Zn 3 (tda) 2 (bipy) 2 (H 2 O) 2 Á 4H 2 O] n (1) and [Co 2 (Htda) 2 (H 2 O) 6 Á5H 2 O] (2) have been synthesized and characterized structurally by X-ray diffraction, where H 3 tda ¼ 1H-1,2,3-triazole-4, 5-dicarboxylic acid and 2,2 0 -bipy ¼ 2,2 0 -bipyridine. Their solid-state structures have been characterized by elemental analysis and IR spectroscopy. The molecular unit of 1 consists of two crystallographically unique Zn(II) ions assuming different coordination geometries, the tda 3À exhibits a hexadentate binding mode chelating three Zn(II) ions; neighboring Zn-Zn distances through tda 3À bridges are 5.910(6), 5.888(5), and 6.279(3) Å , respectively. In 2, two neighboring Co(II) ions are bridged by two Htda 2À ligands, forming a binuclear structure, with Co-Co distance of 4.091 Å and is further linked to generate a 3-D structure via hydrogen bonds. Fluorescent of 1 was investigated.