Isolation of CeLu2N@Ih‐C80 through a Non‐Chromatographic,Two‐Step Chemical Process and Crystallographic Characterization of the Pyramidalized CeLu2N within the Icosahedral Cage |
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Authors: | Prof. Dr. Steven Stevenson Hannah R. Thompson Kristine D. Arvola Kamran B. Ghiassi Prof. Dr. Marilyn M. Olmstead Prof. Dr. Alan L. Balch |
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Affiliation: | 1. Department of Chemistry, Indiana‐Purdue University Fort Wayne, 2101 E. Coliseum Blvd, Fort Wayne, IN, 46805 (USA);2. Department of Chemistry, University of California, Davis, One Shields Avenue, Davis CA, 95616 (USA) |
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Abstract: | By combining two chemical methods of purification, 4 mg of purified CeLu2N@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, CeLu2N@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 CeLu2N@C80 in the co‐crystal CeLu2N@Ih‐C80 ? Ni(octaethylporphyrin) ? 2(toluene) reveals that the Ih‐C80 cage is present with a pyramidalized CeLu2N unit inside. |
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Keywords: | cerium endohedral fullerene lutetium purification structure elucidation |
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