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作 者:岳爽[1,2] 李俊[2] 臧树良[3] 谷学军[2] 于英杰[3] 金浩[2]
机构地区:[1]华东师范大学化学系,上海200062 [2]辽宁大学稀散元素化学研究所,沈阳110036 [3]辽宁石油化工大学化学与材料科学学院,抚顺113001
出 处:《无机化学学报》2010年第5期763-768,共6页Chinese Journal of Inorganic Chemistry
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=1.3295(3)nm,b=0.70115(16)nm,c=1.6164(4)nm,V=1.5068(6)nm3,Z=4,F(000)=744,R1=0.0295,wR2=0.0651。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=0.71303(18)nm,b=1.7153(4)nm,c=1.3503(4)nm,β=91.891(5)°,V=1.6507(7)nm3,Z=4,F(000)=808,R1=0.0443,wR2=0.0988。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=0.6986(2)nm,b=1.0449(4)nm,c=1.1369(3)nm,α=78.58(3)°,β=81.06(2)°,γ=87.87(3)°,V=0.8036(5)nm3,Z=2,F(000)=402,R1=0.0515,wR2=0.1244。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。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=0.1244. And Intermolecular hydrogen bands link the molecules of the complex into two-dimensional network structure.
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