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The DSC diagram of tris(allylammonium) hexachlorobismuthate(III), (C 3 H 5 NH 3 ) 3 [BiCl 6 ], revealed three anomalies at 152, 191 and 299 K. The structure of the salt was determined at 200 and 315 K, below and above the high-temperature phase transition at 299 K. In both phases the crystals are monoclinic. At 200 K the space group is C2/c whereas at 315 K it is C2/m. The structures, at both temperatures, are composed of [BiCl 6 ] 3−  octahedra and allylammonium cations. The organic and inorganic moieties are attracted to each other by a network of the N-H. . .Cl hydrogen bonds. The relationship between corresponding parameters of the unit cells has been found. The phase transition at 299 K, of the order-disorder type, is attributed to the ordering of one non-equivalent allylammonium cation in the low-temperature phase.

Phase Transitions and Distortion of [BiCl 6 ] 3– Octahedra in (C 3 H 5 NH 3 ) 3 [BiCl 6 ] – DSC and Single-Crystal X-Ray Diffraction Studies