It is known from the literature that a slight distortion of the ideal cubic cell is present in the NiO structure. This work shows that such a distortion can be accurately evaluated by means of a refinement of the structural and profile parameters of X-ray powder diffraction data. Moreover, since only small amounts of products are sometimes at disposal to perform structural characterizations, it was thought useful to extend the refinement procedure to X-ray data collected on NiO samples of much lower mass (15-60 mg) than those usually utilized in X-ray diffractometric studies. The results obtained show that reliable structural parameters can be obtained from low mass samples too.