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Frequency-selective homonuclear dipolar recoupling in solid state NMR

机译:固态NMR中的频率选择同核偶极耦合

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摘要

We introduce a new approach to frequency-selective homonuclear dipolar recoupling in solid state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS). This approach, to which we give the acronym SEASHORE, employs alternating periods of double-quantum recoupling and chemical shift evolution to produce phase modulations of the recoupled dipole-dipole interactions that average out undesired couplings, leaving only dipole-dipole couplings between nuclear spins with a selected pair of NMR frequencies. In principle, SEASHORE is applicable to systems with arbitrary coupling strengths and arbitrary sets of NMR frequencies. Arbitrary MAS frequencies are also possible, subject only to restrictions imposed by the pulse sequence chosen for double-quantum recoupling. We demonstrate the efficacy of SEASHORE in experimental 13C NMR measurements of frequency-selective polarization transfer in uniformly 15N,13C-labeled L-valine powder and frequency-selective intermolecular polarization transfer in amyloid fibrils formed by a synthetic decapeptide containing uniformly 15N,13C-labeled residues.
机译:我们介绍了一种新的方法,通过魔术角旋转(MAS)在固态核磁共振(NMR)中进行频率选择性同核偶极耦合。我们将其缩写为SEASHORE的这种方法采用双量子重新耦合和化学位移演化的交替周期来产生重新耦合的偶极子-偶极子相互作用的相位调制,从而平均消除不希望的耦合,而在核自旋之间仅留下偶极子-偶极子耦合。一对选定的NMR频率。原则上,SEASHORE适用于具有任意耦合强度和任意组NMR频率的系统。任意MAS频率也是可能的,仅受为双量子耦合选择的脉冲序列所施加的限制。我们证明SEASHORE在均匀地 15 N, 13 C标记的L-的频率选择性极化转移的实验 13 C NMR测量中的功效缬氨酸粉末和淀粉样原纤维中频率选择性的分子间极化转移,该淀粉样蛋白由含有统一 15 N, 13 C标记残基的合成十肽形成。

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