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Aluminum-rich titanites [Ca(Ti,Al)(O,F)SiO 4 ] with X Al  &gt; 0.53 [X Al  = Al/(Al+Ti)], including the pure end-member CaAlFSiO 4 , were synthesized for the first time in a high-pressure experimental study. The crystal structure of CaAlFSiO 4  was determined by Rietveld analysis of an X-ray powder diffraction pattern. CaAlFSiO 4  is monoclinic, belongs to the space group A2/a, and has the unit-cell dimensions a = 6.9149(2) Å, β = 8.5064(1) Å, c = 6.4384(2) Å, and b = 114.684(2)°. The unit-cell volume is less than 93% of CaTiOSiO 4 , which is consistent with the natural occurrence of Al-rich titanite in high-P rocks. Although previous studies suggested that titanite with X Al  &gt; 0.5 is possibly not stable, this study demonstrates that complete solid solution occurs between CaTiOSiO 4  and CaAlFSiO 4 . The similarity of the crystal structures of titanite and CaAlFSiO 4  explains why in natural Al-rich titanite the end-member CaAlFSiO 4  generally dominates over the hypothetical end-member CaAlOHSiO 4 , which under geological conditions is stable in a different crystal structure.

The synthesis and crystal structure of CaAlFSiO 4 , the Al-F analog of titanite