Recent progress in dipolar recoupling techniques under fast MAS in solid-state NMR spectroscopy

IF 1.8 3区 化学 Q4 CHEMISTRY, PHYSICAL
Yi Ji , Lixin Liang , Xinhe Bao , Guangjin Hou
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引用次数: 14

Abstract

With the recent advances in NMR hardware and probe design technology, magic-angle spinning (MAS) rates over 100 ​kHz are accessible now, even on commercial solid NMR probes. Under such fast MAS conditions, excellent spectral resolution has been achieved by efficient suppression of anisotropic interactions, which also opens an avenue to the proton-detected NMR experiments in solids. Numerous methods have been developed to take full advantage of fast MAS during the last decades. Among them, dipolar recoupling techniques under fast MAS play vital roles in the determination of the molecular structure and dynamics, and are also key elements in multi-dimensional correlation NMR experiments. Herein, we review the dipolar recoupling techniques, especially those developed in the past two decades for fast-to-ultrafast MAS conditions. A major focus for our discussion is the ratio of RF field strength (in frequency) to MAS frequency, ν1/νr, in different pulse sequences, which determines whether these dipolar recoupling techniques are suitable for NMR experiments under fast MAS conditions. Systematic comparisons are made among both heteronuclear and homonuclear dipolar recoupling schemes. In addition, the schemes developed specially for proton-detection NMR experiments under ultrafast MAS conditions are highlighted as well.

Abstract Image

固态核磁共振光谱快速MAS下偶极重偶联技术研究进展
随着核磁共振硬件和探针设计技术的最新进展,现在甚至在商业固体核磁共振探针上也可以实现超过100 kHz的魔角旋转(MAS)速率。在这种快速的MAS条件下,通过有效地抑制各向异性相互作用,获得了优异的光谱分辨率,这也为固体中质子探测核磁共振实验开辟了一条途径。在过去的几十年里,已经开发了许多方法来充分利用快速MAS。其中,快速MAS下的偶极重耦合技术在分子结构和动力学的测定中起着至关重要的作用,也是多维相关核磁共振实验的关键要素。在此,我们回顾了偶极重耦合技术,特别是在过去二十年中开发的用于快速到超快MAS条件的技术。我们讨论的主要焦点是不同脉冲序列中射频场强(频率)与MAS频率的比值ν1/νr,这决定了这些偶极重耦合技术是否适用于快速MAS条件下的核磁共振实验。系统地比较了异核和同核偶极重耦合方案。此外,还重点介绍了超快MAS条件下质子探测核磁共振实验的方案。
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来源期刊
CiteScore
5.30
自引率
9.40%
发文量
42
审稿时长
72 days
期刊介绍: The journal Solid State Nuclear Magnetic Resonance publishes original manuscripts of high scientific quality dealing with all experimental and theoretical aspects of solid state NMR. This includes advances in instrumentation, development of new experimental techniques and methodology, new theoretical insights, new data processing and simulation methods, and original applications of established or novel methods to scientific problems.
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