In our group, the organic compounds 2, 5-dibromoterephthalic acid (H2L1) and 2, 2′-bipyridine (L2) were used as biligands to react with zinc sulfate heptahydrate (ZnSO4·7H2O) and cobalt nitrate hexahydrate (Co(NO3)2·6H2O), respectively, using solvothermal method to obtain a zinc complex ［Zn(L1)(L2)(H2O)］n (1) and a cobalt complex ［Co(L1)(L2)(H2O)］n (2). The structural characterization and properties measurement were performed by single crystal X-ray diffraction, elemental analysis, infrared spectroscopy, ultraviolet spectroscopy, fluorescence spectroscopy, thermogravimetric analysis and other tests. The results show that complex 1 is a monoclinic crystal system with one-dimensional chain structure formed by the coordination of Zn2+ linking L2-1 and L2, each chain forming a three-dimensional network structure by regular stacking under intermolecular hydrogen bonding and π…π conjugation. Complex 2 is a triclinic crystal system with Co1 and Co1i ions linked by carboxylic acid oxygen atoms O4 and O4i on H2L1 to form a bidentate chelated ligand structural unit. A two-dimensional lattice structure is formed with Co2+ ligands connecting L2-1 and L2, and the layers are regularly stacked under O-H…O intermolecular hydrogen bonding and van der Waals forces to form a three-dimensional network structure. Both complexes 1 and 2 contain aromatic heterocycles, carboxyl heterocycles and nitrogen heterocycles, they have good fluorescence property and thermal stability, the maximum emission wavelengths of complex 1 and complex 2 are 345 nm and 333 nm, respectively.