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14N overtone transition in double rotation solid-state NMR

14N overtone transition in double rotation solid-state NMR
14N overtone transition in double rotation solid-state NMR
Solid-state NMR transitions involving outer energy levels of the spin-1 14N nucleus are immune, to first order in perturbation theory, to the broadening caused by the nuclear quadrupole interaction. The corresponding overtone spectra, when acquired in conjunction with magic-angle sample spinning, result in lines, which are just a few kHz wide, permitting the direct detection of nitrogen compounds without the need for labeling. Despite the success of this technique, “overtone” resonances are still broadened due to indirect, second order effects arising from the large quadrupolar interaction. Here we demonstrate that another order of magnitude in spectral resolution may be gained by using double rotation. This brings the width of the 14N solid-state NMR lines much closer to the region commonly associated with high-resolution solid-state NMR spectroscopy of 15N and demonstrates the improvements in resolution that may be possible through the development of pulsed methodologies to suppress these second order effects.
1463-9076
23748-23753
Haies, Ibraheem M.
d14dce0d-4693-429a-8047-7770f3765d02
Jarvis, James A.
ff38f19b-7bfa-4361-b1ce-7cc7df510b92
Brown, Lynda J.
75aa95fa-5d27-46a7-9dbe-0f465a664f5b
Kuprov, Ilya
bb07f28a-5038-4524-8146-e3fc8344c065
Williamson, Philip T. F.
0b7715c6-b60e-4e95-a1b1-6afc8b9f372a
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Haies, Ibraheem M.
d14dce0d-4693-429a-8047-7770f3765d02
Jarvis, James A.
ff38f19b-7bfa-4361-b1ce-7cc7df510b92
Brown, Lynda J.
75aa95fa-5d27-46a7-9dbe-0f465a664f5b
Kuprov, Ilya
bb07f28a-5038-4524-8146-e3fc8344c065
Williamson, Philip T. F.
0b7715c6-b60e-4e95-a1b1-6afc8b9f372a
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691

Haies, Ibraheem M., Jarvis, James A., Brown, Lynda J., Kuprov, Ilya, Williamson, Philip T. F. and Carravetta, Marina (2015) 14N overtone transition in double rotation solid-state NMR. Physical Chemistry Chemical Physics, 17 (37), 23748-23753. (doi:10.1039/C5CP03266K).

Record type: Article

Abstract

Solid-state NMR transitions involving outer energy levels of the spin-1 14N nucleus are immune, to first order in perturbation theory, to the broadening caused by the nuclear quadrupole interaction. The corresponding overtone spectra, when acquired in conjunction with magic-angle sample spinning, result in lines, which are just a few kHz wide, permitting the direct detection of nitrogen compounds without the need for labeling. Despite the success of this technique, “overtone” resonances are still broadened due to indirect, second order effects arising from the large quadrupolar interaction. Here we demonstrate that another order of magnitude in spectral resolution may be gained by using double rotation. This brings the width of the 14N solid-state NMR lines much closer to the region commonly associated with high-resolution solid-state NMR spectroscopy of 15N and demonstrates the improvements in resolution that may be possible through the development of pulsed methodologies to suppress these second order effects.

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Accepted/In Press date: 4 August 2015
e-pub ahead of print date: 7 August 2015
Published date: 7 August 2015
Organisations: Chemistry

Identifiers

Local EPrints ID: 382234
URI: http://eprints.soton.ac.uk/id/eprint/382234
ISSN: 1463-9076
PURE UUID: 10bc3a66-7bd4-471c-a56b-388eca4474be
ORCID for Lynda J. Brown: ORCID iD orcid.org/0000-0002-5678-0814
ORCID for Ilya Kuprov: ORCID iD orcid.org/0000-0003-0430-2682
ORCID for Philip T. F. Williamson: ORCID iD orcid.org/0000-0002-0231-8640
ORCID for Marina Carravetta: ORCID iD orcid.org/0000-0002-6296-2104

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Date deposited: 27 Oct 2015 13:32
Last modified: 18 Feb 2021 17:19

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Contributors

Author: Ibraheem M. Haies
Author: James A. Jarvis
Author: Lynda J. Brown ORCID iD
Author: Ilya Kuprov ORCID iD

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