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 filte
Efficient Double-Quantum Excitation in Rotational Resonance NMR
✍ Scribed by T Karlsson; M Edén; H Luthman; M.H Levitt
- Publisher
- Elsevier Science
- Year
- 2000
- Tongue
- English
- Weight
- 197 KB
- Volume
- 145
- Category
- Article
- ISSN
- 1090-7807
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✦ Synopsis
We present a new technique for double-quantum excitation in magic-angle-spinning solid-state NMR. The method involves (i) preparation of nonequilibrium longitudinal magnetization; (ii) mechanical excitation of zero-quantum coherence by spinning the sample at rotational resonance, and (iii) phase-coherent conversion of the zero-quantum coherence into double-quantum coherence by frequency-selective spin inversion. The double-quantum coherence is converted into observable magnetization by reversing the excitation process, followed by a /2 pulse. The method is technically simple, does not require strong RF fields, and is feasible at high spinning frequencies. In [ 13 C 2 , 15 N]-glycine, with an internuclear 13 C-13 C distance of 0.153 nm, we achieve a doublequantum filtering efficiency of Ӎ56%. In [11,20 -13 C 2 ]-all-E-retinal, with an internuclear 13 C-13 C distance of 0.296 nm, we obtain Ӎ45% double-quantum filtering efficiency.
📜 SIMILAR VOLUMES
The homonuclear dipolar coupling of a directly bonded 13 C-13 C pair has been used to create a dipolar double-quantum filter (D-DQF) to remove the natural-abundance 13 C background in 13 Cf 2 Hg rotationalecho double-resonance (REDOR) experiments. The most efficient version of this experiment has th
## REDOR is a magic-angle spinning experiment for measuring internuclear distances between heteronuclear spin pairs. The basic principles of the REDOR technique are presented. The experimental requirements necessary for quantitative REDOR measurements are also provided.
## Double-quantum filtration under rotational resonance MAS NMR conditions where the chemical shielding anisotropies involved exceed the differences in isotropic chemical shielding is considered by means of numerical simulations and 13 C MAS NMR experiments. The responses of two different pulse se