Titre :

Indirect Detection via Spin-1/2 Nuclei in Solid State NMR Spectroscopy: Application to the Observation of Proximities between Protons and Quadrupolar Nuclei

Auteur(s) :

Lafon, Olivier [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Wang, Q. [Auteur]
Hu, B. W. [Auteur]
Vasconcelos, F. [Auteur]
Trebosc, Julien [Auteur]
Cristol, Sylvain [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Deng, F. [Auteur]
Amoureux, Jean-Paul [Auteur]

Titre de la revue :

J. Phys. Chem. A

Nom court de la revue :

J. Phys. Chem. A

Pagination :

12864-12878

Date de publication :

2009-10-02

ISSN :

1089-5639

Discipline(s) HAL :

Chimie

Résumé en anglais : [en]

We present a comprehensive comparison of through-space heteronuclear correlation techniques for solid state NMR, combining indirect detection and single-channel recoupling method. These techniques, named D-HMQC and D-HSQC, ...
Lire la suite >We present a comprehensive comparison of through-space heteronuclear correlation techniques for solid state NMR, combining indirect detection and single-channel recoupling method. These techniques, named D-HMQC and D-HSQC, do not suffer from dipolar truncation and can be employed to correlate quadrupolar nuclei with spin-1/2 nuclei. The heteronuclear dipolar couplings are restored under magic-angle spinning by applying supercycled symmetry-based pulse sequences (SR412) or simultaneous frequency and amplitude modulation (SFAM). The average Hamiltonian theory (AHT) of these recoupling methods is developed. These results are applied to analyze the performances of D-HMQC and D-HSQC sequences. It is shown that, whatever the magnitude of spin interations, D-HMQC experiment offers larger efficiency and higher robustness than D-HSQC. Furthermore, the spectral resolution in both dimensions of proton detected two-dimensional D-HMQC and D-HSQC spectra can be enhanced by applying recently introduced symmetry-based homonuclear dipolar decoupling schemes that cause a z-rotation of the spins. This is demonstrated by 1H−13C and 1H−23Na correlation experiments on l-histidine and NaH2PO4, respectively. The two-dimensional heteronuclear 1H−23Na correlation spectrum yields the assignment of 23Na resonances of NaH2PO4. This assignment is corroborated by first-principles calculations.Lire moins >

Langue :

Anglais

Établissement(s) :

Université de Lille
CNRS
Centrale Lille
ENSCL
Univ. Artois

Collections :

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

Équipe(s) de recherche :

Modélisation et spectroscopies (MODSPEC)
RMN et matériaux inorganiques (RM2I)

Date de dépôt :

2023-05-30T17:58:46Z