Two new coordination polymers, [Cd(bct)(H2O)]<bold></bold>(H2O) (1) and [Zn(bct)(bip)]<bold>2</bold>(H2O) (2) (H(2)bct=3,5-bis(4-carboxy-phenyl)-1,2,4-triazole, bip=1,4-bis(imidazol-1-ylmethyl)benzene), have been synthesized. Their structures have been determined by single-crystal X-ray diffraction analysis and further characterized by elemental analysis, IR spectroscopy, and thermogravimetric analysis. Compound 1 is a two-dimensional structure with double-layered network, where bct ligands adopt a (4)-k(1),k(1),k(1),k(1) bridging mode linking four five-coordinate Cd ions. Compound 2 exhibits a three-dimensional framework consisting of double-layered helical chains with the bct and bip adopting (3)-k(1),k(1),k(1) and (2)-k(1),k(1) bridging mode, respectively. Complexes 1 and 2 exhibit intense emissions at 399 and 441nm, respectively.