The intercalation of SbCl4F and SbCl3F2 into graphite is described. The c-axis identity period, measured by (00/) x-ray diffraction, is 9.30, 12.69, and 16.04 Å for stages 1, 2, and 3, respectively, of SbCl4 F-intercalated graphite. The c-axis identity period for stage 1 SbCl4F-intercalated graphite is 8.85 Å. Mass spectroscopy shows that the molecule in SbCl4F-intercalated graphite is a (SbCl4F)4 tetramer. The molecule in SbCl3F2-intercalated graphite is a (SbCl3F2)4 tetramer. Mossbauer measurements show that Sb is in a 5 + state in SbCl4F-intercalated graphite.