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A new hydrogen-containing Ca 9 (Fe 0.63 Mg 0.37 )H 0.37 (PO 4 ) 7  phosphate with the whitlockite-type structure has been synthesized by a hydrothermal method and its structure has been studied by the single-crystal X-ray diffraction. The compound crystallizes in the trigonal space group  R 3 c  (traditional for compounds with the whitlockite-type structure) with unit-cell parameters:  a =10.3533(1) Å,   c =37.1097(4) Å. The structure has been determined using the “charge flipping” method. Ca 9 (Fe 0.63 Mg 0.37 )H 0.37 (PO 4 ) 7  structure is similar to that of other members of the whitlockite-type family. The presence of hydrogen in the structure leads to the formation of OH-group with one of the oxygen of PO 4 -tetrahedra. Based on an analysis of the bond valence sums (BVS) a conclusion has been made about localization of H atoms in the structure. Smaller values of BVS for O1 and O10 atoms than ones for other oxygen atoms indicate localization of H atoms between them in a position with site symmetry 18 b .

A new hydrogen-containing whitlockite-type phosphate Ca 9 (Fe 0.63 Mg 0.37 )H 0.37 (PO 4 ) 7 : hydrothermal synthesis and structure