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Homonuclear Decoupling in (1)H NMR of Solids by Remote Correlation

The typical linewidths of (1)H NMR spectra of powdered organic solids at 111 kHz magic‐angle spinning (MAS) are of the order of a few hundred Hz. While this is remarkable in comparison to the tens of kHz observed in spectra of static samples, it is still the key limit to the use of (1)H in solid‐sta...

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Autores principales: Moutzouri, Pinelopi, Paruzzo, Federico M., Simões de Almeida, Bruno, Stevanato, Gabriele, Emsley, Lyndon
Formato: Online Artículo Texto
Lenguaje:English
Publicado: John Wiley and Sons Inc. 2020
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7187420/
https://www.ncbi.nlm.nih.gov/pubmed/31967378
http://dx.doi.org/10.1002/anie.201916335
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author Moutzouri, Pinelopi
Paruzzo, Federico M.
Simões de Almeida, Bruno
Stevanato, Gabriele
Emsley, Lyndon
author_facet Moutzouri, Pinelopi
Paruzzo, Federico M.
Simões de Almeida, Bruno
Stevanato, Gabriele
Emsley, Lyndon
author_sort Moutzouri, Pinelopi
collection PubMed
description The typical linewidths of (1)H NMR spectra of powdered organic solids at 111 kHz magic‐angle spinning (MAS) are of the order of a few hundred Hz. While this is remarkable in comparison to the tens of kHz observed in spectra of static samples, it is still the key limit to the use of (1)H in solid‐state NMR, especially for complex systems. Here, we demonstrate a novel strategy to further improve the spectral resolution. We show that the anti‐z‐COSY experiment can be used to reduce the residual line broadening of (1)H NMR spectra of powdered organic solids. Results obtained with the anti‐z‐COSY sequence at 100 kHz MAS on thymol, β‐AspAla, and strychnine show an improvement in resolution of up to a factor of two compared to conventional spectra acquired at the same spinning rate.
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spelling pubmed-71874202020-04-28 Homonuclear Decoupling in (1)H NMR of Solids by Remote Correlation Moutzouri, Pinelopi Paruzzo, Federico M. Simões de Almeida, Bruno Stevanato, Gabriele Emsley, Lyndon Angew Chem Int Ed Engl Communications The typical linewidths of (1)H NMR spectra of powdered organic solids at 111 kHz magic‐angle spinning (MAS) are of the order of a few hundred Hz. While this is remarkable in comparison to the tens of kHz observed in spectra of static samples, it is still the key limit to the use of (1)H in solid‐state NMR, especially for complex systems. Here, we demonstrate a novel strategy to further improve the spectral resolution. We show that the anti‐z‐COSY experiment can be used to reduce the residual line broadening of (1)H NMR spectra of powdered organic solids. Results obtained with the anti‐z‐COSY sequence at 100 kHz MAS on thymol, β‐AspAla, and strychnine show an improvement in resolution of up to a factor of two compared to conventional spectra acquired at the same spinning rate. John Wiley and Sons Inc. 2020-02-19 2020-04-06 /pmc/articles/PMC7187420/ /pubmed/31967378 http://dx.doi.org/10.1002/anie.201916335 Text en © 2020 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA. This is an open access article under the terms of the http://creativecommons.org/licenses/by-nc/4.0/ License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited and is not used for commercial purposes.
spellingShingle Communications
Moutzouri, Pinelopi
Paruzzo, Federico M.
Simões de Almeida, Bruno
Stevanato, Gabriele
Emsley, Lyndon
Homonuclear Decoupling in (1)H NMR of Solids by Remote Correlation
title Homonuclear Decoupling in (1)H NMR of Solids by Remote Correlation
title_full Homonuclear Decoupling in (1)H NMR of Solids by Remote Correlation
title_fullStr Homonuclear Decoupling in (1)H NMR of Solids by Remote Correlation
title_full_unstemmed Homonuclear Decoupling in (1)H NMR of Solids by Remote Correlation
title_short Homonuclear Decoupling in (1)H NMR of Solids by Remote Correlation
title_sort homonuclear decoupling in (1)h nmr of solids by remote correlation
topic Communications
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7187420/
https://www.ncbi.nlm.nih.gov/pubmed/31967378
http://dx.doi.org/10.1002/anie.201916335
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