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Proton to carbon-13 INEPT in solid-state NMR spectroscopy
- Source :
- Journal of the American Chemical Society, Journal of the American Chemical Society, American Chemical Society, 2005, 127, pp.17296-17302. ⟨10.1021/ja054411x⟩, Journal of the American Chemical Society, 2005, 127, pp.17296-17302. ⟨10.1021/ja054411x⟩
- Publication Year :
- 2005
-
Abstract
- International audience; A refocused INEPT through-bond coherence transfer technique is demonstrated for NMR of rigid organic solids and is shown to provide a valuable building block for the development of NMR correlation experiments in biological solids. The use of efficient proton homonuclear dipolar decoupling in combination with a direct spectral optimization procedure provides minimization of the transverse dephasing of coherences and leads to very efficient through-bond (1)H-(13)C INEPT transfer for crystalline organic compounds. Application of this technique to 2D heteronuclear correlation spectroscopy leads to up to a factor of 3 increase in sensitivity for a carbon-13 enriched sample in comparison to standard through-bond experiments and provides excellent selectivity for one-bond transfer. The method is demonstrated on a microcrystalline sample of the protein Crh (2 x 10.4 kDa).A refocused INEPT through-bond coherence transfer technique is demonstrated for NMR of rigid organic solids and is shown to provide a valuable building block for the development of NMR correlation experiments in biological solids. The use of efficient proton homonuclear dipolar decoupling in combination with a direct spectral optimization procedure provides minimization of the transverse dephasing of coherences and leads to very efficient through-bond (1)H-(13)C INEPT transfer for crystalline organic compounds. Application of this technique to 2D heteronuclear correlation spectroscopy leads to up to a factor of 3 increase in sensitivity for a carbon-13 enriched sample in comparison to standard through-bond experiments and provides excellent selectivity for one-bond transfer. The method is demonstrated on a microcrystalline sample of the protein Crh (2 x 10.4 kDa).
- Subjects :
- Chemistry
Dephasing
Analytical chemistry
Pulse sequence
02 engineering and technology
General Chemistry
010402 general chemistry
021001 nanoscience & nanotechnology
01 natural sciences
Biochemistry
Catalysis
Homonuclear molecule
0104 chemical sciences
Colloid and Surface Chemistry
Heteronuclear molecule
Solid-state nuclear magnetic resonance
[SDV.BBM]Life Sciences [q-bio]/Biochemistry, Molecular Biology
0210 nano-technology
Spectroscopy
Two-dimensional nuclear magnetic resonance spectroscopy
Heteronuclear single quantum coherence spectroscopy
Subjects
Details
- ISSN :
- 00027863 and 15205126
- Volume :
- 127
- Issue :
- 49
- Database :
- OpenAIRE
- Journal :
- Journal of the American Chemical Society
- Accession number :
- edsair.doi.dedup.....3ce09a9c1b80f60dcb91f4d9e50b251f
- Full Text :
- https://doi.org/10.1021/ja054411x⟩