Isolation of CeLu2N@Ih‐C80 through a Non‐Chromatographic, Two‐Step Chemical Process and Crystallographic Characterization of the Pyramidalized CeLu2N within the Icosahedral Cage. Issue 29 (8th June 2015) - Stevenson, Steven
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.