Transmission infrared, Attenuated Total Reflectance (ATR) and Raman spectra of crystalline methylammonium iodide (MAI) and formamidinium iodide (FAI) in the temperature interval starting from –170 ºC to 200 ºC were studied. The spectra recorded in the region from 4000 to 500 cm–1 enabled resolving the ambiguities associated with the origin of some bands. For the first time a complete and detailed vibrational investigation and assignment of the IR spectra of these compounds based on the differences in the temperature dependent IR spectra for all phases, including the metastable ones, have been made. The findings support the already established crystal structure of the phases for both compounds. The correlation between the overtones and fundamental modes has been confirmed based on the temperature induced isosbestic point.
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