2-Acetylpyridine-(4-phenylsemicarbazone) and o-vanillin-(4-phenylsemicarbazone) have been prepared and characterized on the basis of elemental analyses, infrared, electronic, ¹H and ¹³C NMR spectra. Several nickel(II) and copper(II) complexes have been obtained from these ligands. The IR spectra of the ligands as well as those of their complexes suggest that 2-acetylpyridine-(4-phenylsemicarbazone) is a neutral tridentate molecule while o-vanillin-(4-phenylsemicarbazone) is a monobasic tridentate molecule. On the basis of the analytical data, magnetic moments and spectral data, a square-planar geometry has been proposed for the nickel(II) and copper(II) complexes with these ligands. Some representative complexes of copper(II) and nickel(II) were found to have remarkable antifungal and antibacterial activity.