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The polycrystalline spinel oxides NiX Co1-X Fe2O4 with composition x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0 were prepared by conventional solid state ceramic sintering technique in air at 1300°C. X-ray diffraction experiments were carried out on all the samples at room temperature in order to characterize the materials. X-ray diffraction patterns showed sharp peaks indicating the formation of single phase cubic spinel structure. The neutron diffraction experiments were performed on all samples at room temperature, with an incident monochromatic neutron beam of wavelength λ = 1.5656 Å. The experimental neutron diffraction data were analyzed using the computer program FullProf in the Reitveld method. Reitveld refinement of the neutron diffraction data reveals that the samples possess cubic symmetry corresponding to the space group F d-3m. Cation distribution between the two sublattices of the spinel structure has been found from the analysis of the neutron diffraction data. Lattice parameters, oxygen position parameters, and overall temperature factors have also been determined from the analysis of neutron diffraction data. The lattice parameter decreases and oxygen position parameter increases with increasing Ni content in the system. Sublattices and net magnetic moments have been determined from the refinement of neutron diffraction data. The magnetic structure at room temperature was found to be ferrimagnetic for all the samples.