The electrochemical oxidation of graphite in a nitromethane solution containing the (perfluoropinacolato)borate anion, (B[OC(CF3)(2)C(CF3)(2)O](2)(-)), produces a new acceptor-type graphite intercalation compound (GIC). Stage 1-3 GICs are obtained and characterized by electrochemical methods and powder X-ray diffraction. The gallery height, d(i), of 14.0-14.5 Angstrom indicates a single intercalate layer between graphene sheets. The GICs are produced at higher charge efficiency and are more oxidatively stable than the previously reported intercalation of N(SO2CF3)(2)(-) from this solvent. The GICs are more stable to ambient exposure than most acceptor-type GICs; even the stage 1 material will persist in air for several hours. (C) 2003 The Electrochemical Society.