In this investigation, we report synthesis of new Copper - Barium complex. This compound has been characterized using FT-IR and UV–Vis spectroscopy. The electrochemical properties of compound have also been investigated by cyclic voltammetry and the complex shows irreversible redox behavior. Also in this study we report facile synthesis of Copper-Barium nanocomposites oxide under thermal decomposition, using [Cu(Opd)3]2[Ba(SCN)6(H2O)2] precursor complex. Characterization of Copper-Barium Oxide nanocomposites was carried out by scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX),X-ray powder diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. The X-ray diffraction pattern at room temperature revealed that, highly pure and crystallized Cu2BaO4 with tetragonal structure.