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Isolation of CeLu2N at Ih-C80 through a Non-Chromatographic, Two-Step Chemical Process and Crystallographic Characterization of the Pyramidalized CeLu2N within the Icosahedral Cage

Abstract

© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. By combining two chemical methods of purification, 4mg of purified CeLu2N at C80 was readily isolated from 500mg 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 stage1, CeLu2N at C80 was selectively precipitated by virtue of its low first oxidation potential (+0.01V) and the judicious choice of MgCl2 as the Lewis acid precipitant. For stage2, 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 stage1. Crystallographic analysis of CeLu2N at C80 in the co-crystal CeLu2N at Ih-C80Ni(octaethylporphyrin)2(toluene) reveals that the Ih-C80 cage is present with a pyramidalized CeLu2N unit inside.

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