The synthesis of a novel ligand and its metal complexes. The hydroxybenzaldehyde derivative of diacetylmonoximehydrazide (HDMHmHB) ligand was prepared by reacting 3-hydroxybenzaldehyde with diacetylmonoxime hydrazide. Mononuclear complexes of this ligand of the type [M(DMHmHB)2] were synthesised in the presence of MeOH, where M= FeII, MnII, CoII, NiII, PdII, CuII, ZnII, HgII, and CdII, and the metal: ligand molar ratio is (1:2). For FeII , MnII , CoII , NiII , and CuII complexes, it is proposed that the metal ion complexes [[M(DMHmHB)2] be six-coordinated with an N4O2 donor environment, and four-coordinated with an N4 donor environment. The coordination of the ligand is performed by the oxime nitrogen, imine nitrogen, and phenolic oxygen atoms. Based on 1H-NMR, ESR, FT(IR), elemental analysis (C, H, N), magnetic susceptibility tests, and electronic spectroscopy, the structures of the complexes were hypothesised.