Abstract Nanostructures of coordination polymers,(CuL 1). 0.5 DMF. 0.5 EtOH. 1.5 H 2 O (1),[H 2 L 1= 5-(4-Carboxy phenyl azo) salicyilic acid],(Cu (L 2) 2)(2),[HL 2= 5-(4-Carboxy phenyl azo) salicylaldehyde] have been synthesized by the reaction of H 2 L 1 and HL 2 with Cu (OAc) 2. H 2 O by sonochemical process. CuO nanostructures were synthesized from calcination and thermal decomposition of compounds 1–2 nanostructures. Metalic copper ...