A multi-temperature X-ray diffraction study was performed on the colossal magnetoresistive thiospinel FeCr 2S 4 to find out if structural phase transitions are associated with the magnetic transitions of the two Fe and Cr sublattices. The temperature dependence of the cell parameters was carefully screened, and the crystal structure was determined at four different temperatures. The present X-ray diffraction experiment, the first performed on a single crystal, confirms that bulk FeCr 2S 4 is not subject to structural phase transformations in the temperature range 293–23 K. The occurrence of the forbidden (0 0 2) reflection and the non-stoichiometric sample composition are discussed.