Chromium (V1) tetrafluoride oxide can be prepared in high yield and purity from Cr02Fz and KrF, in HF solution. The vibrational spectra of gaseous, solid, and matrix-isolated CrF40 and its BrF, and HF solutions are reported, as well as the I9F NMR spectra of the BrF, and SOzCIF solutions. The data confirm for gaseous, matrix-isolated, and dissolved CrF40 a monomeric, squarepyramidal structure of symmetry C, and for solid CrF40 a fluorine- ...