A new cobalt complex [Co (L)3 ] (1 ),HL=2,4-dichloro-6-methylimino-methyl-phenol,was syn-thesized by solvothermal method from 3,5-dichloro-2-hydroxybenzaldehyde,methylamine and Co (NO3 )2 · 6H2 O.The structure was characterized by elemental analysis,IR and X-ray single crystal diffraction.Complex 1 belongs to the monoclinic system,space group P21/n,with a=1.427 9(2)nm,b=1.993 3(3)nm,c=1.960 6 (3)nm;β=101.338(13)°,V=5.471 6(13)nm3,Z=8,Dc =1.622 g·cm-3,R1 =0.076,wR2 =0.168,S=1.05 .Each CoⅢatom is six coordinated by three N and three O from three bidentate ligands HL to give a slightly distorted octahedral geometry.Molecules are extended to 3D framework through the Cl…Cl and C—H…Cl hydro-gen bonds.%以3，5-二氯水杨醛、甲胺、六水合硝酸钴为原料，采用溶剂热法在无水乙醇溶液中合成了一个新的单核钴（III）配合物[Co（L）3]（1），HL＝3，5-二溴水杨醛缩甲胺希夫碱，其结构经元素分析、IR和单晶X射线衍射表征。配合物1属于单斜晶系，P21／n空间群，晶胞参数a＝1.4279（2）nm，b＝1.9933（3）nm，c＝1.9606（3）nm，β＝101.338（13）°，V＝5.4716（13）nm3，Z＝8，Dc ＝1.622 g·cm－3，R1＝0.076，wR2＝0.168，S＝1.05。配合物1中Co（Ⅲ）分别与3个二齿配体上的3个O原子和3个N原子配位，形成轻度扭曲的八面体构型。分子间通过Cl…Cl和C—H…Cl弱作用相互连接成为三维网络结构。
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