Solid solutions of Me 3 (PO 4 ) 2 in Ni 3 (PO 4 ) 2 , with the olivine-related sarcopside structure ( P 2 1 / a ), have been prepared and equilibrated at 1070 K ( Me = Mg, Mn, Fe, Co, Cu, or Zn). Accurate unit cell dimensions have been obtained from Guinier-Hägg photographic X-ray diffraction data. The cell volumes of the (Ni l – z Me z )3(PO 4 ) 2 phases are correlated to the size and amount of Me 2+ . Rietveld full-profile refinements based on neutron powder diffraction data have been utilized to determine the distribution of cations among the two distinct octahedral sites M1 and M2. The preference for M1 over M2 is Ni 2+ > Co 2+ > Mg 2+ , Zn 2+ > Mn 2+ > > Fe 2+ . The cation distribution results are compared with corresponding results for olivines, orthopyroxenes, and some other oxosalt structures with metal-oxygen octahedra similar in size and shape to those in olivine. It is concluded that the Ni 2+ / Me 2+ distributions in these structure types are mainly controlled by crystal field energies, while the size effects are small.
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