Measuring 19F shift anisotropies and 1H–19F dipolar interactions with ultrafast MAS NMR

A new 19F anisotropic–isotropic shift correlation experiment is described that operates with ultrafast MAS, resulting in good resolution of isotropic 19F shifts in the detection dimension. The new experiment makes use of a recoupling sequence designed using symmetry principles that reintroduces the...

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Main Authors: Martini, Francesca, Miah, Habeeba K., Iuga, Dinu, Geppi, Marco, Titman, Jeremy J.
Format: Article
Published: Elsevier 2015
Subjects:
Online Access:https://eprints.nottingham.ac.uk/30389/
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author Martini, Francesca
Miah, Habeeba K.
Iuga, Dinu
Geppi, Marco
Titman, Jeremy J.
author_facet Martini, Francesca
Miah, Habeeba K.
Iuga, Dinu
Geppi, Marco
Titman, Jeremy J.
author_sort Martini, Francesca
building Nottingham Research Data Repository
collection Online Access
description A new 19F anisotropic–isotropic shift correlation experiment is described that operates with ultrafast MAS, resulting in good resolution of isotropic 19F shifts in the detection dimension. The new experiment makes use of a recoupling sequence designed using symmetry principles that reintroduces the 19F chemical shift anisotropy in the indirect dimension. The situations in which the new experiment is appropriate are discussed, and the 19F shift anisotropy parameters in poly(difluoroethylene) (PVDF) are measured. In addition, similar recoupling sequences are shown to be effective for measuring 1H–19F distances via the heteronuclear dipolar interaction. This is demonstrated by application to a recently synthesized zirconium phosphonate material that contains one-dimensional chains linked by H–F hydrogen bonds.
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spelling nottingham-303892020-05-04T17:15:55Z https://eprints.nottingham.ac.uk/30389/ Measuring 19F shift anisotropies and 1H–19F dipolar interactions with ultrafast MAS NMR Martini, Francesca Miah, Habeeba K. Iuga, Dinu Geppi, Marco Titman, Jeremy J. A new 19F anisotropic–isotropic shift correlation experiment is described that operates with ultrafast MAS, resulting in good resolution of isotropic 19F shifts in the detection dimension. The new experiment makes use of a recoupling sequence designed using symmetry principles that reintroduces the 19F chemical shift anisotropy in the indirect dimension. The situations in which the new experiment is appropriate are discussed, and the 19F shift anisotropy parameters in poly(difluoroethylene) (PVDF) are measured. In addition, similar recoupling sequences are shown to be effective for measuring 1H–19F distances via the heteronuclear dipolar interaction. This is demonstrated by application to a recently synthesized zirconium phosphonate material that contains one-dimensional chains linked by H–F hydrogen bonds. Elsevier 2015-10-01 Article PeerReviewed Martini, Francesca, Miah, Habeeba K., Iuga, Dinu, Geppi, Marco and Titman, Jeremy J. (2015) Measuring 19F shift anisotropies and 1H–19F dipolar interactions with ultrafast MAS NMR. Journal of Magnetic Resonance, 259 . pp. 102-107. ISSN 1090-7807 Chemical shift anisotropy; Ultrafast magic angle spinning; Anisotropic–isotropic shift correlation; Symmetry-based recoupling sequence; Heteronuclear dipolar coupling; Dipole-shift correlation http://www.sciencedirect.com/science/article/pii/S109078071500169X doi:10.1016/j.jmr.2015.08.004 doi:10.1016/j.jmr.2015.08.004
spellingShingle Chemical shift anisotropy; Ultrafast magic angle spinning; Anisotropic–isotropic shift correlation; Symmetry-based recoupling sequence; Heteronuclear dipolar coupling; Dipole-shift correlation
Martini, Francesca
Miah, Habeeba K.
Iuga, Dinu
Geppi, Marco
Titman, Jeremy J.
Measuring 19F shift anisotropies and 1H–19F dipolar interactions with ultrafast MAS NMR
title Measuring 19F shift anisotropies and 1H–19F dipolar interactions with ultrafast MAS NMR
title_full Measuring 19F shift anisotropies and 1H–19F dipolar interactions with ultrafast MAS NMR
title_fullStr Measuring 19F shift anisotropies and 1H–19F dipolar interactions with ultrafast MAS NMR
title_full_unstemmed Measuring 19F shift anisotropies and 1H–19F dipolar interactions with ultrafast MAS NMR
title_short Measuring 19F shift anisotropies and 1H–19F dipolar interactions with ultrafast MAS NMR
title_sort measuring 19f shift anisotropies and 1h–19f dipolar interactions with ultrafast mas nmr
topic Chemical shift anisotropy; Ultrafast magic angle spinning; Anisotropic–isotropic shift correlation; Symmetry-based recoupling sequence; Heteronuclear dipolar coupling; Dipole-shift correlation
url https://eprints.nottingham.ac.uk/30389/
https://eprints.nottingham.ac.uk/30389/
https://eprints.nottingham.ac.uk/30389/