Based on the different oxidation potentials of endohedral fullerenes Sc3N@C80 Ih and D5h and Sc3N@C78, an efficient and useful method that avoids HPLC has been developed for their separation. Selective chemical oxidation of the Sc3N@D5h-C80 isomer and Sc3N@C78 by using an acetylferrocenium salt [Fe(COCH3C5H4)Cp](+) followed by column chromatographic separation and reduction with CH3SNa resulted in the isolation of pure Sc3N@Ih-C80, Sc3N@C78, and a mixture of Sc3N@D5h-C80 and Sc3N@C68.
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