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The present article is devoted to the characterization of the structural phase transitions of the [CH 3 NH 3 ][Co(COOH) 3 ] ( 1 ) perovskite-like metal-organic compound through variable-temperature single-crystal neutron diffraction. At room temperature, compound 1 crystallizes in the orthorhombic space group Pnma (phase I ). A decrease in temperature gives rise to a first phase transition from the space group Pnma to an incommensurate phase (phase II ) at approximately 128 K. At about 96 K, this incommensurate phase evolves into a second phase with a sharp change in the modulation vector (phase III ). At lower temperatures ( ca 78 K), the crystal structure again becomes commensurate and can be described in the monoclinic space group P 2 1 / n (phase IV ). Although phases I and IV have been reported previously [Boča et al. (2004). Acta Cryst. C 60 , m631-m633; Gómez-Aguirre et al. (2016). J. Am. Chem. Soc.  138 , 1122-1125; Mazzuca et al. (2018). Chem. Eur. J.  24 , 388-399], phases III and IV corresponding to the Pnma (00γ)0 s 0 space group have not yet been described. These phase transitions involve not only the occurrence of small distortions in the three-dimensional anionic [Co(HCOO) 3 ] - framework, but also the reorganization of the [CH 3 NH 3 ] + counter-ions in the cavities of the structure, which gives rise to an alteration of the hydrogen-bonded network, modifying the electrical properties of compound 1 .

Incommensurate structures of the [CH3NH3][Co(COOH)3] compound

Incommensurate structures of the [CH₃NH₃][Co(COOH)₃] compound