Larimi Motahareh G, Tycko Robert
Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases, National Institutes of Health, Bethesda, MD 20892-0520, USA.
Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases, National Institutes of Health, Bethesda, MD 20892-0520, USA.
J Magn Reson. 2025 Aug;377:107908. doi: 10.1016/j.jmr.2025.107908. Epub 2025 May 28.
We investigate the effects of insufficient P pulse amplitudes on C-detected PC Rotational-Echo Double-Resonance (REDOR) measurements in a 17.5 T magnetic field. Experimental REDOR data on two compounds show that normalized REDOR difference signals ΔS/S are suppressed when the amplitudes of P π pulse trains are not very large compared with the P chemical shift anisotropies. This behavior is explained theoretically by an analysis of the effects of imperfections in π pulse rotations due to the orientation-dependent and time-dependent resonance offsets under magic-angle spinning in REDOR measurements. We show that effects of the same pulse imperfections can be observed directly by measurements of an effective relaxation time [Formula: see text] for longitudinal P spin polarization under identical π pulse trains.
我们研究了在17.5 T磁场中,P脉冲幅度不足对C检测的PC旋转回波双共振(REDOR)测量的影响。两种化合物的实验REDOR数据表明,当P π脉冲序列的幅度与P化学位移各向异性相比不是很大时,归一化的REDOR差异信号ΔS/S会受到抑制。通过分析REDOR测量中魔角旋转下由于取向依赖性和时间依赖性共振偏移导致的π脉冲旋转不完美的影响,从理论上解释了这种行为。我们表明,在相同的π脉冲序列下,通过测量纵向P自旋极化的有效弛豫时间[公式:见正文],可以直接观察到相同脉冲不完美的影响。