Production and isolation of Ca@C{sup 82} (I-IV) and Ca@C{sup 84} (I,II) metallofullerenes
- Nagoya Univ. (Japan)
Almost all of the metallofullerenes prepared so far have incorporated La, Y, and Sc or several lanthanide elements such as Gd and Pr. The endohederal structures of Y@C{sup 82} and Sc{sup 2}@C{sup 84} have been finally confirmed by recent synchrotron X-ray powder diffraction and {sup 13}C NMR studies, respectively. This paper reports the first production, isolation, and spectroscopic study on several structural isomers of Ca@C{sup 82} and Ca@C{sup 84}. The details of the production and separation/isolation of endohedral metallofullerenes have been described elsewhere. Briefly, soot-containing Ca@C{sup 82}, Ca@C{sup 84}, and other calcium metallofullerenes was produced in direct-current (350-400 A) arc-discharge of a calcium/graphite composite rod (Toyo Tanso Co. Ltd., 12.5 x 12.5 x 240 mm, 0.3 atomic %) under He flow (8-10 L/min) at 50 Torr. The soot was collected under totally anaerobic conditions and was extracted by CS{sup 2}. The Ca@C{sup 82} and Ca@C{sup 84} fullerenes were separated by the two-stage high-performance liquid chromatography (HPLC) method. The retention times of the present isomers are very close to each other; therefore the final isolation of the isomers was achieved by recycling (2-9 times) the HPLC process to increase the resolution. 23 refs., 3 figs.
- OSTI ID:
- 426233
- Journal Information:
- Journal of the American Chemical Society, Vol. 118, Issue 45; Other Information: PBD: 13 Nov 1996
- Country of Publication:
- United States
- Language:
- English
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