Efficient deuterium-carbon REDOR NMR spectroscopy.
Phase modulated pulses for deuterium recoupling in (2)H-(13)C REDOR NMR spectroscopy have been introduced to improve dephasing of the detected (13)C nuclei. The deuterium inversion properties of phase modulated recoupling pulses have been studied experimentally on l-alanine-2-d(1) and theoretically using average Hamiltonian theory and exact simulations of the equation of motion of the density matrix. The best (13)C dephasing was observed when XYXYX ( PM5) deuterium recoupling pulses were applied. A comparison to the 90 degrees -180 degrees -90 degrees ( CPL) composite pulse scheme revealed an improvement of recoupling on the order of 2. 5. Simple CW recoupling pulses of the same length of PM5 and CPL pulses showed the weakest (13)C dephasing. Simulations have shown that the (2)H recoupling efficiency of PM5 REDOR experiments approach the very efficient REAPDOR results. However, in our case a REAPDOR study of l-alanine-2-d(1) resulted in a significant decrease of the (13)C signal intensity due to pulse imperfections of (13)C pi-pulses. The new PM5-REDOR technique has been employed to study the torsion angle between C1/2 and C5 in ethylmalonic acid-4-d(2).[1]References
- Efficient deuterium-carbon REDOR NMR spectroscopy. Sack, I., Vega, S. J. Magn. Reson. (2000) [Pubmed]
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