Journal
JOURNAL OF MAGNETIC RESONANCE
Volume 244, Issue -, Pages 107-113Publisher
ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jmr.2014.03.003
Keywords
Magic angle spinning; Solid state NMR; Dipolar interaction; Quadrupolar coupling; REDOR; Distance measurement; Universal curve
Funding
- Binational Science Foundation (BSF) [2011077]
- Tel Aviv Center for Nanosciences and Nanotechnology
- Directorate For Engineering
- Div Of Chem, Bioeng, Env, & Transp Sys [2011077] Funding Source: National Science Foundation
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Distances between a spin-1/2 and a spin > 1/2 can be efficiently measured by a variety of magic-angle spinning solid state NMR methods such as Rotational Echo Adiabatic Passage Double Resonance (REAPDOR), Low-Alpha/Low-Amplitude REDOR (LA-REDOR) and Rotational-Echo Saturation-Pulse Double-Resonance (R/S-RESPDOR). In this manuscript we show that the incorporation of a phase modulation into a long quadrupolar recoupling pulse, lasting 10 rotor periods that are sandwiched between rotor-synchronized pairs of dipolar recoupling pi pulses, extends significantly the range of the values of the quadrupole moments that can be accessed by the experiment. We show by a combination of simulations and experiments that the new method, phase-modulated LA-REDOR, is very weakly dependent on the actual value of the radio-frequency field, and is highly robust with respect to off-resonance irradiation. The experimental results can be fitted by numerical simulations or using a universal formula corresponding to an equal-transition-probability model. Phase-modulated LA-REDOR C-13{B-11} and N-15{V-51} dipolar recoupling experiments confirm the accuracy and applicability of this new method. (C) 2014 Elsevier Inc. All rights reserved.
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