Two new mixed-ligand coordination polymers of [Zn(μ-mptrz)(mptrz)(μ-en)0.5]n (1) and {[Cd(μ3-mptrz)(μ-en)0.5Br].DMSO}n (2) were prepared from the reaction of 4-methyl-1,2,4-triazole-3-thiol (Hmptrz) and ethylene diamine (en) with ZnBr2 and CdBr2 in CH3OH, respectively. Both complexes were characterized by spectral methods (IR, UV-Vis, 1H NMR and luminescence), elemental analysis, thermal analysis (TG, DTA) and single crystal X-ray diffraction. The X-ray structural analysis indicated that the structures of these two compounds are two-dimensional (2D) layer structures. In complex 1, each Zn atom has a distorted tetrahedral coordination geometry, and the Zn centers are linked by µ-mptrzˉ to form a linear chain of [Zn(μ-mptrz)(mptrz)]n in b-direction, which are further bridged by the en ligands to form a two-dimensional layer network. Also, in complex 2, each Cd atom has an distorted octahedral coordination geometry, and the Cd centers are linked by three µ-mptrzˉ anions to form one-dimensional stair-stepped coordination polymers of [Cd(μ3-mptrz)Br]n in a-direction, which are further bridged by the en ligands to form a two-dimensional layer network