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固态核磁共振中P脉冲幅度不足对C检测PC旋转回波双共振测量的影响。

Effects of insufficient P pulse amplitudes on C-detected PC rotational-echo double-resonance measurements in solid state NMR.

作者信息

Larimi Motahareh G, Tycko Robert

机构信息

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.

出版信息

J Magn Reson. 2025 Aug;377:107908. doi: 10.1016/j.jmr.2025.107908. Epub 2025 May 28.

Abstract

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.

摘要

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。

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