新型含硫化合物的合成及其晶体结构研究

Abstract

[中文文摘]通过简单的一步亲核取代反应合成了一新型含硫化合物(4-羧基甲硫醇基-2,3,5,6-四氯-苯硫醇基)乙酸(1),产物经乙酸乙酯重结晶分离纯化,并在适当的条件下培养得到单晶,测定了该化合物的晶体结构,以及其DMSO加合物的晶体结构.其中该化合物晶体属于单斜晶系,空间群为P21/c,a=0.508 93(4)nm,b=0.969 81(7)nm,c=1.439 1(1)nm,β=91.036(4)°,V=0.710 20(9)nm3,Z=2,Dc=1.843 g/cm3,F(000)=392,μ=1.133,R1[I>2σ(I)]=0.097 3,wR2[I>2σ(I)]=0.193 1.其DMSO加合物的晶体结构属于正交晶系,空间群为Pnma,a=1.372 48(2)nm,b=2.883 6(4)nm,c=0.461 48(6)nm,V=1.826 4(4)nm3,Z=4,Dc=1.703 g/cm3,F(000)=936,μ=1.010,R1[I>2σ(I)]=0.088 8,wR2[I>2σ(I)]=0.203 9.晶体结构分析表明,分子间氢键是这一化合物的一大特点.[英文文摘]A new compound containing sulfur atoms(4-carboxymethylsulfanyl-2,3,5,6-tetrachloro-phenylsulfanyl)-acetic acid(1) was synthesized via a simple one-pot nucleophilic substitution reaction.The product was separated and purified by recrystallization from acetic acid ethyl ester.Crystals suitable for crystallography and its DMSO complexes were obtained with slow evaporation of appropriate solvent.The crystal structure of the title compound belongs to monoclinic system with space group P21/c,a=0.508 93(4) nm,b= 0.969 81(7) nm,c= 1.439 1(1)nm,β=91.036(4)0,V=0.710 20 (9)nm3,Z=2,Dc=1.843 g/cm3, F(000)=392,μ= 1.133,R1[I>2σ(I)]=0.097 3,wR2[I>2σ(I)]= 0.193 1.The crystal of its DMSO complex belongs to orthorhombic system with space group Pnma,a=1.372 48(2)nm,b=2.883 6(4)nm,c= 0.461 48(6)nm,V= 1.826 4(4)nm3,Z= 4,Dc= 1.703 g/cm3,F(000)=936,μ= 1.010,R1[I>2σ (I)]=0.088 8,wR2[I>2σ(I)]=0.203 9.The crystal structure analysis shows that this compound exhibits intermolecular hydrogen bonds.