Utilizing 3,5-bis(x-pyridyl)-1,2,4-triazole (x-Hpytz, x = 3; x = 4) as multidentate ligands, six novel coordination polymers with Zn(II) or Cd(II) metal ions were prepared: [Zn(3-pytz)0.5(OH)0.5Cl]n (1, 1D ladder), {[Zn(3-Hpytz)(H2O)4] [Zn(3-Hpytz)(H2O)3·SO4]SO4·5H2O}n (2·5H2O, 1D chain), [Cd(3-Hpytz)(SO4)]n (3, 3D framework), {[Cd(3-Hyptz)SO4·3H2O]·2H2O}n (4·2H2O, 1D chain), [Zn(4-pytz)Cl]n (5, 3D framework) and [Zn2(4-pytz)(SO4)(OH)]n (6, 3D framework). All compounds were obtained from hydrothermal reactions, with the exception of compound 4 which was obtained by solvent diffusion at room temperature. All compounds were characterized by FTIR, elemental analysis and TGA analysis and their structures were determined by X-ray diffraction. All compounds exhibited substantial thermal stability and showed photofluorescent properties that resulted from ligand π–π* transition.