A set of experiments to determine homo-and heteronuclear vicinal coupling constants in uniformly 13C-labeled DNA oligonucleotides is presented. 2D and 3D HCCH-E.COSY experiments were used to measure 3Jm coupling constants in the deoxyribose ring, a refocused HMBC experiment was used to measure 3Jm c
13C/15N distance determination by CPMAS NMR in uniformly 13C labeled molecules
✍ Scribed by Maggy Hologne; Jésus Raya; Jérôme Hirschinger
- Publisher
- John Wiley and Sons
- Year
- 2006
- Tongue
- English
- Weight
- 216 KB
- Volume
- 44
- Category
- Article
- ISSN
- 0749-1581
- DOI
- 10.1002/mrc.1744
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✦ Synopsis
The REDOR and CPMAS techniques are applied for measuring 13C-15N dipolar coupling constants in glycine. It is shown that the selective CP or SPECIFIC CP technique removes the coherent evolution of the spin system under homonuclear 13C-13C J couplings. While the large coupling constant (approximately 900 Hz) is readily determined because of the presence of large oscillations in the CPMAS dynamics, their absence precludes the measurement of the small coupling constant (approximately 200 Hz). The experimental results and numerical simulations demonstrate that the determination of 13C-15N coupling constants of medium size (<1 kHz) by the CPMAS technique is mainly limited by the strength of the 1H decoupling field and the size of the 13C and 15N chemical shift anisotropies.
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