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3-三氯化锡基丙烯酸乙酯与水杨醛缩m-溴-苯胺席夫碱配合物的室温固相合成及晶体结构

Solid-state Synthesis and Structure of 3-Ethoxycarbonylethyltin Trichloride with N-Saliyldene-4-Br-aniline Schiff Base

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【作者】 李忠芳王素文王捷王宇新王亚权

【Author】 LI Zhong-Fanga, b WANG Su-Wenb WANG Jieb WANG Yu-Xina WANG Ya-Quanc a (School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China) b (Shandong University of Technology, Zibo 255049, China) c (State Key Laboratory of C1 Chemistry and Chemical Engineering, Tianjin University, Tianjin 300072, China)

【机构】 天津大学化工学院化学工程国家重点实验室,山东理工大学化学工程学院,山东理工大学化学工程学院,天津大学化工学院化学工程国家重点实验室,天津大学碳一化学化工国家重点实验室 天津300072山东理工大学化学工程学院,淄博255049,淄博255049,淄博255049,天津300072,天津300072

【摘要】 用室温固相合成法研究了酯基锡EtO2CCH2CH2SnCl3 1 与Schiff碱2-HOC6H4- CH=NC6H4Br-3 2 合成标题化合物(3-EtO2CCH2CH2SnCl3)?2-HOC6H4CH= N-C6H4Br-3) 3的配位反应。利用元素分析, UV-VIS, IR, 1H NMR等方法对配合物的结构进行了表征, 采用单晶X-射线衍射方法测定了3的晶体结构。3的分子式为C18H19BrCl3NO3Sn, Mr = 602.29。晶体属三斜晶系, P空间群, a = 7.75(2), b = 10.578(2), c = 13.936(3) , = 83.663(3), = 75.909(3), = 76.691(3), V = 1077(4) 3, Z=2, Dc = 1.858 g/cm3, F(000) = 588, = 3.433 mm-1, R = 0.0547, wR = 0.1341。Schiff碱是以酚羟基上的O原子与中心Sn原子配位, Schiff碱分子中的分子内氢键, 形成配合物后得到加强, 提出了3的2种共振式。与中心Sn原子配位的3个Cl原子、2个O原子和1个C原子形成畸变的八面体结构。

【Abstract】 The title compound (3-EtO2CCH2CH2SnCl3)(2-HOC6H4CH=NC6H4Br-3) 3 was synthesized by solid- state reaction of 3-EtO2CCH2CH2SnCl3 1 with 2-HOC6H4CH=NC6H4Br-3 2 Schiff base at room temperature. It was characterized by m.p., UV-VIS, IR, 1H NMR and elemental analyses. Its crystal structure was determined by X-ray diffraction analysis with C18H19BrCl3NO3Sn, Mr = 602.29, triclinic, P, a = 7.750(16), b = 10.578(2), c = 13.936(3) , = 83.663(3). = 75.909(3), ?= 76.691(3), V = 1077(4) 3, Z = 2, Dc = 1.858 g/cm3, F(000) = 588, = 3.433 mm-1, R = 0.0547 and wR = 0.1341 for 4122 observed reflections (I>2s(I)). The phenolic O atom of the Schiff base is coordinated to the central Sn atom, and the intramolecular hydrogen bonds in this Schiff base are reinforced when the complex forms. Two possible resonance formulas of 3 are suggested. The central Sn atom is coordinated by three Cl, one C and two O atoms, resulting in a distorted octahedron.

【基金】 国家973课题(No. G20000264); 国家自然科学基金(No. 29976033); 山东省科技攻关课题(No. 021130105); 山东理工大学科研基金资助
  • 【文献出处】 结构化学 ,Chinese Journal of Structural Chemistry , 编辑部邮箱 ,2003年06期
  • 【分类号】O641.4
  • 【被引频次】7
  • 【下载频次】159
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