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, γ-Fe2O3 and Co3O4 nanoparticles were successfully prepared by a facile thermal decomposition route, employing [Fe(C32H22N4O2)]·2H2O and [Co(C16H11N3O4)].H2O 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 γ-Fe2O3 and Co3O4nanoparticles with average size of ∼ 9 and 30 nm, respectively. The electrical conduction is governed by the hopping mechanism. The thermoelectric power measurements confirmed that Co3O4 nanoparticles are non-degenerate semiconductor with Fermi energy ∼1.21 eV while γ-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 γ- Fe2O3 NPs show superparamagnetic behavior at room temperature.