A new vicinal dioxime ligand containing azo and thione chromophores, namely 1,3-bis[4-(phenyldiazenyl)-phenyl]-2-thiooxaimidazoline-4,5-dione dioxime (bppH 2 ), was synthesized by the reaction of cyanogen di-N-oxide with N,N 0 -bis(4-phenylazophenyl) thiourea in dichloromethane solution at -10°C. Mononuclear complexes of bppH 2 with nickel(II), cobalt(II), and copper(II) were synthesized. The complexes, [Ni(bppH) 2 ], [Cu(bppH) 2 ], and [Co(bppH) 2 ] were characterized by several techniques using elemental analyses, conductivity measurements, FT-IR, and electronic spectral studies. The data suggest that the ligand coordinates through the N,N atoms, as do most vic-dioximes. The molar conductivities in DMF solution indicate nonelectrolytic nature for the complexes. Antimicrobial activities of the ligand and its metal complexes were estimated for five bacteria, namely Klebsiella pneumoniae, Micrococcus luteus, Mycobacterium smegmatis, Enterobacter cloaca and Bacillus megaterium and three fungi, namely Candida albicans, Kluyveromyces marxianus, and Rhodotorula rubra.