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Mn 3+  distribution at octahedral M1, M2, and M3 sites of piemontite and its effect on structural changes were investigated by X-ray Rietveld analysis of synthetic Ca 2 Al 3-p Mn 3+  p Si 3 O 12 (OH) piemontites. The material studied was synthesized from starting materials of Ca 2 Al 3-q Mn 3+  q Si 3 O 12.5  + H 2 O in hydrothermal experiments with P fluid  of 200 and 350 MPa and temperature of 500 °C. Piemontites crystallized as single phases from q = 0.5, 0.75, 1.0, and 1.1 starting materials, whereas minor amounts of bixbyite and parawollastonite were associated with those synthesized from q = 1.5 and 1.75 starting materials. EPMA analyses of synthetic piemontites showed that the maximum Mn 3+  content was 1.3(1) apfu. Site preference of Mn 3+  at the octahedral sites is M3 &gt; M1 &gt;&gt; M2. Mn 3+  occupancies (g) at the M3 and M1 sites are correlated with the p-value in piemontite as gM3 = - 0.20p2 + 1.00p and g M1  = 0.23p 2  - 0.06p, respectively, where 0.0 ≤ p ≤ 1.3. With increasing p-value, the mean M3-O and M1-O distances of piemontites increase, but the M1-O1 distance and the O5-Si3-O6 angle change nonlinearly due to the Jahn-Teller effect. The nonlinear variations of the a and c parameters with increasing p are caused by changes in the M1-O1 distance and the O5-Si3-O6 angle, respectively. The M3 octahedra, which are more distorted than the M1 octahedra, become more tetragonally compressed with increasing Mn 3+  at the M3 site, due to the substantial increase of the M3-O1 distance.

An X-ray Rietveld study of piemontite on the join Ca 2 Al 3 Si 3 O 12 (OH)–Ca 2 Mn 3 3+ Si 3 O 12 (OH) formed by hydrothermal synthesis