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research article

Observation of 1H-1H J-couplings in fast magic-angle-spinning solid-state NMR spectroscopy

Torodii, Daria  
•
Holmes, Jacob B.  
•
Grohe, Kristof
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December 30, 2024
Nature Communications

While 1H-1H J-couplings are the cornerstone of all spectral assignment methods in solution-state NMR, they are yet to be observed in solids. Here we observe 1H-1H J-couplings in plastic crystals of (1S)-(−)-camphor in solid-state NMR at magic angle spinning (MAS) rates of 100 kHz and above. This is enabled in this special case because the intrinsic coherence lifetimes at fast MAS rates become longer than the inverse of the 1H-1H J couplings. For example, at 160 kHz MAS the coherence lifetimes are longer than 20 ms, corresponding to refocused linewidths of less than 15 Hz. As a result, we are able to record two-dimensional 1H-1H J resolved spectra that allow the observation and measurement of 1H-1H J-couplings in solid camphor. The J-couplings also lead to unambiguous through-bond correlations in 1H-1H refocused incredible natural abundance double quantum transfer (INADEQUATE) and uniform-sign cross-peak double-quantum-filtered correlation spectroscopy (UC2QFCOSY) experiments.

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Type
research article
DOI
10.1038/s41467-024-55126-9
Scopus ID

2-s2.0-85213683062

Author(s)
Torodii, Daria  
Holmes, Jacob B.  
Grohe, Kristof
de Oliveira-Silva, Rodrigo
Wegner, Sebastian
Sakellariou, Dimitrios
Emsley, Lyndon  
Date Issued

2024-12-30

Publisher

Nature Research

Published in
Nature Communications
Volume

15

Article Number

10799

Editorial or Peer reviewed

REVIEWED

Written at

EPFL

EPFL units
LRM  
FunderFunding(s)Grant NumberGrant URL

Swiss National Science Foundation

200020_212046

KU Leuven

STG-18-00289

RelationRelated workURL/DOI

IsSupplementedBy

raw data and notebooks

https://zenodo.org/records/14186568
Available on Infoscience
January 10, 2025
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/242696
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