The incomplete hydrolysis of XeF(6) has been used to prepare a xenon oxyfluoride, XeOF(4). The latter is a clear, colorless liquid, freezing at -41 degrees C. The infrared and Raman spectra show that the XeOF(4) molecule has a fourfold symmetry axis. The large Xe-O stretching force constant indicates the Xe-O bond has appreciable double bond character.