Graphite intercalation compounds with large fluoroanions

Over the past 20 years, a number of relatively large, perfluorinated anions have been found to intercalate into graphite. This review will describe the background, some syntheses and structures of these graphite intercalations compounds (GIC's). The fluoroanion intercalates include perfluoroalkylimides, perfluoroalkylsulfonates, and perfluoroalkylborate esters. Synthetic methods can include either chemical oxidation, for example using K₂MnF₆ in anhydrous or hydrous hydrofluoric acids or electrochemical oxidation. These gallery structures present in these GIC's are larger and more complex than for most previously-known GIC's, and therefore may be important in advancing the known chemistry of graphite. In this review, the relationship of intercalate packing, orientation and conformation is discussed.     

Facile and efficient synthesis of C2-symmetrical 1,3,5-triazine polycarboxylate ligands under microwave irradiation

A rapid and efficient method for preparation of C₂-symmetrical 1,3,5-triazine polycarboxylate ligands was developed. The reactions included either selective mono- or di-substitution of 2,4,6-trichloro-1,3,5-triazine with various nucleophiles containing carboxyl group(s), followed by nucleophilic displacement of the remained chloride(s) in aqueous media under microwave irradiation. Novel C₂-symmetrical tripodal ligands were afforded in good yields and purities under short reaction time with simple work-up, which are potentially useful as structural directing units in metal-organic frameworks.     

The first synthesis of a graphite bis(oxalato)borate intercalation compound

A new graphite intercalation compound containing the bis(oxalato)borate anion, B[OC(O)C(O)O]₂⁻, is prepared for the first time by chemical oxidation of graphite with fluorine gas in the presence of a solution containing the intercalate anion in anhydrous hydrofluoric acid. The products of stage 1-3 compounds are characterized by powder X-ray diffraction, thermogravimetric analysis, and elemental analyses. X-ray diffraction data indicate a standing-up orientation for the borate anion, with long axis perpendicular to the graphene sheets. Elemental analyses provide x and δ for the nominal composition of C_xB[OC(O)C(O)O]₂·δF, where the chelate borate and fluoride are co-intercalates, and indicate a low borate, and high fluoride, intercalate content as compared to anion packing in other graphite intercalation compounds.