Abstract: Two complexes of pyrazole-3-carboxylic acid, Ag (Py-3-CA)_n (1) andPb₂ (Py-3-CA)_4n (2)(Py-3-CA=pyrazole-3-carboxylic acid), were synthesized by hydrothermal method. The complexes were characterized by IR spectroscopy, elemental, fluorescence, X-ray powder diffraction and single-crystal X-ray diffraction analyses. The results showed that the complex 1 belongs to monoclinic crystal,P2₁/c space group, unit cell parameter a=0.859 97(4) nm,b=0.576 70(2) nm,c=1.012 87(4) nm,β=97.673(4)°,V=0.49783(4) nm³,Z=4,and the complex 2 belongs to monoclinic crystal,P2₁/c space group, unit cell parameter a=1.107 64(3) nm,b=2.366 60(6) nm,c=0.863 20(2) nm,β=110.313(3)°,V=2.122 02(10) nm³,Z=4. The complexes were linked to three-dimensional structures by the hydrogen bonds. The results of fluorescence measurements showed that complex 1 and 2 had fluorescent properties.