A new phosphate, Na2.5Y0.5Mg7(PO4)6 was synthesized as single crystals by the flux method and as a powdered sample by the Pechini technique, and investigated by single crystal X-ray diffraction, charge distribution (CD) and 31p NMR spectroscopy. This compound crystallized in the rhombohedral space group R -3 and its equivalent hexagonal cell had the following parameters: a=1.4976(6) nm, c=4.2599(7) nm, Z=18. The structure consisted of MgO5, MgO6, YO6, (Na, Y)O8 and NaOx (x=6, 7 and 9) polyhedra which were linked either directly through common comers, edges and faces and by means of the PO4 tetrahedra via common comers and edges, giving rise to a com-plex three-dimensional framework, similar to that of the fillowite-like structure. The cation distribution was confirmed by charge distribution (CD) calculations and 31P NMR spectroscopy study.
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