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Quantitative analysis of Q2 14N quadrupolar coupling using 1H detected 14N solid-state NMR†

Quantitative analysis of Q2 14N quadrupolar coupling using 1H detected 14N solid-state NMR†
Quantitative analysis of Q2 14N quadrupolar coupling using 1H detected 14N solid-state NMR†
Magic-angle spinning solid-state NMR is increasingly utilized to study the naturally abundant, spin-1 nucleus 14N, providing insights into the structure and dynamics of biological and organic molecules. In particular, the characterisation of 14N sites using indirect detection has proven useful for complex molecules, where the ‘spy’ nucleus provides enhanced sensitivity and resolution. Here we exploit the sensitivity of proton detection, to indirectly characterise 14N sites using a moderate rf field to generate coherence between the 1H and 14N at moderate and fast-magic-angle spinning frequencies. Efficient numerical simulations have been developed that have allowed us to quantitatively analyse the resulting 14N lineshapes to determine both the size and asymmetry of the quadrupolar interaction. Exploiting only naturally occurring abundant isotopes will aid the analysis of materials with the need to resort to isotope labelling, whilst providing additional insights into the structure and dynamics that the characterisation of the quadrupolar interaction affords.
1463-9076
5941-5949
Jarvis, James
0992a573-1255-4f1c-9111-8027528acb77
Concistre, Maria
ec95c9d4-ecb8-4c28-a464-8c3adba9e86d
Haies, Ibraheem
f27584b7-74d7-4d07-af1d-3cd9333cf101
Bounds, Richard
3f108fd4-8375-4d0d-8718-e8be7a0ef7f7
Kuprov, Ilya
bb07f28a-5038-4524-8146-e3fc8344c065
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Williamson, Philip
0b7715c6-b60e-4e95-a1b1-6afc8b9f372a
Jarvis, James
0992a573-1255-4f1c-9111-8027528acb77
Concistre, Maria
ec95c9d4-ecb8-4c28-a464-8c3adba9e86d
Haies, Ibraheem
f27584b7-74d7-4d07-af1d-3cd9333cf101
Bounds, Richard
3f108fd4-8375-4d0d-8718-e8be7a0ef7f7
Kuprov, Ilya
bb07f28a-5038-4524-8146-e3fc8344c065
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Williamson, Philip
0b7715c6-b60e-4e95-a1b1-6afc8b9f372a

Jarvis, James, Concistre, Maria, Haies, Ibraheem, Bounds, Richard, Kuprov, Ilya, Carravetta, Marina and Williamson, Philip (2019) Quantitative analysis of Q2 14N quadrupolar coupling using 1H detected 14N solid-state NMR†. Physical Chemistry Chemical Physics, 21 (11), 5941-5949. (doi:10.1039/C8CP06276E).

Record type: Article

Abstract

Magic-angle spinning solid-state NMR is increasingly utilized to study the naturally abundant, spin-1 nucleus 14N, providing insights into the structure and dynamics of biological and organic molecules. In particular, the characterisation of 14N sites using indirect detection has proven useful for complex molecules, where the ‘spy’ nucleus provides enhanced sensitivity and resolution. Here we exploit the sensitivity of proton detection, to indirectly characterise 14N sites using a moderate rf field to generate coherence between the 1H and 14N at moderate and fast-magic-angle spinning frequencies. Efficient numerical simulations have been developed that have allowed us to quantitatively analyse the resulting 14N lineshapes to determine both the size and asymmetry of the quadrupolar interaction. Exploiting only naturally occurring abundant isotopes will aid the analysis of materials with the need to resort to isotope labelling, whilst providing additional insights into the structure and dynamics that the characterisation of the quadrupolar interaction affords.

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C8CP06276E_PTW - Accepted Manuscript
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More information

Accepted/In Press date: 29 January 2019
e-pub ahead of print date: 27 February 2019
Published date: 21 March 2019

Identifiers

Local EPrints ID: 428122
URI: http://eprints.soton.ac.uk/id/eprint/428122
ISSN: 1463-9076
PURE UUID: a880bee3-6ee7-4b0a-b054-113c83405776
ORCID for Ilya Kuprov: ORCID iD orcid.org/0000-0003-0430-2682
ORCID for Marina Carravetta: ORCID iD orcid.org/0000-0002-6296-2104
ORCID for Philip Williamson: ORCID iD orcid.org/0000-0002-0231-8640

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Date deposited: 12 Feb 2019 17:30
Last modified: 15 Sep 2021 05:22

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