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Measurement of 14N Quadrupole Couplings in Biomolecular Solids Using Indirect-Detection 14N Solid-State NMR with DNP

Measurement of 14N Quadrupole Couplings in Biomolecular Solids Using Indirect-Detection 14N Solid-State NMR with DNP
Measurement of 14N Quadrupole Couplings in Biomolecular Solids Using Indirect-Detection 14N Solid-State NMR with DNP
The quadrupolar interaction experienced by the spin-1 14N nucleus is known to be extremely sensitive to local structure and dynamics. Furthermore, the 14N isotope is 99.6% naturally abundant, making it an attractive target for characterisation of nitrogen-rich biological molecules by solid-state NMR. In this study, dynamic nuclear polarization (DNP) is used in conjunction with indirect 14N detected solid-state NMR experiments to simultaneously characterise the quadrupolar interaction at multiple 14N sites in the backbone of the microcrystalline protein, GB3. Considerable variation in the quadrupolar interaction (>700 kHz) is observed throughout the protein backbone. The distribution in quadrupolar interactions observed reports on the variation in local backbone conformation and subtle differences in hydrogen-bonding; demonstrating a new route to the structural and dynamic analysis of biomolecules.
1359-7345
12116-12119
Jarvis, James
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Haies, Ibraheem
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Lelli, Moreno
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Rossini, Aaron
b247b70f-8111-4392-994f-e9e32e7b2cb4
Kuprov, Ilya
bb07f28a-5038-4524-8146-e3fc8344c065
Carravetta, Marina
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Williamson, Philip
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Jarvis, James
59de8efd-053f-49da-80b4-8df7b74fa325
Haies, Ibraheem
f27584b7-74d7-4d07-af1d-3cd9333cf101
Lelli, Moreno
4a9fb9fb-d8f5-41c3-b280-30e7ca814538
Rossini, Aaron
b247b70f-8111-4392-994f-e9e32e7b2cb4
Kuprov, Ilya
bb07f28a-5038-4524-8146-e3fc8344c065
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Williamson, Philip
0b7715c6-b60e-4e95-a1b1-6afc8b9f372a

Jarvis, James, Haies, Ibraheem, Lelli, Moreno, Rossini, Aaron, Kuprov, Ilya, Carravetta, Marina and Williamson, Philip (2017) Measurement of 14N Quadrupole Couplings in Biomolecular Solids Using Indirect-Detection 14N Solid-State NMR with DNP. Chemical Communications, 53 (89), 12116-12119. (doi:10.1039/c7cc03462h).

Record type: Article

Abstract

The quadrupolar interaction experienced by the spin-1 14N nucleus is known to be extremely sensitive to local structure and dynamics. Furthermore, the 14N isotope is 99.6% naturally abundant, making it an attractive target for characterisation of nitrogen-rich biological molecules by solid-state NMR. In this study, dynamic nuclear polarization (DNP) is used in conjunction with indirect 14N detected solid-state NMR experiments to simultaneously characterise the quadrupolar interaction at multiple 14N sites in the backbone of the microcrystalline protein, GB3. Considerable variation in the quadrupolar interaction (>700 kHz) is observed throughout the protein backbone. The distribution in quadrupolar interactions observed reports on the variation in local backbone conformation and subtle differences in hydrogen-bonding; demonstrating a new route to the structural and dynamic analysis of biomolecules.

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Accepted/In Press date: 15 August 2017
e-pub ahead of print date: 26 August 2017
Published date: 18 November 2017

Identifiers

Local EPrints ID: 413886
URI: https://eprints.soton.ac.uk/id/eprint/413886
ISSN: 1359-7345
PURE UUID: 49b8e776-1bb8-4455-8c22-64bbb40f6a39
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: 08 Sep 2017 16:30
Last modified: 10 Sep 2019 04:44

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Contributors

Author: James Jarvis
Author: Ibraheem Haies
Author: Moreno Lelli
Author: Aaron Rossini
Author: Ilya Kuprov ORCID iD

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