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Chromyl fluoride provides a nonconducting solution in anhydrous hydrogen fluoride with Raman spectroscopic features indistinguishable from those of the solute in the gas phase, indicating no fluoride or proton transfer in solution. With increasing acidity in the SbF5–HF solvent system, CrO2F2forms cationic species, the nature of which is discussed. The acidity-dependence of cationic speciation in HF–TaF5and in HF–AsF5is consistent with that in HF–SbF5. Keywords: chromyl fluoride, antimony fluoride, Lewis acid, Raman spectroscopy, hydrogen fluoride.