In this study, the synthesis of a novel tetraoxime (LH4) 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 H-1-NMR, C-13-NMR, HMQC, FT-IR, UV-Vis, thermogravimetric analysis (TGA), molar conductances, elemental analyses, and magnetic susceptibility.