2[NiL2(H2O)2]?DMF(L=quinoline-2-carboxylic acid radical, DMF=N,N-dimethylformamide) was synthesized by hydrothermal method using quinoline-2-carboxylic acid and nickel sulfate as raw material. Its structure and property was analysized and characterized by X-ray, PXRD, EA, IR, TG and Fl. The title complex is orthorhombic system, and belong to space group Pna21； with a=2.06753(6) nm， b=0.82571(3) nm，c=2.34776(7) nm， V=4.0081(2) nm3， Z=4， Mr=951.210， Dc=1.576 g/cm3。The title complex is a mononuclear complex, which is expanded into a three-dimensional supramolecular structure by intermolecular hydrogen bonding and π-π stacking. Fluorescence spectrum analysis show that both the ligand and the title complex have good fluorescence properties, and the fluorescence properties of the title complex are better than that of the ligand.