2-Aminopyridine (2-ampy) and acetylacetone has been allowed to react with the Ni(II) and Co(II) metal salts to give complexes of the type [CoIII(acac)2(2-ampy)2]ClO4 (1), [NiII(acac)2(2-ampy)H2O]ClO4(2-ampyH) (2), and [NiII(acac)2(2-ampy)H2O] (3). The crystal structures of the complexes have been determined by X-ray diffraction. The data of antimicrobial analysis have indicated that the complexes have rather good activities against bacterial species. Through investigating the antioxidant activity by FRAP and anti-hemolytic assay, all the metal complexes have shown an acceptable activity. In addition, NiO nanoparticles have been prepared by the combustion synthesis method of complex 3 at 700°C for 8 h.