This paper reports a new method for the synthesis of [Co(Salen)(PPh 3 )(H 2 O)] 4 [Fe(CN) 6 ] [Co(Salophen)(PPh 3 )(H 2 O)] 4 [Fe(CN) 6 ] (where salen and salophen are tetradentates Schiff base ligands) complexes as a novel precursor to prepare Co 3 O 4 /CoFe 2 O 4 nano magnetic compounds by thermal decomposition at 500, 550 and 600°C. The precursor complexes were identified by FT-IR and UV-Vis spectroscopy and its thermal behavior was studied via TG/DTA. The samples were characterized by Powder X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), and Fourier Transform Infrared Spectroscopy (FT-IR). Magnetic properties of the synthesized nanoparticles were determined by Vibrating Sample Magnetometer (VSM) at room temperature and magnetic parameters such as the saturation magnetization (M s ), remanence magnetization (M r ), the coercive field (H c ) and the squareness ratio (SQ = M r /M s ) were determined. The purity, composition and stoichiometry of the prepared sample were studied by Electron Diffraction X-ray spectroscopy (EDX) spectra. The prepared nano-composites show features like high magnetization, good chemical stability and dispersivity, which are useful in some practical applications.