【摘要】 合成了水杨醛-3,4,5-三甲氧基苯甲酰腙(1)、5-溴-水杨醛-3,4,5-三甲氧基苯甲酰腙(2)和4-氯苯甲醛-3,4,5-三甲氧基苯甲酰腙(3),通过FT-IR、1HNMR等进行了结构表征。用X射线单晶衍射测定了3个化合物的晶体结构。结果表明化合物1和2都属于斜方晶系,P2(1)/c空间群,化合物3属于三斜晶系,P-1空间群,晶体通过分子间氢键作用形成一维的无限链状结构。它们的晶体学参数分别为:1.a=1.5348(12)nm,b=1.3330(11)nm,c=0.8299(7)nm,α=90.00°,β=99.854(16)°,γ=90.00°,V=1.6730(2)nm3,Z=4,Dc=1.312g/cm3,F(000)=696,R=0.1016,wR=0.1936;2.a=1.14157(19)nm,b=1.6279(3)nm,c=0.9738(16)nm,α=90.00°,β=100.210(16)°,γ=90.00°,V=1.7144(4)nm3,Z=4,Dc=1.586g/cm3,F(000)=832,R=0.0669,wR=0.0969;3.a=0.5119(2)nm,b=0.8210(4)nm,c=2.0276(9)nm,α=101.055(7)°,β=92.362(7)°,γ=101.459(7)°,V=0.8169(7)nm3,Z=2,Dc=1.418g/cm3,F(000)=364,R=0.0516,wR=0.1276。更多还原

【Abstract】 Three titled compounds namely(E)-N’-(2-hydroxybenzylidene)-3,4,5-trimethoxybenzohydrazide(1),(E)-N’-(5-bromo-2-hydroxybenzylidene)-3,4,5-trimethoxybenzohydrazide(2) and(E)-N’-(4-cholobenzylidene)-3,4,5-trimethoxybenzohydrazide(3) have been synthesized,and characterized by IR and 1H NMR.Their crystalline and molecular structures have been determined by single crystal X-ray diffraction.Both compounds 1 and 2 belong to monoclinic system,space group P2(1)/c,with a=1.534 8(12)nm,b=1.333 0(11)nm,c=0.829 9(7)nm,α=90.00°,β=99.854(16)°,γ=90.00°,V=1.673 0(2)nm3,Z=4,Dc=1.312 g/cm3,F(000)=696,R=0.101 6,wR=0.193 6,for compound 1;a=1.141 57(19)nm,b=1.627 9(3)nm,c=0.973 8(16)nm,α=90.00°,β=100.210(16)°,γ=90.00°,V=1.714 4(4)nm3,Z=4,Dc=1.586 g/cm3,F(000)=832,R=0.066 9,wR=0.096 9 for compound 2.Compound 3 belongs to triclinic system,space group P-1,with a=0.511 9(2)nm,b=0.821 0(4)nm,c=2.027 6(9)nm,α=101.055(7)°,β=92.362(7)°,γ=101.459(7)°,V=0.816 9(7)nm3,Z=2,Dc=1.418 g/cm3,F(000)=364,R=0.051 6,wR=0.127 6.In the crystals there exist several intermolecular hydrogen bonds,through which one-dimensional infinite-chain structures were formed.更多还原