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Off-resonance 13C–2H REDOR NMR for site-resolved studies of molecular motion
Journal of Biomolecular NMR ( IF 2.7 ) Pub Date : 2021-08-03 , DOI: 10.1007/s10858-021-00377-7
Martin D Gelenter 1 , Kelly J Chen 1 , Mei Hong 1
Affiliation  

We introduce a 13C–2H Rotational Echo DOuble Resonance (REDOR) technique that uses the difference between on-resonance and off-resonance 2H irradiation to detect dynamic segments in deuterated molecules. By selectively inverting specific regions of the 2H magic-angle spinning (MAS) sideband manifold to recouple some of the deuterons to nearby carbons, we distinguish dynamic and rigid residues in 1D and 2D 13C spectra. We demonstrate this approach on deuterated GB1, H/D exchanged GB1, and perdeuterated bacterial cellulose. Numerical simulations reproduce the measured mixing-time and 2H carrier-frequency dependence of the REDOR dephasing of bacterial cellulose. Combining numerical simulations with experiments thus allow the extraction of motionally averaged quadrupolar couplings from REDOR dephasing values.



中文翻译:

非共振 13C–2H REDOR NMR 用于分子运动的位点分辨研究

我们介绍了一种13 C – 2 H 旋转回波双共振 (REDOR) 技术,该技术使用共振和非共振2 H 辐射之间的差异来检测氘化分子中的动态片段。通过选择性地反转2 H 魔角自旋 (MAS) 边带流形的特定区域以将一些氘核重新耦合到附近的碳,我们区分了一维和二维13 C 光谱中的动态和刚性残基。我们在氘化 GB1、H/D 交换 GB1 和过氘化细菌纤维素上演示了这种方法。数值模拟再现了测量的混合时间和2细菌纤维素的REDOR去相位的H 载波频率依赖性。因此,将数值模拟与实验相结合,可以从 REDOR 相移值中提取运动平均的四极耦合。

更新日期:2021-08-03
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