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Broadband measurement of true transverse relaxation rates in systems with coupled protons: application to the study of conformational exchange

Accurate measurement of transverse relaxation rates in coupled spin systems is important in the study of molecular dynamics, but is severely complicated by the signal modulations caused by scalar couplings in spin echo experiments. The most widely used experiments for measuring transverse relaxation...

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Autores principales: Kiraly, Peter, Dal Poggetto, Guilherme, Castañar, Laura, Nilsson, Mathias, Deák, Andrea, Morris, Gareth A.
Formato: Online Artículo Texto
Lenguaje:English
Publicado: The Royal Society of Chemistry 2021
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8447259/
https://www.ncbi.nlm.nih.gov/pubmed/34667556
http://dx.doi.org/10.1039/d1sc03391c
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author Kiraly, Peter
Dal Poggetto, Guilherme
Castañar, Laura
Nilsson, Mathias
Deák, Andrea
Morris, Gareth A.
author_facet Kiraly, Peter
Dal Poggetto, Guilherme
Castañar, Laura
Nilsson, Mathias
Deák, Andrea
Morris, Gareth A.
author_sort Kiraly, Peter
collection PubMed
description Accurate measurement of transverse relaxation rates in coupled spin systems is important in the study of molecular dynamics, but is severely complicated by the signal modulations caused by scalar couplings in spin echo experiments. The most widely used experiments for measuring transverse relaxation in coupled systems, CPMG and PROJECT, can suppress such modulations, but they also both suppress some relaxation contributions, and average relaxation rates between coupled spins. Here we introduce a new experiment which for the first time allows accurate broadband measurement of transverse relaxation rates of coupled protons, and hence the determination of exchange rate constants in slow exchange from relaxation measurements. The problems encountered with existing methods are illustrated, and the use of the new method is demonstrated for the classic case of hindered amide rotation and for the more challenging problem of exchange between helical enantiomers of a gold(i) complex.
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spelling pubmed-84472592021-10-18 Broadband measurement of true transverse relaxation rates in systems with coupled protons: application to the study of conformational exchange Kiraly, Peter Dal Poggetto, Guilherme Castañar, Laura Nilsson, Mathias Deák, Andrea Morris, Gareth A. Chem Sci Chemistry Accurate measurement of transverse relaxation rates in coupled spin systems is important in the study of molecular dynamics, but is severely complicated by the signal modulations caused by scalar couplings in spin echo experiments. The most widely used experiments for measuring transverse relaxation in coupled systems, CPMG and PROJECT, can suppress such modulations, but they also both suppress some relaxation contributions, and average relaxation rates between coupled spins. Here we introduce a new experiment which for the first time allows accurate broadband measurement of transverse relaxation rates of coupled protons, and hence the determination of exchange rate constants in slow exchange from relaxation measurements. The problems encountered with existing methods are illustrated, and the use of the new method is demonstrated for the classic case of hindered amide rotation and for the more challenging problem of exchange between helical enantiomers of a gold(i) complex. The Royal Society of Chemistry 2021-08-03 /pmc/articles/PMC8447259/ /pubmed/34667556 http://dx.doi.org/10.1039/d1sc03391c Text en This journal is © The Royal Society of Chemistry https://creativecommons.org/licenses/by/3.0/
spellingShingle Chemistry
Kiraly, Peter
Dal Poggetto, Guilherme
Castañar, Laura
Nilsson, Mathias
Deák, Andrea
Morris, Gareth A.
Broadband measurement of true transverse relaxation rates in systems with coupled protons: application to the study of conformational exchange
title Broadband measurement of true transverse relaxation rates in systems with coupled protons: application to the study of conformational exchange
title_full Broadband measurement of true transverse relaxation rates in systems with coupled protons: application to the study of conformational exchange
title_fullStr Broadband measurement of true transverse relaxation rates in systems with coupled protons: application to the study of conformational exchange
title_full_unstemmed Broadband measurement of true transverse relaxation rates in systems with coupled protons: application to the study of conformational exchange
title_short Broadband measurement of true transverse relaxation rates in systems with coupled protons: application to the study of conformational exchange
title_sort broadband measurement of true transverse relaxation rates in systems with coupled protons: application to the study of conformational exchange
topic Chemistry
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8447259/
https://www.ncbi.nlm.nih.gov/pubmed/34667556
http://dx.doi.org/10.1039/d1sc03391c
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