Complexes of the Cr(III), Fe(III), Rh(III), Ru (III), Mo hexagonal valence and Co(II) were prepared using the azo dye 1,1'-(1,3-phenylene bis(diazene-2,1-diyl))bis(2,4,6-trihydroxy-3,1-phenylene))bis(ethan-1-one), which was prepared newly from diazonium salt with 2,4,6-trihydroxyacetophenone, after isolation. The compounds were characterized using proton and carbon nuclear magnetic resonance of the ligand and fine elemental analysis, infrared, ultraviolet-visible, mass measurement, thermogravimetric analysis, differential thermal scanning, metal percentage determination, chlorine content determination, magnetic susceptibility, and molar conductivity. The results showed that the tetra coordinated anionic bond, when linked to metal ions via the two phenolic oxygen atoms and the two azo nitrogen atoms, gave octahedral mononuclear complexes for all the complexes. With the exception of cobalt, where the complex was a tetrahedral dinuclear and the ligand was hexadentate when linked via the two phenolic oxygen atoms, the two carbonyl oxygen atoms, and the two azo nitrogen atoms. The potential of the prepared compounds as antioxidants and their ability to suppress free radicals were also studied, and some compounds were identified for evaluation of their anticancer effectiveness. The potential of the prepared compounds as antioxidants and their ability to suppress free radicals were also studied, and some compounds were identified for evaluation of their anticancer activity against MCF-7 cells