Metal complexes of the type [Co(phen)(2)(4-NO(2)pcyd)(2)].CH3OH, 1, [Zn(phen)(2)(4-NO(2)pcyd)(2)].CH3OH, 2, [Cd(phen)(2)(4-NO(2)pcyd)(2)], and 3, (phen=1,10-phenanthroline, 4-NO(2)pcyd=4-nitro phenylcyanamide) have been studied. The synthesis, characterization, and the biological activities of complexes 1-3 have been investigated. The geometries of complexes 1-3 were confirmed by single-crystal X-ray crystallography. The interactions of complexes 1-3 with human serum albumin (HSA) were studied using fluorescence and circular dichroism spectroscopy. The thermodynamic studies have showed the reaction for the binding of complexes 1-3 with HSA is hydrophobic (H-0?0 and S-0>0). The in vitro cytotoxic potential of complexes 1-3 and their complexes with HSA were examined. The complexes 1-3 with HSA enhance about 3-fold cytotoxicity in cancer cells lines.