摘要
在不加任何碱的条件下,三[2-(亚水杨基胺)乙基]胺与苦味酸锌[Zn(Pic)2 6H2O]在乙醇中反应,得到了较为少见的多胺单缩合西夫碱配体的配合物[ZnN(CH2CH2NH2)2(CH2CH2N=CH-C6H4O)] Pic。化学式为C19H23N7O8Zn,Mr=542.81,晶体属三斜晶系,空间群为P,晶胞参数为a=0.7494(3),b=1.1917(5),c=1.3142(6)nm,a=78.111(7),b=79.093(7),g=78.577(7),V=1.1121(8)nm3,Dc=1.621g/cm3,m(MoKa)=1.167mm-1,Z=2,F(000)=560,在1.60<q<25.03悍段谝陨璺绞绞盏蕉懒⒀苌涞?631个,其中I>2s(I)的可观测点为2433个,最终偏离因子R=0.0555,wR=0.1139。配合物中Zn(II)与配体的4个N原子和1个O原子配位形成变形的三角双锥结构,桥头N和O为锥顶,4个配位N中桥头N与金属离子的配位作用最弱。晶体通过p-p堆积和分子内、分子间的氢键作用形成二维层状超分子结构。
A relatively rare complex [ZnN(CH2CH2NH2)2(CH2CH2N=CHC6H4O)]Pic (C19H23N7O8Zn, Mr = 542.81) was prepared by the reaction of tris(2-(salicylideneimino)ethyl) amine with zinc picrate [Zn(Pic)2] in ethanol. Without any base, the C=N of ligand was partially decomposed by the picric acid which was formed from the picric anion and phenol proton. The crystal structure was determined by single-crystal X-ray diffraction analy- sis: triclinic, space group P, a = 0.7494(3), b = 1.1917(5), c = 1.3142(6) nm, a = 78.111(7), b = 79.093(7), g = 78.577(7), V = 1.1121(8) nm3, Dc = 1.621 g/cm3, m(MoKa) = 1.167 mm-1, Z = 2, F(000) = 560, R = 0.0557 and wR = 0.1167. The ligand is coordinated to Zn(II) via four N and one O atoms, and the coordination geometry can be described as a distorted trigonal bipyramid, with the O and bridgehead N atoms lying on the top of the pyramid to form the weak ZnN bond. In the crystal, the complex molecules are assembled to form a two-dimensional layer structure via p-p stacking, intra- and intermolecular hydrogen-bonds.
基金
兰州大学留校博士启动基金资助
