A fabricated Azo ligand (E)-1-[4-(3,4-dichloro-2-hydroxyphenyl) diazenyl] phenylethan-1-one was produced by a coupling reaction between diazonium salt made from p-aminoacetophenone and a basic solution of 2,3-dichlorophenol. The azo compound was used to form complexes with Cr(III), Co(II), Ni(II), and Cu(II) ions at a 2L:1M molar ratio in an alcoholic medium. The ligand and its complexes were characterized using a set of spectroscopic techniques to obtain chemical and structural information. Infrared with Fourier transformation; ultraviolet and visible; ¹H/¹³C nuclear magnetic resonance; mass; thermal analysis and micro elemental analysis spectrometry, as well as molar conductivity. The results certified the chemical moiety and geometric fabrication. Azo dye acts as a bidentate ligand with phenol/hydroxy terminals. The finding was that Cr(III), Co(II), and Ni(II) complexes were characterized by a six-coordinate (distorted octahedral) geometry, whereas the Cu(II) complex had a tetrahedral structure. Thermal decomposition of the ligand and the selected complex was studied to assess stability upon heating and to determine the final residue.