甲基三氧化铼卤代席夫碱配合物的合成及晶体结构
Synthesis and Crystal Structures of Methyl Trioxide Rhenium Halogenated Schiff-Bases Complexes
作者单位
王春玲 河北工业大学化工学院天津 300130 
张月成 河北工业大学化工学院天津 300130 
丁春浦 河北工业大学化工学院天津 300130 
赵继全 河北工业大学化工学院天津 300130 
摘要: 利用4-氟苯胺、4-氯苯胺与2-吡啶甲醛缩合得到2个席夫碱(S1,S2),席夫碱与甲基三氧化铼(Ⅶ)反应生成相应的配合物(1,2)。利用核磁共振波谱、红外光谱、质谱、元素分析和X-射线单晶衍射方法对配合物进行了表征。X-射线单晶衍射分析表明,配合物1晶体属于三斜晶系,空间群P1,a=0.783 65(16) nm,b=0.844 97(17) nm,c=1.004 2(2) nm,β=76.62(3)°,V=0.635 0(2) nm3Mr=449.45,Z=2,Dc=2.351 g·cm-3F(000)=424,最终偏离因子R1=0.022 8,wR2=0.058 6。 配合物2晶体属于单斜晶系,空间群 P21/na=0.953 60(8) nm,b=1.410 70(17) nm,c=1.070 90(10) nm,β=108.188(6)°,V=1.368 6(2) nm3Mr=465.90,Z=4,Dc=2.261 g·cm-3F(000)=880,最终偏离因子R1=0.031 5,wR2=0.061 5。配合物12都具有不规则八面体构型。
关键词: 甲基三氧化铼(Ⅶ)配合物  卤代席夫碱  晶体结构
基金项目: 
Abstract: Two Schiff-bases were prepared by the condensation of 2-pyridinecarboxaldehyde with 4-fluoroaniline and 4-chloroaniline respectively. The two Schiff-bases as ligands coordinated with methyltrioxorhenium(Ⅶ) to afford the corresponding complexes (1, 2) smoothly. The complexes were characterized by NMR, IR, MS, elemental analysis and X-ray diffraction single crystal structure analysis. Crystal structure analysis showed that complex 1 belongs to triclinic, space group P1, a=0.783 65(16) nm, b=0.844 97(17) nm, c=1.004 2(2) nm, β=76.62(3)°, V=0.635 0(2) nm3, Mr=449.45, Z=2, Dc=2.351 g·cm-3, F(000)=424 and final R1=0.022 8,wR2=0.058 6, and complex 2 belongs to monoclinic, space group P21/n, a=0.953 60(8) nm, b=1.410 70(17) nm, c=1.070 90(10) nm, β=108.188(6)°, V=1.368 6(2) nm3, Mr=465.90, Z=4, Dc=2.261 g·cm-3, F(000)=880, and final R1=0.031 5, wR2=0.061 5. It was also showed that both complex 1 and 2 had distorted octahedral geometry. CCDC: 797928, 1; 797929, 2.
Keywords: methyltrioxorhenium(Ⅶ) complex  halogenated Schiff-base  crystal structure
 
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王春玲,张月成,丁春浦,赵继全.甲基三氧化铼卤代席夫碱配合物的合成及晶体结构[J].无机化学学报,2011,27(1):114-118.
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