Two new complexes[Co2(L)(4,4'-bip)(H2O)3]n(1)and{[Co(L')2(phen)]·2H2O)}n(2)(H4L =1-(3,5-dicarboxybenzyl)-3,5-pyrazole dicarboxylic acid,H3L'= 1-(3,5-dicarboxybenzyl)-3-pyrazole carboxylic acid,4,4'-bip = 4,4'-bis(1-imidazolyl)biphenyl,phen = 1,10-phenanthroline)were synthesized.Complexes 1 and 2 have been characterized by IR spectrography,X-ray single-crystal diffraction,elemental analysis and thermogravimetry.1 crystallizes in monoclinic system,space group P21/c.Complex 2 crystallizes in monoclinic system,space group I2/a.It is remarkable that in situ hydrothermal decarboxylation was observed during preparing complex 2.In addition,magnetic analysis indicates that antiferromagnetic interaction exists among Co(Ⅱ)ions in complexes 1 and 2.