Isolation and Crystallographic Characterization of Gd3N@D2(35)-C88 through Non-Chromatographic Methods

• Published in: Inorganic chemistry Vol. 55; no. 1; pp. 62 - 67
• Main Authors: Stevenson, Steven, Arvola, Kristine D, Fahim, Muska, Martin, Benjamin R, Ghiassi, Kamran B, Olmstead, Marilyn M, Balch, Alan L
• Format: Journal Article
• Language: English
• Published: United States 04.01.2016
• ISSN: 1520-510X
• DOI: 10.1021/acs.inorgchem.5b01814

While several nonchromatographic methods are available for the isolation and purification of endohedral fullerenes of the type M3N@Ih-C80, little work has been done that would allow other members of the M3N@C2n family to be isolated with minimal chromatography. Here, we report that Gd3N@D2(35)-C88 can be isolated from the multitude of endohedral and empty cage fullerenes present in carbon soot obtained by electric-arc synthesis using Gd2O3-doped graphite rods. The procedure developed utilizes successive precipitation with the Lewis acids CaCl2 and ZnCl2 followed by treatment with amino-functionalized silica gel. The structure of the product was identified by single-crystal X-ray diffraction.