Title

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

Document Type

Article

Publication Date

6-8-2015

Publication Source

Chemistry - European Journal

Volume

21

Issue

29

Inclusive pages

10362–10368

DOI

10.1002/chem.201500915

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.

Disciplines

Chemistry

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