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

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。

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

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.