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

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［ＳｎＣＩ３｛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）Ａ，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。

The six new tin (Ⅳ) complexes of containing 2 - methoxycarbonylpropyl, [ SnCl3 { CH2 CH (CH3 ) CO2CH3} L1n] (n = 1, 2) and [SnCI3 -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, [SnCI3 {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) A, 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.