Observation of 1H-1H J-couplings in fast magic-angle-spinning solid-state NMR spectroscopy
Abstract 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....
Saved in:
| Main Authors: | , , , , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
Nature Portfolio
2024-12-01
|
| Series: | Nature Communications |
| Online Access: | https://doi.org/10.1038/s41467-024-55126-9 |
| Tags: |
Add Tag
No Tags, Be the first to tag this record!
|
| _version_ | 1841559290250264576 |
|---|---|
| author | Daria Torodii Jacob B. Holmes Kristof Grohe Rodrigo de Oliveira-Silva Sebastian Wegner Dimitrios Sakellariou Lyndon Emsley |
| author_facet | Daria Torodii Jacob B. Holmes Kristof Grohe Rodrigo de Oliveira-Silva Sebastian Wegner Dimitrios Sakellariou Lyndon Emsley |
| author_sort | Daria Torodii |
| collection | DOAJ |
| description | Abstract 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. |
| format | Article |
| id | doaj-art-77a24ff20186491dac62a6d606149020 |
| institution | Kabale University |
| issn | 2041-1723 |
| language | English |
| publishDate | 2024-12-01 |
| publisher | Nature Portfolio |
| record_format | Article |
| series | Nature Communications |
| spelling | doaj-art-77a24ff20186491dac62a6d6061490202025-01-05T12:36:23ZengNature PortfolioNature Communications2041-17232024-12-011511610.1038/s41467-024-55126-9Observation of 1H-1H J-couplings in fast magic-angle-spinning solid-state NMR spectroscopyDaria Torodii0Jacob B. Holmes1Kristof Grohe2Rodrigo de Oliveira-Silva3Sebastian Wegner4Dimitrios Sakellariou5Lyndon Emsley6Institut des Sciences et Ingénierie Chimiques, École Polytechnique Fédérale de Lausanne (EPFL)Institut des Sciences et Ingénierie Chimiques, École Polytechnique Fédérale de Lausanne (EPFL)Bruker BioSpin GmbH & Co KGKU Leuven, M2S, cMACS, Celestijnenlaan 200FBruker BioSpin GmbH & Co KGKU Leuven, M2S, cMACS, Celestijnenlaan 200FInstitut des Sciences et Ingénierie Chimiques, École Polytechnique Fédérale de Lausanne (EPFL)Abstract 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.https://doi.org/10.1038/s41467-024-55126-9 |
| spellingShingle | Daria Torodii Jacob B. Holmes Kristof Grohe Rodrigo de Oliveira-Silva Sebastian Wegner Dimitrios Sakellariou Lyndon Emsley Observation of 1H-1H J-couplings in fast magic-angle-spinning solid-state NMR spectroscopy Nature Communications |
| title | Observation of 1H-1H J-couplings in fast magic-angle-spinning solid-state NMR spectroscopy |
| title_full | Observation of 1H-1H J-couplings in fast magic-angle-spinning solid-state NMR spectroscopy |
| title_fullStr | Observation of 1H-1H J-couplings in fast magic-angle-spinning solid-state NMR spectroscopy |
| title_full_unstemmed | Observation of 1H-1H J-couplings in fast magic-angle-spinning solid-state NMR spectroscopy |
| title_short | Observation of 1H-1H J-couplings in fast magic-angle-spinning solid-state NMR spectroscopy |
| title_sort | observation of 1h 1h j couplings in fast magic angle spinning solid state nmr spectroscopy |
| url | https://doi.org/10.1038/s41467-024-55126-9 |
| work_keys_str_mv | AT dariatorodii observationof1h1hjcouplingsinfastmagicanglespinningsolidstatenmrspectroscopy AT jacobbholmes observationof1h1hjcouplingsinfastmagicanglespinningsolidstatenmrspectroscopy AT kristofgrohe observationof1h1hjcouplingsinfastmagicanglespinningsolidstatenmrspectroscopy AT rodrigodeoliveirasilva observationof1h1hjcouplingsinfastmagicanglespinningsolidstatenmrspectroscopy AT sebastianwegner observationof1h1hjcouplingsinfastmagicanglespinningsolidstatenmrspectroscopy AT dimitriossakellariou observationof1h1hjcouplingsinfastmagicanglespinningsolidstatenmrspectroscopy AT lyndonemsley observationof1h1hjcouplingsinfastmagicanglespinningsolidstatenmrspectroscopy |