Using novel compounds for synthesis of metal oxide nanomaterials can tune their physical properties due to the associated variation in the shape, size and crystallinity. In this work, gamma-Fe2O3 and Co3O4 nanoparticles were successfully prepared by a facile thermal decomposition route, employing [Fe(C32H22N4O2)]center dot 2H(2)O and [Co(C16H11N3O4)]center dot 1/2H(2)O complexes, respectively as new precursors. The x-ray diffraction and high resolution transmission electron microscopy investigation confirmed that the materials consist of highly pure spinel gamma-Fe2O3 and Co(3)O(4 )nanoparticles with average size of similar to 9 and 30 nm, respectively. The electrical conduction is governed by the hopping mechanism. The thermoelectric power measurements confirmed that Co3O4 nano-particles are non-degenerate semiconductor with Fermi energy similar to 1.21 eV while gamma-Fe2O3 nanoparticles showed a degenerate to non-degenerate transition. The Co3O4 nanoparticles showed a weak ferromagnetic ordering that could be attributed to uncompensated surface spins due to finite-size effects. But gamma-Fe2O3 NPs show super-paramagnetic behavior at room temperature.