The conversion Of (C2.5F)n fluorine-graphite intercalation compounds (GIC) into covalent graphite fluoride during a post-treatment in pure F-2 gas is studied by solid-state NMR. First, a careful characterization of the starting material is performed; in particular, for the first time for fluorinated carbons, two-dimensional F-19 -> C-13 cross-polarization wide-line separation (CP-WISE) experiments were carried out. This completes the classical NMR data such as F-19 and C-13 chemical shifts, quantitative C-13 solid echo, and C-F bond length measurements, which were estimated by dipolar recoupling using inverse CP MAS. The data of the raw (C2.5F)n and of the samples post-fluorinated at 350, 450, and 550 degrees C were compared to investigate the C-F bonding as a function of the treatment temperature. The C-F bonding, is discussed taking into account a hyperconjugation of the C-F bonds with neighboring unfluorinated carbon atoms.