With the help of facile single source molecular precursor the synthesis of CuAl2O4 nanopowder with well-defined structural framework was carried out via cost-effective soft–chemical approach with two and three coordination state around copper and Aluminum atom respectively. The synthesized nanoparticles were thoroughly characterized by using several physicochemical techniques such as XRD, SEM, TEM, thermal analysis, UV and FT-IR for structural, optical and morphological studies. With the adjustment of reaction parameters allows us for systematic tuning of particle size, shape as well as to control the other functional properties. It can be concluded that self-assembly is an integral part which take place by understanding the metal chemistry during synthetic approach and therefore help to opens a new exciting opportunities for better understanding the reaction conditions, growth and along its mechanistic approach which leads to fabrication of potential nanodevise in near future.