Indirect Detection via Spin-1/2 Nuclei in ...
Document type :
Article dans une revue scientifique: Article original
DOI :
PMID :
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Title :
Indirect Detection via Spin-1/2 Nuclei in Solid State NMR Spectroscopy: Application to the Observation of Proximities between Protons and Quadrupolar Nuclei
Author(s) :
Lafon, Olivier [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Wang, Qiang [Auteur]
Université de Lille
Chinese Academy of Sciences [Wuhan Branch]
Hu, Bingwen [Auteur]
Université de Lille
Vasconcelos, Filipe [Auteur]
Université de Lille
Trebosc, Julien [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Cristol, Sylvain [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Deng, Feng [Auteur]
Chinese Academy of Sciences [Wuhan Branch]
Amoureux, Jean-Paul [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]

Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Wang, Qiang [Auteur]
Université de Lille
Chinese Academy of Sciences [Wuhan Branch]
Hu, Bingwen [Auteur]
Université de Lille
Vasconcelos, Filipe [Auteur]
Université de Lille
Trebosc, Julien [Auteur]

Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Cristol, Sylvain [Auteur]

Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Deng, Feng [Auteur]
Chinese Academy of Sciences [Wuhan Branch]
Amoureux, Jean-Paul [Auteur]

Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Journal title :
Journal of Physical Chemistry A
Abbreviated title :
J. Phys. Chem. A
Volume number :
113
Pages :
12864-12878
Publication date :
2009-10-02
ISSN :
1089-5639
HAL domain(s) :
Chimie
English abstract : [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, ...
Show more >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.Show less >
Show more >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.Show less >
Language :
Anglais
Audience :
Internationale
Popular science :
Non
Administrative institution(s) :
Université de Lille
CNRS
Centrale Lille
ENSCL
Univ. Artois
CNRS
Centrale Lille
ENSCL
Univ. Artois
Collections :
Research team(s) :
Modélisation et spectroscopies (MODSPEC)
RMN et matériaux inorganiques (RM2I)
RMN et matériaux inorganiques (RM2I)
Submission date :
2023-05-30T17:58:46Z
2024-04-26T08:23:39Z
2024-04-26T08:23:39Z