Isolation of CeLu2 N@Ih -C80 through a Non-Chromatographic, Two-Step Chemical Process and Crystallographic Characterization of the Pyramidalized CeLu2 N within the Icosahedral Cage

Journal Reference

Chemistry. 2015;21(29):10362-8.

Stevenson S1, Thompson HR2, Arvola KD2, Ghiassi KB3, Olmstead MM4, Balch AL5.

[expand title=”Show Affiliations”]
  1. Department of Chemistry, Indiana-Purdue University Fort Wayne, 2101 E. Coliseum Blvd, Fort Wayne, IN, 46805 (USA). [email protected].
  2. Department of Chemistry, Indiana-Purdue University Fort Wayne, 2101 E. Coliseum Blvd, Fort Wayne, IN, 46805 (USA).
  3. Department of Chemistry, University of California, Davis, One Shields Avenue, Davis CA, 95616 (USA).
  4. Department of Chemistry, University of California, Davis, One Shields Avenue, Davis CA, 95616 (USA). [email protected].
  5. Department of Chemistry, University of California, Davis, One Shields Avenue, Davis CA, 95616 (USA). [email protected].
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Abstract

By combining two chemical methods of purification, 4 mg of purified CeLu2 N@C80 was readily isolated from 500 mg of carbon soot extract without the use of recycling HPLC, a method which has previously been necessary to obtain pure samples of endohedral fullerenes. In stage 1, CeLu2 N@C80 was selectively precipitated by virtue of its low first oxidation potential (+0.01 V) and the judicious choice of MgCl2 as the Lewis acid precipitant. For stage 2, we used a stir and filter approach (SAFA), which employed the electron-rich NH2 groups immobilized on silica gel to selectively bind residual endohedrals and higher cage fullerenes that were contaminants from stage 1. Crystallographic analysis of CeLu2 N@C80 in the co-crystal CeLu2 N@Ih -C80 ⋅Ni(octaethylporphyrin)⋅2(toluene) reveals that the Ih -C80 cage is present with a pyramidalized CeLu2 N unit inside.

© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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