Title :

Probing 29Si-17O connectivities and proximities by solid-state NMR

Author(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

Journal title :

Journal of Magnetic Resonance

Volume number :

330

Pages :

107029

Publication date :

2021-09

ISSN :

10907807

HAL domain(s) :

Chimie/Chimie inorganique

English abstract : [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 ...
Show more >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.Show less >

Language :

Anglais

Audience :

Internationale

Popular science :

Non

Administrative institution(s) :

CNRS
Centrale Lille
ENSCL
Univ. Artois
Université de Lille

Collections :

• Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181

Research team(s) :

RMN et matériaux inorganiques (RM2I)

Submission date :

2022-03-24T09:03:01Z
2024-01-16T17:25:58Z