In this study, the synthesis of a novel tetraoxime (LH 4) derivative containing hydrazone side groups, and its transition metal complexes with Ni(II), Cu(II), Co(II), and Zn(II) ions, were reported. The ligand was synthesized by reacting anti-glyoximehydrazine (GH 2 ) with terephthaldialdehyde. Polymeric complexes with Ni(II) and Co(II) and binuclear complexes with Cu(II) and Zn(II) of this tetraoxime were isolated.Structural assignments were supported by a combination of 1 H-NMR, 13 C-NMR, HMQC, FT-IR, UV-Vis, thermogravimetric analysis (TGA), molar conductances, elemental analyses, and magnetic susceptibility.