The investigations of bismuth halide chemistry in DMSO/MeOH solutions led to the discovery of a new solvent-stabilized compound with a chemical formula of CsBiBr·3DMSO. In addition, a new phase of CsBiBr was generated as a result of a crystal-to-crystal transition driven by the change in the solvent composition. The solvent stabilized CsBiBr·3DMSO adopts an orthorhombic 222 type crystal structure with unit cell dimension of = 13.6160(6) Å, = 14.4359(8) Å, and = 14.6487(7) Å. Bulk single crystals of CsBiBr·3DMSO with average size of 4.5 × 3.5 × 3.5 mm were grown by the antisolvent crystal growth method. With the change of the solvent composition from 2:1 DMSO: MeOH to 1:1 DMSO: MeOH, the single crystals of CsBiBr·3DMSO underwent a crystal-to-crystal transition yielding another structurally distinct CsBiBr phase, with a tetragonal 4/ type structure and unit cell dimensions of = 9.8394(5) Å, = 9.8394(5) Å, and = 8.0950(6) Å. Both compounds exhibit isolated BiBr octahedral resembling the structures of the zero-dimensional (0D) perovskites.
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