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Pré-Publication, Document De Travail Année : 2024

Making 1H-1H couplings more accessible and accurate with selective 2DJ NMR experiments aided by 13C satellites

Résumé

1H-1H coupling constants are one of the primary sources of information for NMR structural analysis. Several selective 2DJ experiments have been proposed that allow their individual measurement at pure shift resolution. However, all these experiments fail in the not uncommon case when coupled protons have very close chemical shifts. Firstly, the coupling between protons with overlapping multiplets is inaccessible due to the inability of a frequency-selective pulse to invert just one of them. Secondly, the strong coupling condition affects the accuracy of coupling measurements involving third spins. These shortcomings impose a limit on the effectiveness of state-of-the-art experiments, such as G-SERF or PSYCHEDELIC. Here, we introduce two new and complementary selective 2DJ experiments that we coin SERFBIRD and SATASERF. These experiments overcome the aforementioned issues by utilizing the 13C satellite signals at natural isotope abundance, which resolve the chemical shift degeneracy. We demonstrate the utility of these experiments on the tetrasaccharide stachyose and the challenging case of norcamphor, for the latter achieving measurement of all JHH couplings while only few were accessible with PSYCHEDELIC. The new experiments are applicable to any organic compound and will prove valuable for configurational and conformational analyses.
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Licence : CC BY - Paternité
Licence : CC BY - Paternité

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hal-04438247 , version 1 (05-02-2024)

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François-Xavier Cantrelle, Emmanuelle Boll, Davy Sinnaeve. Making 1H-1H couplings more accessible and accurate with selective 2DJ NMR experiments aided by 13C satellites. 2024. ⟨hal-04438247⟩
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