In this work, herein we report the synthesis, structural characterization and in vitro cytotoxic evaluation of two mixed Co(II)/Ni(II)-nalidixic acid-bipyridyl complexes (1 and 2). The structural analysis of metal complexes 1 and 2 was carried out by analytical and multispectroscopic techniques (FT-IR, UV-vis, EPR, sXRD). The crystallographic details of complexes 1 and 2 revealed a monoclinic crystal system with P21/c space group.