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Modest Offset Difference Internuclear Selective Transfer via Homonuclear Dipolar Coupling

[Image: see text] Homonuclear dipolar recoupling is routinely used for magic-angle spinning NMR-based structure determination. In fully protonated samples, only short proton–proton distances are accessible to broadband recoupling approaches because of high proton density. Selective methods allow det...

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Autores principales: Nimerovsky, Evgeny, Najbauer, Eszter E., Movellan, Kumar Tekwani, Xue, Kai, Becker, Stefan, Andreas, Loren B.
Formato: Online Artículo Texto
Lenguaje:English
Publicado: American Chemical Society 2022
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8859849/
https://www.ncbi.nlm.nih.gov/pubmed/35133845
http://dx.doi.org/10.1021/acs.jpclett.1c03871
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author Nimerovsky, Evgeny
Najbauer, Eszter E.
Movellan, Kumar Tekwani
Xue, Kai
Becker, Stefan
Andreas, Loren B.
author_facet Nimerovsky, Evgeny
Najbauer, Eszter E.
Movellan, Kumar Tekwani
Xue, Kai
Becker, Stefan
Andreas, Loren B.
author_sort Nimerovsky, Evgeny
collection PubMed
description [Image: see text] Homonuclear dipolar recoupling is routinely used for magic-angle spinning NMR-based structure determination. In fully protonated samples, only short proton–proton distances are accessible to broadband recoupling approaches because of high proton density. Selective methods allow detection of longer distances by directing polarization to a subset of spins. Here we introduce the selective pulse sequence MODIST, which recouples spins that have a modest chemical shift offset difference, and demonstrate it to selectively record correlations between amide protons. The sequence was selected for good retention of total signal, leading to up to twice the intensity for proton–proton correlations compared with other selective methods. The sequence is effective across a range of spinning conditions and magnetic fields, here tested at 55.555 and 100 kHz magic-angle spinning and at proton Larmor frequencies from 600 to 1200 MHz. For influenza A M2 in lipid bilayers, cross-peaks characteristic of a helical conformation are observed.
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spelling pubmed-88598492022-02-22 Modest Offset Difference Internuclear Selective Transfer via Homonuclear Dipolar Coupling Nimerovsky, Evgeny Najbauer, Eszter E. Movellan, Kumar Tekwani Xue, Kai Becker, Stefan Andreas, Loren B. J Phys Chem Lett [Image: see text] Homonuclear dipolar recoupling is routinely used for magic-angle spinning NMR-based structure determination. In fully protonated samples, only short proton–proton distances are accessible to broadband recoupling approaches because of high proton density. Selective methods allow detection of longer distances by directing polarization to a subset of spins. Here we introduce the selective pulse sequence MODIST, which recouples spins that have a modest chemical shift offset difference, and demonstrate it to selectively record correlations between amide protons. The sequence was selected for good retention of total signal, leading to up to twice the intensity for proton–proton correlations compared with other selective methods. The sequence is effective across a range of spinning conditions and magnetic fields, here tested at 55.555 and 100 kHz magic-angle spinning and at proton Larmor frequencies from 600 to 1200 MHz. For influenza A M2 in lipid bilayers, cross-peaks characteristic of a helical conformation are observed. American Chemical Society 2022-02-08 2022-02-17 /pmc/articles/PMC8859849/ /pubmed/35133845 http://dx.doi.org/10.1021/acs.jpclett.1c03871 Text en © 2022 The Authors. Published by American Chemical Society https://creativecommons.org/licenses/by/4.0/Permits the broadest form of re-use including for commercial purposes, provided that author attribution and integrity are maintained (https://creativecommons.org/licenses/by/4.0/).
spellingShingle Nimerovsky, Evgeny
Najbauer, Eszter E.
Movellan, Kumar Tekwani
Xue, Kai
Becker, Stefan
Andreas, Loren B.
Modest Offset Difference Internuclear Selective Transfer via Homonuclear Dipolar Coupling
title Modest Offset Difference Internuclear Selective Transfer via Homonuclear Dipolar Coupling
title_full Modest Offset Difference Internuclear Selective Transfer via Homonuclear Dipolar Coupling
title_fullStr Modest Offset Difference Internuclear Selective Transfer via Homonuclear Dipolar Coupling
title_full_unstemmed Modest Offset Difference Internuclear Selective Transfer via Homonuclear Dipolar Coupling
title_short Modest Offset Difference Internuclear Selective Transfer via Homonuclear Dipolar Coupling
title_sort modest offset difference internuclear selective transfer via homonuclear dipolar coupling
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8859849/
https://www.ncbi.nlm.nih.gov/pubmed/35133845
http://dx.doi.org/10.1021/acs.jpclett.1c03871
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