In the current study, the heteronuclear coordination polymer C12H18Cu2MgO12 was synthesized in crystalline form using the gradual evaporation method and utilized as a precursor for the synthesis of CuO/MgO mixed nano-oxide. The crystal structure and thermal stability of the polymer were confirmed. Following the calcination of the polymer compound at 500°C, CuO/MgO mixed nano-oxide were synthesized. The morphology and structure of the nanopowders were characterized through FE-SEM, EDX, XRD, FT-IR, VSM, XPS, ICP-OES, and TEM techniques. Ultimately, the nanopowders were employed as catalysts in the azide–alkyne cycloaddition reaction. With very low leaching of copper (2.40 ppm) and magnesium ions (0.52 ppm), CuO/MgO nanocatalyst recycling and reuse were achieved for up to five cycles.
