The subsequent co-refinement to X-ray and neutron powder diffraction data included the new phase (87.4 wt%), V 2-x Ni x O 3 (6.8 wt%), and NiO (5.8 wt%). The x value in V 2-x Ni x O 3 refined to 0.5058 ± 0.0060, indicating the solid solution was below its reported solubility limit of x = 0.75. The refinements and impurity phase contributions are shown in Fig. and refined atomic parameters are reported in Table . The Fe 2 O 3 impurity introduced by ball milling was not included due to its extremely small contribution to the structural peaks. Every peak reported by Gianoglio and Ramonda was observed.