It seems that the use of coordination compounds as suitable precursors to synthesize ferrite micro/nanoparticles via solid-state methods has not been well developed. For this purpose, [Co(en) 3 ][Fe(ox) 3 ] complex (where en = ethylenediamine and ox = oxalate) as a novel precursor was used to prepare CoFe 2 O 4 nanoparticles. Solid-state thermal decomposition of the synthesized precursor at different temperatures in the range of 400-800°C led to the formation of CoFe 2 O 4 micro/nanoparticles with various particle sizes. X-ray diffraction patterns showed that pure CoFe 2 O 4 and CoFe 2 O 4 /Co 3 O 4 composite have been formed by thermal decomposition of the precursor at 700 and 800°C, respectively. In addition, it was concluded that by increasing the calcination temperature, particles sizes of the CoFe 2 O 4 nanoparticles increased as expected. According to the optical properties of the products, it was found that CoFe 2 O 4 micro/nanoparticles were semiconductors with electronic band gap of between 2.1 and 3.2 eV.