Direct detection of hydrogen bonds in supramolecular systems using 1H-15N Heteronuclear multiple quantum coherence spectroscopy

Michael A. Jinks, Mark Howard, Federica Rizzi, Stephen M. Goldup, Andrew D. Burnett, Andrew J. Wilson*

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

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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.

Original languageEnglish
Pages (from-to)23127-23133
Number of pages7
JournalJournal of the American Chemical Society
Volume144
Issue number50
Early online date12 Dec 2022
DOIs
Publication statusPublished - 21 Dec 2022

Bibliographical note

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.

ASJC Scopus subject areas

  • Catalysis
  • General Chemistry
  • Biochemistry
  • Colloid and Surface Chemistry

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