Seven-minute synthesis of pure Cs,-C60Cl6 from [60]fullerene and iodine monochloride:: First IR, Raman, and mass spectra of 99 mol % C60Cl6

Three previously reported procedures for the synthesis of pure C-s-C60Cl6 from C-60 and ICI dissolved in benzene or 1,2-dichlorobenzene were shown to actually yield complex mixtures of products that contain, at best, 54-80% C-s-Cl-60(6) based on HPLC integrated intensities. MALDI mass spectrometry was used for the first time to identify other components of the reaction mixtures. An improved synthetic procedure was developed for the synthesis of about 150 mg batches of chlorofullerenes containing 90% C-s-C60Cl6 based on HPLC intensities. The optimum reaction time was decreased from several days to seven minutes. Small amounts of the product were purified by HPLC (toluene eluent) to 99% purity. The pure compound C-s-6C(60)Cl(6) is stable for at least three months as a solvent-free powder at 25 degrees C. The Raman, far-IR, and MALDI mass spectra of pure C-s-C60Cl6 are reported for the first time. The Raman and far-IR spectra, the first reported for any C60Cln chlorofullerene, were used to carry out a vibrational analysis of C-s-C60Cl6 at the DFT level of theory.