胺(L1)、苯甲醛缩邻氨基苯酚(HL2)及2-甲基-8-羟基喹啉(HL3)的低热固相反应合成了六个新的含2-甲酯基丙基的锡(Ⅳ)配合物[SnCl3{CH2CH(CH3)CO2CH3}L1n](n=1,2)和[SnCl3-n{CH2CH(CH3)CO2CH3}Ln](n=1,2;L=L2,L3),通过元素分析、红外光谱、核磁共振对其结构进行了表征。用X-射线单晶衍射测定了[SnCl3{CH2CH(CH3)CO2CH3}L1]的晶体结构,晶体属于单斜晶系,空间群p21/n,a=8.0173(12),b=25.867(2),c=10.4353(9)Å,β=102.725(7)°,Z=1.该配合物为含有L1的氧原子和分子内羰基氧原子配位的畸变八面体结构。 |
关键词: 锡(Ⅳ)配合物 固相反应 2-甲酯基丙基三氯化锡 晶体结构 |
基金项目: 晶体材料国家重点实验室开放基金;山东省自然科学基金资助项目(No.Q97B03123). |
Abstract: The six new tin (Ⅳ) complexes of containing 2-methoxycarbonylpropyl, [SnCl3{CH2CH(CH3) CO2CH3}L1n] (n = 1, 2) and [SnCl3-n{CH2CH(CH3)CO2CH3} Ln] (n = 1, 2; L = L2, L3), were synthesized by reaction of 2-methoxycarbonylpropyltin trichloride with hexamethylphosphoramide (L1), 2-phenylmethyleneiminophenol (HL2) and 2-methyl-8-hydroxyquinoline (HL3) in solid state at low-heating temperature and characterized by means of elemental analysis, IR, 1H NMR spectra.The crystal structure of the complex, [SnCl3{CH2CH(CH3)CO2CH3}L1], was determined by X-ray single crystal diffraction.The crystal belongs to monoclinic with space group P21/n, a = 8.0173 (12), b = 25.867(2), c = 10.4353(9)Å, 102.725(7), Z = 1.The tin atom in this structure is in a distorted octahedral coordination environment with the oxygen atoms of L1 and intramolecular carbonyl. |
Keywords: tin (Ⅳ) complex solid state reaction 2-methoxycarbonylpropyltin trichloride crystal structure |
投稿时间:2000-02-08 修订日期:2000-04-24 |
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田来进,丁养军,赵斌,周正宇.2-甲酯基丙基合锡(Ⅳ)配合物的固相合成[J].无机化学学报,2000,16(5):783-787. |
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