甲基三氧化铼卤代席夫碱配合物的合成及晶体结构

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髪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=0.78365(16)nm,b=0.84497(17)nm,c=1.0042(2)nm,β=76.62(3)°,V=0.6350(2)nm3,Mr=449.45,Z=2,Dc=2.351 g.cm-3,F(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/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,最终偏离因子R1=0.031 5,wR2=0.061 5。配合物1和2都具有不规则八面体构型。

Synthesis and Crystal Structures of Methyl Trioxide Rhenium Halogenated Schiff-Bases Complexes

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(Ⅳ) 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.