A solid-state nuclear magnetic resonance (NMR) technique is described for obtaining constraints on the backbone conformation of a protein or peptide that is prepared with uniform 15 N, 13 C labeling of consecutive pairs of amino acids or of longer segments. The technique, called double single-quantu
Double-Quantum Excitation in the NMR of Spinning Solids by Pulse-Assisted Rotational Resonance
✍ Scribed by T. Karlsson; C.E. Hughes; J. Schmedt auf der Günne; M.H. Levitt
- Publisher
- Elsevier Science
- Year
- 2001
- Tongue
- English
- Weight
- 144 KB
- Volume
- 148
- Category
- Article
- ISSN
- 1090-7807
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✦ Synopsis
We describe a new technique for double-quantum excitation in magic-angle-spinning NMR of powdered solids. The technique is designed to efficiently excite double-quantum coherence in the vicinity of a rotational resonance condition. The offset from rotational resonance allows the double-quantum filtered signals to be observed with high resolution and sensitivity. The method uses rotational excitation of zero-quantum coherence, assisted by radiofrequency pulse cycles. The zero-quantum coherence is converted into double-quantum coherence by a frequency-selective inversion sequence. Experiments on [ 13 C 2 , 15 N]-glycine demonstrate a double-quantum filtering efficiency of Ӎ41% at a sample rotation frequency of 8.300 kHz, which is 1.600 kHz away from the n ؍ 1 rotational resonance. We achieve 32% double-quantum filtering efficiency at a spinning frequency of 9.250 kHz, which is 2.550 kHz away from rotational resonance.
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