期刊
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
卷 130, 期 42, 页码 13996-13999出版社
AMER CHEMICAL SOC
DOI: 10.1021/ja805579m
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We put ammonia into an open-cage fullerene with a 20-membered ring (1) as the orifice and examined the properties of the complex using NMR and MALDI-TOF mass spectroscopy. The proton NMR shows a broad resonance corresponding to endohedral NH3 at delta(H) = -12.3 ppm relative to TMS. This resonance was seen to narrow when a N-14 decoupling frequency was applied. MALDI spectroscopy confirmed the presence of both 1 (m/z = 1172) and 1 + NH3 (m/z = 1189), and integrated intensities of MALDI peak trains and NMR resonances indicate an incorporation fraction of 35-50% under our experimental conditions. NMR observations showed a diminished incorporation fraction after 6 months of storage at -10 degrees C, which indicates that ammonia slowly escapes from the open-cage fullerene.
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