Putting Ammonia into a Chemically Opened Fullerene

Putting Ammonia into a Chemically Opened Fullerene

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 δH = −12.3 ppm relative to TMS. This resonance was see...

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Veröffentlicht in:Journal of the American Chemical Society 2008-10, Vol.130 (42), p.13996-13999
Hauptverfasser: Whitener, Keith E, Frunzi, Michael, Iwamatsu, Sho-ichi, Murata, Shizuaki, Cross, R. James, Saunders, Martin
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Sprache:eng
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Ammonia - chemistry
Fullerenes - chemistry
Magnetic Resonance Spectroscopy - methods
Magnetic Resonance Spectroscopy - standards
Molecular Conformation
Reference Standards
Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization - methods
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container_end_page 13999
container_issue 42
container_start_page 13996
container_title Journal of the American Chemical Society
container_volume 130
creator Whitener, Keith E
Frunzi, Michael
Iwamatsu, Sho-ichi
Murata, Shizuaki
Cross, R. James
Saunders, Martin
description 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 δH = −12.3 ppm relative to TMS. This resonance was seen to narrow when a 14N 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 °C, which indicates that ammonia slowly escapes from the open-cage fullerene.
doi_str_mv 10.1021/ja805579m
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subjects Ammonia - chemistry
Fullerenes - chemistry
Magnetic Resonance Spectroscopy - methods
Magnetic Resonance Spectroscopy - standards
Molecular Conformation
Reference Standards
Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization - methods
title Putting Ammonia into a Chemically Opened Fullerene
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