The NiCexFe2-xO4 polycrystalline spinel compound with composition x = 0.005, 0.010, 0.015, and 0.02 was synthesized by the solid reaction method using the high energy milling (HEM) apparatus. Measurement of the neutron diffraction patterns is carried out at room temperature using a high resolution powder neutron diffractometer (HRPD), wavelength λ = 1.8213 Å. The measured neutron diffraction data were analyzed by the Rietveld method utilizing the FullProf analysis code. The results of the neutron diffraction pattern refinement revealed that the sample has a cubic symmetry, the Fd-3m space group, mixed inverse spinel structure, A-site occupied by cation Fe3+, Ni2+, dan Ce3+. Whereas the B-site is only occupied by Fe3+ and Ni2+. The mole fraction of Fe3+ at the B-site is greater than the Fe3+ mole fraction at the A-site, whereas the mole fraction of Ni2+ at the B-site is smaller than the mole fraction of Ni2+ at the B-site. As a result of Ce3+ doping, oxygen position parameters increase, magnetic moments on B-site, and the net magnetic moments decrease. Ni2+ concentrations at the A-site and the B-site were not affected by the amount of Ce3+ substitutions. Without substitution and after Ce3+ substitution, the O-site occupancy factor is still oxygen deficient.