Rapid Structural Analysis of Minute Quantities of Organic Solids by Exhausting 1H Polarization in Solid-State NMR Spectroscopy Under Fast Magic Angle Spinning.
Rapid Structural Analysis of Minute Quantities of Organic Solids by Exhausting 1H Polarization in Solid-State NMR Spectroscopy Under Fast Magic Angle Spinning.
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DOI：
10.1021/acs.jpclett.1c03672
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发表时间：
2021-12
期刊：
影响因子：
--
通讯作者：
Z. Yan;Rongchun Zhang
中科院分区：
文献类型：
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作者：
Z. Yan;Rongchun Zhang
固态核磁共振（NMR）通常由于涉及低γ核时固有的低信号灵敏度而受到显著的限制。在这里，我们报告了一个优雅的固态NMR方法，用于微量有机固体的快速结构分析。通过在间接维上对化学位移的交错演化进行编码，在1H维上对化学位移的交错获取，在快速魔角旋转（MAS）条件下，在一次实验中，几乎不增加实验时间，同时获得了质子探测的同质1H/1H和异质13 C/1H化学位移相关（HETCOR）谱.我们进一步表明，在传统的1H-检测HETCOR实验时间，多个home-home 1H/1H相关光谱可以记录除了HETCOR光谱，使1H-1H距离的测定。我们建立了丰富的1H极化可以有效地操纵和充分利用质子检测的固态NMR光谱提取更关键的结构信息，从而减少总的实验时间。
Solid-state nuclear magnetic resonance (NMR) often suffers from significant limitations due to the inherent low signal sensitivity when low-γ nuclei are involved. Herein, we report an elegant solid-state NMR approach for rapid structural analysis of minute amounts of organic solids. By encoding staggered chemical shift evolution in the indirect dimension and staggered acquisition in the 1H dimension, a proton-detected homonuclear 1H/1H and heteronuclear 13C/1H chemical shift correlation (HETCOR) spectrum can be obtained simultaneously in a single experiment at a fast magic-angle-spinning (MAS) condition with barely increasing the experimental time. We further show that during the conventional 1H-detected HETCOR experimental time, multiple homonuclear 1H/1H correlation spectra can be recorded in addition to the HETCOR spectrum, enabling the determination of 1H-1H distances. We establish that abundant 1H polarization can be efficiently manipulated and fully utilized in proton-detected solid-state NMR spectroscopy for extraction of more critical structural information and thus reduction of the total experimental time.