ABSTRACT: Synthesis, spectroscopy and temperature effects on the complexes of Co(II), Ni(II), Cu(II), Zn(II) With ligands N-ethyldiisopropylamine, diethylenetriamine and the preparation of nano-oxides of the metals by heating the synthesized complexes In this research, the synthesis method, the spectral review and magnetic properties of mononuclear complexes of Cobalt (II) ion, Nickel (II), Copper (II) and Zinc (II) are described by using Ligands N-ethyldiisopropylamine, diethylenetriamine and Cobalt (II) nitrat salt –Nickel (II) nitrat – Copper (II) nitrat – Zinc (II) nitrat – Cobalt (II) sulfate salt – Nickel (II) sulfate and Copper (II) sulfate. Methanol solvent has been used To bind ligands to the metal in non-aqueous environment and also to give chance to metal to become multi nuclear with Alkoxide. The complex synthesis was perfomed in one step and then characterized by infrared spectroscopy (FT-IR), ultra-violet visible spectroscopy (UV-Vis), basis analysis (C.H.N) and investigating the magnetic properties. Ligands disintegrated or separated from complex and metal ions changed to Copper oxide, Nickel oxide, Cobalt oxide and Zinc oxide nanoparticles, after synthesizing of complexes and heating them at 800 °C for 2 hours. After synthesizing the nanoparticles, detected the nanoparticles was performed by using infrared spectroscopy (FT-IR) techniques, X-ray powder diffraction (XRD).