Titre :

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

Auteur(s) :

Cantrelle, François-Xavier [Auteur]
Biologie Structurale Intégrative [ERL 9002 - INSERM U1167 - BSI]
Facteurs de Risque et Déterminants Moléculaires des Maladies liées au Vieillissement - U 1167 [RID-AGE]
Boll, Emmanuelle [Auteur]
Biologie Structurale Intégrative [ERL 9002 - INSERM U1167 - BSI]
Facteurs de Risque et Déterminants Moléculaires des Maladies liées au Vieillissement - U 1167 [RID-AGE]
Sinnaeve, Davy [Auteur correspondant]
Biologie Structurale Intégrative [ERL 9002 - INSERM U1167 - BSI]
Facteurs de Risque et Déterminants Moléculaires des Maladies liées au Vieillissement - U 1167 [RID-AGE]

Date de publication :

2024-01-17

Mot(s)-clé(s) en anglais :

NMR spectroscopy
Homonuclear couplings
Pure shift NMR
2DJ spectroscopy
Stachyose
Norcamphor
NMR methodology

Discipline(s) HAL :

Chimie/Chimie analytique

Résumé en anglais : [en]

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. ...
Lire la suite >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.Lire moins >

Langue :

Anglais

Projet ANR :

RMN à haute résolution et anisotrope pour dévoiler des ensembles conformationnels de biopolymères flexibles : une stratégie générale

Collections :

• Facteurs de risque et déterminants moléculaires des maladies liées au vieillissement (RID-AGE) - U1167

Source :

Harvested from HAL