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research article

Barriers to resolution in 1H NMR of rotating solids

de Almeida, Bruno Simoes
•
Torodii, Daria  
•
Moutzouri, Pinelopi  
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September 28, 2023
Journal of Magnetic Resonance

The role of 1H solid-state NMR in structure elucidation of solids is becoming more preponderant, particularly as faster magic-angle spinning rates (MAS) become available which improve 1H detected assignment strategies. However, current 1H spectral resolution is still relatively poor, with linewidths of typically a few hundred Hz, even at the fastest rates available today. Here we detail and assess the factors limiting proton linewidths and line shapes in MAS experiments with five different samples, exemplifying the different sources of broadening that affect the residual linewidth. We disentangle the different contributions through one-and two-dimensional ex-periments: by using dilution to identify the contribution of ABMS; by using extensive deuteration to identify the dipolar contributions; and by using variable MAS rates to determine the ratio between homogeneous and inhomogeneous components. We find that the overall widths and the nature of the different contributions to the linewidths can vary very considerably. While we find that faster spinning always yields narrower lines and longer coherence lifetimes, we also find that for some resonances the dipolar contribution is no longer dominant at 100 kHz MAS. When the inhomogeneous sources of broadening, such as ABMS and chemical shift disorder, are dominant, two-dimensional 1H-1H correlation experiments yield better resolution for assignment. Particularly the extraction of the antidiagonal of a 2D peak will remove any correlated inhomogeneous broadening, giving substantially narrower 1H linewidths.

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Type
research article
DOI
10.1016/j.jmr.2023.107557
Web of Science ID

WOS:001097473200001

Author(s)
de Almeida, Bruno Simoes
Torodii, Daria  
Moutzouri, Pinelopi  
Emsley, Lyndon  
Date Issued

2023-09-28

Publisher

Academic Press Inc - Elsevier Science

Published in
Journal of Magnetic Resonance
Volume

355

Article Number

107557

Subjects

Life Sciences & Biomedicine

•

Physical Sciences

•

Technology

•

Solid-State Nmr

•

Magic Angle Spinning

•

1 H Resolution

•

Magnetic Susceptibility

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Chemical Disorder

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Organic Solids

Editorial or Peer reviewed

REVIEWED

Written at

EPFL

EPFL units
LRM  
FunderGrant Number

Swiss National Science Foundation

200020_212046

European Union

101008500

Available on Infoscience
February 19, 2024
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/204167
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