Bidentate ligands have been synthesized by the reaction of 2,4-dichlorobenzaldehyde with 4-amino-5-mercapto-1,2,4-triazole and 4-amino-5-mercapto-3-propyl-1,2,4-triazole. The ligands react with acetates of Co(II), Ni(II), Cu(II), and Zn(II) to yield 1:2 [metal:ligand] complexes. The newly synthesized compounds were characterized by elemental analyses, spectral (UV-Vis, IR, H-1 NMR, fluorescence, ESR) studies, thermal techniques, and magnetic measurements. Thermal studies of the complexes showed a multistep decomposition pattern. A square planar geometry for Cu(II) and octahedral geometry for Co(II), Ni(II), and Zn(II) complexes have been proposed. The synthesized complexes exhibit enhanced antimicrobial activity against Staphylococcus aureus, Bacillus subtilis, Aspergillus niger, and A. flavus compared to parent ligands. However, tested compounds did not exhibit any activity against Escherichia coli and Pseudomonas aeruginosa.