Accurate NMR determination of C–H or N–H ...
Type de document :
Article dans une revue scientifique
URL permanente :
Titre :
Accurate NMR determination of C–H or N–H distances for unlabeled molecules
Auteur(s) :
Nishiyama, Yusuke [Auteur]
RIKEN Center for Life Science Technologies [RIKEN CLST]
Malon, M. [Auteur]
RIKEN Center for Life Science Technologies [RIKEN CLST]
Potrzebowski, Marek J. [Auteur]
Institute of Physics, Polish Academy of Sciences
Paluch, Piotr [Auteur]
Institute of Physics, Polish Academy of Sciences
Amoureux, Jean-Paul [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
East China Normal University [Shangaï] [ECNU]
RIKEN Center for Life Science Technologies [RIKEN CLST]
Malon, M. [Auteur]
RIKEN Center for Life Science Technologies [RIKEN CLST]
Potrzebowski, Marek J. [Auteur]
Institute of Physics, Polish Academy of Sciences
Paluch, Piotr [Auteur]
Institute of Physics, Polish Academy of Sciences
Amoureux, Jean-Paul [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
East China Normal University [Shangaï] [ECNU]
Titre de la revue :
Solid State Nuclear Magnetic Resonance
Numéro :
73
Pagination :
15-21
Date de publication :
2016-02
Discipline(s) HAL :
Chimie/Chimie inorganique
Résumé en anglais : [en]
Cross-Polarization with Variable Contact-time (CP-VC) is very efficient at ultra-fast MAS (νR≥60 kHz) to measure accurately the dipolar interactions corresponding to C–H or N–H short distances, which are very useful for ...
Lire la suite >Cross-Polarization with Variable Contact-time (CP-VC) is very efficient at ultra-fast MAS (νR≥60 kHz) to measure accurately the dipolar interactions corresponding to C–H or N–H short distances, which are very useful for resonance assignment and for analysis of dynamics. Here, we demonstrate the CP-VC experiment with 1H detection. In the case of C–H distances, we compare the CP-VC signals with direct (13C) and indirect (1H) detection and find that the latter allows a S/N gain of ca. 2.5, which means a gain of ca. 6 in experimental time. The main powerful characteristics of CP-VC methods are related to the ultra-fast spinning speed and to the fact that most of the time only the value of the dipolar peak separation has to be used to obtain the information. As a result, CP-VC methods are: (i) easy to set up and to use, and robust with respect to (ii) rf-inhomogeneity thus allowing the use of full rotor samples, (iii) rf mismatch, and (iv) offsets and chemical shift anisotropies. It must be noted that the CP-VC 2D method with indirect 1H detection requires the proton resolution and is thus mainly applicable to small or perdeuterated molecules. We also show that an analysis of the dynamics can even be performed, with a reasonable experimental time, on unlabeled samples with 13C or even 15N natural abundance.Lire moins >
Lire la suite >Cross-Polarization with Variable Contact-time (CP-VC) is very efficient at ultra-fast MAS (νR≥60 kHz) to measure accurately the dipolar interactions corresponding to C–H or N–H short distances, which are very useful for resonance assignment and for analysis of dynamics. Here, we demonstrate the CP-VC experiment with 1H detection. In the case of C–H distances, we compare the CP-VC signals with direct (13C) and indirect (1H) detection and find that the latter allows a S/N gain of ca. 2.5, which means a gain of ca. 6 in experimental time. The main powerful characteristics of CP-VC methods are related to the ultra-fast spinning speed and to the fact that most of the time only the value of the dipolar peak separation has to be used to obtain the information. As a result, CP-VC methods are: (i) easy to set up and to use, and robust with respect to (ii) rf-inhomogeneity thus allowing the use of full rotor samples, (iii) rf mismatch, and (iv) offsets and chemical shift anisotropies. It must be noted that the CP-VC 2D method with indirect 1H detection requires the proton resolution and is thus mainly applicable to small or perdeuterated molecules. We also show that an analysis of the dynamics can even be performed, with a reasonable experimental time, on unlabeled samples with 13C or even 15N natural abundance.Lire moins >
Langue :
Anglais
Audience :
Internationale
Vulgarisation :
Non
Établissement(s) :
ENSCL
CNRS
Centrale Lille
Univ. Artois
Université de Lille
CNRS
Centrale Lille
Univ. Artois
Université de Lille
Collections :
Équipe(s) de recherche :
RMN et matériaux inorganiques (RM2I)
Date de dépôt :
2019-09-25T14:06:17Z
2024-04-22T11:29:41Z
2024-04-22T11:29:41Z