Probing 29Si-17O connectivities and ...
Type de document :
Article dans une revue scientifique: Article original
URL permanente :
Titre :
Probing 29Si-17O connectivities and proximities by solid-state NMR
Auteur(s) :
Pourpoint, Frederique [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Venel, Florian [Auteur]
Giovine, Raynald [Auteur]
Trebosc, Julien [Auteur]
Vancompernolle, Tom [Auteur]
Taoufik, Mostafa [Auteur]
Sarou-Kanian, Vincent [Auteur]
Gauvin, Regis [Auteur]
Unité de Catalyse et de Chimie du Solide (UCCS) - UMR 8181
Lafon, Olivier [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Venel, Florian [Auteur]
Giovine, Raynald [Auteur]
Trebosc, Julien [Auteur]
Vancompernolle, Tom [Auteur]
Taoufik, Mostafa [Auteur]
Sarou-Kanian, Vincent [Auteur]
Gauvin, Regis [Auteur]
Unité de Catalyse et de Chimie du Solide (UCCS) - UMR 8181
Lafon, Olivier [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Titre de la revue :
Journal of Magnetic Resonance
Numéro :
330
Pagination :
107029
Date de publication :
2021-09
ISSN :
10907807
Discipline(s) HAL :
Chimie/Chimie inorganique
Résumé en anglais : [en]
The measurement of dipolar and J- couplings between 29Si and 17O isotopes is challenging owing to (i) the low abundance of both isotopes and (ii) their close Larmor frequencies, which only differ by 19%. These issues are ...
Lire la suite >The measurement of dipolar and J- couplings between 29Si and 17O isotopes is challenging owing to (i) the low abundance of both isotopes and (ii) their close Larmor frequencies, which only differ by 19%. These issues are circumvented here by the use of isotopic enrichment and dedicated triple-resonance magic-angle spinning NMR probe. The surface of 29Si-enriched silica was labelled with 17O isotope and heated at 80 and 200 °C. 29Si-17O connectivities and proximities were probed using two-dimensional (2D) through-bond and through-space heteronuclear multiple-quantum coherences (J- and D-HMQC) experiments between 17O and 29Si nuclei. The simulation of the build-up of the J- and D-HMQC signals allowed the first experimental measurement of J- and dipolar coupling constants between 17O and 29Si nuclei. These HMQC experiments allow distinguishing two distinct siloxane (SiOSi) oxygen sites: (i) those covalently bonded to Q3 and Q4 groups, having a hydroxyl group as a second neighbour and (ii) those covalently bonded to two Q4 groups. The measured J- and dipolar coupling constants of siloxane 17O nucleus with Q4 29Si nuclei differ from those with Q3 29Si nuclei. These results indicate that the 29Si-17O one-bond J-coupling and Si-O bond length depend on the second neighbours of the Si atoms.Lire moins >
Lire la suite >The measurement of dipolar and J- couplings between 29Si and 17O isotopes is challenging owing to (i) the low abundance of both isotopes and (ii) their close Larmor frequencies, which only differ by 19%. These issues are circumvented here by the use of isotopic enrichment and dedicated triple-resonance magic-angle spinning NMR probe. The surface of 29Si-enriched silica was labelled with 17O isotope and heated at 80 and 200 °C. 29Si-17O connectivities and proximities were probed using two-dimensional (2D) through-bond and through-space heteronuclear multiple-quantum coherences (J- and D-HMQC) experiments between 17O and 29Si nuclei. The simulation of the build-up of the J- and D-HMQC signals allowed the first experimental measurement of J- and dipolar coupling constants between 17O and 29Si nuclei. These HMQC experiments allow distinguishing two distinct siloxane (SiOSi) oxygen sites: (i) those covalently bonded to Q3 and Q4 groups, having a hydroxyl group as a second neighbour and (ii) those covalently bonded to two Q4 groups. The measured J- and dipolar coupling constants of siloxane 17O nucleus with Q4 29Si nuclei differ from those with Q3 29Si nuclei. These results indicate that the 29Si-17O one-bond J-coupling and Si-O bond length depend on the second neighbours of the Si atoms.Lire moins >
Langue :
Anglais
Audience :
Internationale
Vulgarisation :
Non
Établissement(s) :
CNRS
Centrale Lille
ENSCL
Univ. Artois
Université de Lille
Centrale Lille
ENSCL
Univ. Artois
Université de Lille
Collections :
Équipe(s) de recherche :
RMN et matériaux inorganiques (RM2I)
Date de dépôt :
2022-03-24T09:03:01Z
2024-01-16T17:25:58Z
2024-01-16T17:25:58Z
Fichiers
- document
- Accès libre
- Accéder au document