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Temperature-dependent single-crystal X‑ray data were collected on gismondine (GIS) Ca 4 (Al 8 Si 8 O 32 )・18H 2 O from Rio Pian del Foco, Genova province, Italy, in steps of 25 °C up to 600 °C. At room temperature, gismondine has space group P2 1 /c with a = 10.0214(1), b = 10.5997(1), c = 9.8327(1) Å, b = 92.363(1)°, V = 1043.58(2) Å 3 . This structure remained stable up to 50 °C. The dehydration behavior then divided into two different pathways depending on the sample. In the more frequent path I, the LT P2 1 2 1 2 1  structure (phase B) Ca 4 (Al 8 Si 8 O 32 ) ・12H 2 O [a = 13.6801(8), b = 10.4670(6), c = 13.8667(9) Å, V = 1985.6(2) Å 3 ] formed at 75 °C. The orthorhombic structure has a doubled volume relative to the monoclinic room-temperature structure. At 150 °C the HT P2 1 2 1 2 1  structure (phase C) with 8 H 2 O pfu [a = 13.9014(12), b = 8.9469(8), c = 13.9697(14) Å, V = 1737.5(3) Å 3 ] occurred. This phase C has strongly compressed elliptical channels with Ca ions bonding to adjacent walls. At high temperature (300 °C), the quality of the diffraction pattern in path I further degraded and became inclusive.

Topotactic transformation and dehydration of the zeolite gismondine to a novel Ca feldspar structure