Sulfaguanidinesalicylaldimine is a good bacteriostatic and a good complexing agent. Schiff-base complexes of Cu(II), Ni(II), Co(II), Zn(II), Cd(II), VO(IV), and UO 2 (VI) have been synthesized. The structural features of the complexes have been confirmed by microanalytical data, FAB mass, IR, UV-Vis, 1 H-NMR, and EPR spectra. Molar conductance indicates the presence of nonelectrolytes. Spectroscopic and other analytical studies reveal the square-planar geometry for copper, square-pyramidal geometry for oxovanadium, seven-coordinate UO 2 (VI) complex, and octahedral geometry for other complexes. The EPR spectrum of the copper complex in the powdered form at 77 K was recorded. The redox behavior of the copper and oxovanadium complexes was studied using cyclic voltammetry. Antimicrobial activities of the compounds have been studied against microorganisms such as Escherichia coli, Staphylococcus aureus, and Candida by well-diffusion technique in DMSO. Some of the complexes have higher activity than the free ligand and the standard.