Journal
INTERNATIONAL JOURNAL OF MASS SPECTROMETRY
Volume 210, Issue 1-3, Pages 241-247Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/S1387-3806(01)00420-1
Keywords
endohedral fullerenes; high-temperature high-pressure incorporation; MIKEs
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Several new diatomic molecule-containing endohedral fullerenes were prepared by heating C,,,, or C, under high pressures of the corresponding gases. The species prepared are N-2@C-60, N-2@C-70, (CO)-C-13@C-60, and (HeNe)-He-3-Ne-22@C-70. Their existence was demonstrated through high sensitivity, wide dynamic range mass spectrometry. Out of two thousand C-60 molecules about one is observed to incorporate N-2. The nitrogen molecule containing endohedral molecules are stable and the mass spectrometric signal is not lost even after several hours heating at 500 K. The corresponding endohedral ions undergo the Rice shrink-wrap mechanism; a mass-analyzed ion kinetic energy spectrum demonstrates the loss of a C, unit from the cage. The observation of (CO)-C-13@C-60 by mass spectrometry opens up the possibility for future NMR studies of this molecule. The observation of (HeNe)-He-3-Ne-22@C-70 is in accordance with the promoter mechanism of Thiel and co-worker [J. Am. Chem. Soc. 118 (1996) 7164 Helv. Chim. Acta 80 (1997) 495], whereby the singly and doubly occupied fullerenes are in equilibrium but the empty and filled fullerenes are not. (C) 2001 Elsevier Science B.V.
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