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在固态核磁共振中使用偶极回波编辑的R-对称序列进行高效异核极化转移。

Highly efficient heteronuclear polarization transfer using dipolar-echo edited R-symmetry sequences in solid-state NMR.

作者信息

Liang Lixin, Chen Kuizhi, Hou Guangjin

机构信息

State Key Laboratory of Catalysis, Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences Zhongshan Road 457 Dalian 116023 China

出版信息

Chem Sci. 2024 Dec 21;16(5):2251-2257. doi: 10.1039/d4sc07965e. eCollection 2025 Jan 29.

Abstract

In solid-state NMR, dipolar-based heteronuclear polarization transfer has been extensively used for sensitivity enhancement and multidimensional correlations, but its efficiency often suffers from undesired spin interactions and hardware limitations. Herein, we propose a novel dipolar-echo edited R-symmetry (DEER) sequence, which is further incorporated into the INEPT-type scheme, dubbed DEER-INEPT, for achieving highly efficient heteronuclear polarization transfer. Numerical simulations and NMR experiments demonstrate that DEER-INEPT offers significantly improved robustness, enabling efficient polarization transfer under a wide range of MAS conditions, from slow to ultrafast rates, outperforming existing methods. Its high efficiency leads to noticeably enhanced sensitivity in both H → X and X → H transfers, applicable to both spin-1/2 and spin-half-integer quadrupolar nuclei. DEER-INEPT is expected to be widely used in various systems, offering advantages in both sensitivity enhancement and structural analysis.

摘要

在固态核磁共振中,基于偶极的异核极化转移已被广泛用于提高灵敏度和进行多维关联,但它的效率常常受到不期望的自旋相互作用和硬件限制的影响。在此,我们提出了一种新颖的偶极回波编辑R对称(DEER)序列,该序列进一步被纳入INEPT型方案,称为DEER-INEPT,以实现高效的异核极化转移。数值模拟和核磁共振实验表明,DEER-INEPT具有显著提高的稳健性,能够在从慢速到超快速率的广泛MAS条件下实现高效的极化转移,优于现有方法。其高效率导致在H→X和X→H转移中灵敏度显著提高,适用于自旋1/2和自旋半整数四极核。DEER-INEPT有望在各种系统中得到广泛应用,在提高灵敏度和结构分析方面均具有优势。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/518e/11778243/dcf3f042ad91/d4sc07965e-f1.jpg

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