Abstract: Using pyrazole-3-carboxylic acid as the main ligand, two complexes Ag₃(3-PCA)₃ Ag(DMAP)_{2 3}·10H₂O (1) andCu₂(3-PCA)₂(DMAP)₄·2H₂O (2) (3-PCA=pyrazole-3-carboxylic acid, DMAP=4-Dimethylaminopyridine) were synthesized by solvothermal reaction. Their crystal structures were determined by using x-ray single crystal diffractometer, and characterized by IR spectroscopy. The results show that complex (1) belongs to monoclinic, the space group Pc, a=0.9409(8) nm, b=1.3411(8) nm, c=2.8699(2) nm, Z=2, V=3.621 5(5) nm³, and complex (2) belongs to the triclinic system, space group Pī, a=0.8999(14) nm, b=1.0870(18) nm, c=1.1050(17) nm, α=78.426(14) °, β=68.732(15) °, γ=87.237(13) °, Z=1, V=0.9865(3) nm³. The solid-state fluorescence test of the complex (1) confirmed its fluorescence properties; The interaction of complex (2) with BSA was studied.