在室温条件下合成了2个配合物[Ni(DBTA)(DMF)(H2O)4](1)和[Co(DBTA)(DMF)(H2O)4](2)(D-H2DBTA=D-(+)-二苯甲酰酒石酸,DMF=N,N-二甲基甲酰胺),并通过元素分析、FT-IR光谱、X射线单晶及粉末衍射表征了2个配合物的结构.X射线单晶衍射结果表明,2个配合物同构,属于单斜晶系,P21空间群.配合物由配位键形成零维结构,再通过分子间氢键形成三维网状结构.荧光分析表明当激发波长为280 nm时,配合物1和2具有较强的荧光.尽管2个配合物同构,但表现出不同的磁性质:配合物1主要表现出Ni2+离子间弱的反铁磁相互作用,而配合物2则表现为Co2+离子的磁各向异性以及Co2+离子间强的反铁磁相互作用.“,”Two coordination compounds [Ni(DBTA)(DMF)(H2O)4] (1) and [Co(DBTA)(DMF)(H2O)4] (2) (D-H2DBTA=(+)-2,3-dibenzoyl-D-tartaric acid, DMF=N,N-dimethylformamide) have been synthesized at room temperature, and characterized by elemental analyses (EA), FT-IR, X-ray single-crystal and powder diffraction analyses. The structural analysis shows that complexes 1 and 2 are isomorphic. They belong to the monoclinic system with P21 space group and display a zero-dimensional structure constructed from coordination bonds, which is further interlinked to form a three-dimensional network via hydrogen-bonding interactions. Fluorescence measurements indicate that 1 and 2 can exhibit strong fluorescence using 280 nm as the excitation wavelength. Though 1 and 2 are isomorphic, they dis-played different magnetic properties. Complex 1 dominates weak antiferromagnetic couplings between Ni2+cations, while complex 2 exhibits the magnetic anisotropy of the Co2+center and antiferromagnetic interactions between the Co2+cations. CCDC:2072164, 1;2065592, 2.