期刊
PHYSICAL CHEMISTRY CHEMICAL PHYSICS
卷 13, 期 13, 页码 5967-5973出版社
ROYAL SOC CHEMISTRY
DOI: 10.1039/c0cp01907k
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资金
- Region Nord/Pas de Calais
- Europe (FEDER)
- CNRS
- French Minister of Science
- USTL
- ENSCL
- Cortec-Net
- Bruker BIOSPIN
- TGIR RMN THC [FR-3050]
- ECNU
- Ministry of Science and Technology of China [2009IM030700]
- National Natural Science Foundation of China [10804122, 20773159, 20933009]
We show that C-13-H-1 dipolar couplings in fully protonated organic solids can be measured by applying a Symmetry-based Resonance-Echo DOuble-Resonance (S-REDOR) experiment at ultra-fast Magic-Angle Spinning (MAS). The C-13-H-1 dipolar couplings are recovered by using the R12(3)(5) recoupling scheme, while the interference of H-1-H-1 dipolar couplings are suppressed by the symmetry properties of this sequence and the use of high MAS frequency (65 kHz). The R12(3)(5) method is especially advantageous for large C-13-H-1 dipolar interactions, since the dipolar recoupling time can be incremented by steps as short as one rotor period. This allows a fine sampling for the rising part of the dipolar dephasing curve. We demonstrate experimentally that one-bond C-13-H-1 dipolar coupling in the order of 22 kHz can be accurately determined. Furthermore, the proposed method allows a rapid evaluation of the dipolar coupling by fitting the S-REDOR dipolar dephasing curve with an analytical expression.
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