镓的席夫碱配合物的合成及晶体结构
Schiff Base Complex of Gallium: Synthesis and Crystal Structure
作者单位
岳 爽 华东师范大学化学系上海 200062
辽宁大学稀散元素化学研究所沈阳 110036 
李 俊 辽宁大学稀散元素化学研究所沈阳 110036 
臧树良 辽宁石油化工大学化学与材料科学学院抚顺 113001 
谷学军 辽宁大学稀散元素化学研究所沈阳 110036 
于英杰 辽宁石油化工大学化学与材料科学学院抚顺 113001 
金 浩 辽宁大学稀散元素化学研究所沈阳 110036 
摘要: 在无水无氧条件下,合成了3个镓的席夫碱配合物GaCl3(C13H11NO) (1)、GaCl3(C14H13NO2)(2)和GaCl3(C13H9ClNO) (3),对它们进行了元素分析、核磁共振、红外光谱等表征,并用X射线衍射测定了配合物的单晶结构。各配合物配位方式均为配体中酚羟基氧原子与中心镓原子配位,在空间上形成畸变的四面体结构。配合物1属于正交晶系,Pnma空间群,晶胞参数:a=1.329 5(3) nm,b=0.701 15(16) nm,c=1.616 4(4) nm,V=1.506 8(6) nm3,Z=4,F(000)=744,R1=0.029 5,wR2=0.065 1。配合物依靠分子间的氢键作用进一步联结成二维网状结构。配合物2属于单斜晶系,P21/n空间群,晶胞参数:a=0.713 03(18) nm,b=1.715 3(4) nm,c=1.350 3(4) nm,β=91.891(5)°,V=1.650 7(7) nm3,Z=4,F(000)=808,R1=0.044 3,wR2=0.098 8。配合物依靠分子间的氢键作用进一步联结成二维网状结构。配合物3属于三斜晶系,P1 空间群,晶胞参数:a=0.698 6(2) nm,b=1.044 9(4) nm,c=1.136 9(3) nm,α=78.58(3)°,β=81.06(2)°,γ=87.87(3)°,V=0.803 6(5) nm3,Z=2,F(000)=402,R1=0.051 5,wR2=0.124 4。配合物依靠分子间的氢键作用进一步联结成二维网状结构。
关键词: 席夫碱  镓配合物  合成  晶体结构
基金项目: 
Abstract: The new Schiff base complexes of gallium GaCl3(C13H11NO) (1),GaCl3(C14H13NO2)(2) and GaCl3(C13H9ClNO) (3) were synthesized under argon atmosphere with the glove box and characterized by elemental analysis, 1H NMR, IR, and the crystal structures were determined by single-crystal X-ray diffraction. In these complexes, the Ga center is four-coordinate with distorted tetrahedron geometry. The complex 1 crystallizes in an orthorhombic system, the space group Pnma with a=1.329 5(3) nm, b=0.701 15(16) nm, c=1.616 4(4) nm, V=1.506 8(6) nm3, Z=4, F(000)=744,R1=0.029 5, wR2=0.065 1. And Intermolecular hydrogen bands link the molecules of the complex into two-dimensional network structure. The complex 2 crystallizes in a monoclinic system, the space group P21/n with a=0.713 03(18) nm, b=1.715 3(4) nm, c=1.350 3(4) nm, β=91.891(5)°, V=1.650 7(7) nm3, Z=4, F(000)=808, R1=0.044 3, wR2=0.098 8. And Intermolecular hydrogen bands link the molecules of the complex into two-dimensional network structure. The complex 3 crystallizes in a triclinic system, the space group P1 with a=0.698 6(2) nm, b=1.044 9(4) nm, c=1.136 9(3) nm, α=78.58(3)°, β=81.06(2)°, γ=87.87(3)°, V=0.803 6(5) nm3, Z=2, F(000)=402, R1=0.051 5, wR2=0.124 4. And Intermolecular hydrogen bands link the molecules of the complex into two-dimensional network structure. CCDC: 649105, 1; 649104, 2; 763895, 3.
Keywords: Schiff base  gallium complex  synthesis  crystal structure
 
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岳 爽,李 俊,臧树良,谷学军,于英杰,金 浩.镓的席夫碱配合物的合成及晶体结构[J].无机化学学报,2010,26(5):763-768.
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