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Direct detection of hydrogen bonds in supramolecular systems using 1H– 15N Heteronuclear Multiple Quantum Coherence Spectroscopy

Direct detection of hydrogen bonds in supramolecular systems using 1H– 15N Heteronuclear Multiple Quantum Coherence Spectroscopy
Direct detection of hydrogen bonds in supramolecular systems using 1H– 15N Heteronuclear Multiple Quantum Coherence Spectroscopy
Hydrogen-bonded supramolecular systems are usually characterized in solution through analysis of NMR data such as complexation-induced shifts and nuclear Overhauser effects (nOe). Routine direct detection of hydrogen bonding particularly in multicomponent mixtures, even with the aid of 2D NMR experiments for full assignment, is more challenging. We describe an elementary rapid 1H-15N HMQC NMR experiment which addresses these challenges without the need for complex pulse sequences. Under readily accessible conditions (243/263 K, 50 mM solutions) and natural 15N abundance, unambiguous assignment of 15N resonances facilitates direct detection of intra- and intermolecular hydrogen bonds in mechanically interlocked structures and quadruply hydrogen-bonded dimers-of dialkylaminoureidopyrimidinones, ureidopyrimidinones, and diamidonaphthyridines-in single or multicomponent mixtures to establish tautomeric configuration, conformation, and, to resolve self-sorted speciation.
0002-7863
23127-23133
Jinks, Michael A.
c8ce33cc-8ead-4763-b294-ae94ce0475d0
Howard, Mark
8182d6ac-b787-443a-bcb9-1182fd973254
Rizzi, Federica
f05be5f8-7711-4796-9cd3-9fa5b238ea3e
Goldup, Stephen M.
0a93eedd-98bb-42c1-a963-e2815665e937
Burnett, Andrew D.
00650f69-922f-47ae-9105-c9c86f094913
Wilson, Andrew J.
673697c0-09c0-4aed-87a4-7ca1f1f44a15
Jinks, Michael A.
c8ce33cc-8ead-4763-b294-ae94ce0475d0
Howard, Mark
8182d6ac-b787-443a-bcb9-1182fd973254
Rizzi, Federica
f05be5f8-7711-4796-9cd3-9fa5b238ea3e
Goldup, Stephen M.
0a93eedd-98bb-42c1-a963-e2815665e937
Burnett, Andrew D.
00650f69-922f-47ae-9105-c9c86f094913
Wilson, Andrew J.
673697c0-09c0-4aed-87a4-7ca1f1f44a15

Jinks, Michael A., Howard, Mark, Rizzi, Federica, Goldup, Stephen M., Burnett, Andrew D. and Wilson, Andrew J. (2022) Direct detection of hydrogen bonds in supramolecular systems using 1H– 15N Heteronuclear Multiple Quantum Coherence Spectroscopy. Journal of the American Chemical Society, 144 (50), 23127-23133. (doi:10.1021/jacs.2c10742).

Record type: Article

Abstract

Hydrogen-bonded supramolecular systems are usually characterized in solution through analysis of NMR data such as complexation-induced shifts and nuclear Overhauser effects (nOe). Routine direct detection of hydrogen bonding particularly in multicomponent mixtures, even with the aid of 2D NMR experiments for full assignment, is more challenging. We describe an elementary rapid 1H-15N HMQC NMR experiment which addresses these challenges without the need for complex pulse sequences. Under readily accessible conditions (243/263 K, 50 mM solutions) and natural 15N abundance, unambiguous assignment of 15N resonances facilitates direct detection of intra- and intermolecular hydrogen bonds in mechanically interlocked structures and quadruply hydrogen-bonded dimers-of dialkylaminoureidopyrimidinones, ureidopyrimidinones, and diamidonaphthyridines-in single or multicomponent mixtures to establish tautomeric configuration, conformation, and, to resolve self-sorted speciation.

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More information

e-pub ahead of print date: 12 December 2022
Published date: 21 December 2022
Additional Information: Funding Information: This work was supported by the EPSRC EP/T011726/1, EP/P007449/1 (a fellowship awarded to A.D.B.), and ERC grant 724987 (awarded to S.M.G.). Publisher Copyright: © 2022 The Authors. Published by American Chemical Society.

Identifiers

Local EPrints ID: 475703
URI: http://eprints.soton.ac.uk/id/eprint/475703
ISSN: 0002-7863
PURE UUID: 6a329349-161b-4825-8f0e-267115db19b8
ORCID for Stephen M. Goldup: ORCID iD orcid.org/0000-0003-3781-0464

Catalogue record

Date deposited: 24 Mar 2023 18:20
Last modified: 05 Jun 2024 19:13

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Contributors

Author: Michael A. Jinks
Author: Mark Howard
Author: Federica Rizzi
Author: Andrew D. Burnett
Author: Andrew J. Wilson

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