Department of Chemistry and Biochemistry, University of Delaware, Newark, Delaware 19716, United States.
Department of Chemistry and Biochemistry, University of Delaware, Newark, Delaware 19716, United States; Pittsburgh Center for HIV Protein Interactions, University of Pittsburgh School of Medicine, 1051 Biomedical Science Tower 3, 3501 Fifth Avenue, Pittsburgh, PA 15261, United States.
J Magn Reson. 2023 Mar;348:107382. doi: 10.1016/j.jmr.2023.107382. Epub 2023 Jan 23.
Chemical shift tensors (CSTs) are sensitive probes of structure and dynamics. R-symmetry pulse sequences (RNCSA) can efficiently recouple CSTs of varying magnitudes in magic angle spinning (MAS) NMR experiments, for a broad range of conditions and MAS frequencies. Herein, we introduce dual-channel R-symmetry pulse sequences for simultaneously recording CSTs of two different nuclei in a single experiment (DORNE-CSA). We demonstrate the performance of DORNE-CSA sequences for simultaneous measurement of C and N CSTs, on a U-C,N-labeled microcrystalline l-histidine. We show that the DORNE-CSA method is robust, provides accurate CST parameters, and takes only half of the measurement time compared to a pair of RNCSA experiments otherwise required for recording the CSTs of individual nuclei. DORNE-CSA approach is broadly applicable to a wide range of biological and inorganic systems.
化学位移张量(CST)是结构和动力学的敏感探针。R 对称性脉冲序列(RNCSA)可在魔角旋转(MAS)NMR 实验中有效地重新耦合不同幅度的 CST,适用于广泛的条件和 MAS 频率。在此,我们引入双通道 R 对称性脉冲序列,用于在单次实验中同时记录两个不同核的 CST(DORNE-CSA)。我们展示了 DORNE-CSA 序列在同时测量 U-C,N 标记的微晶 l-组氨酸的 C 和 N CST 方面的性能。我们表明,DORNE-CSA 方法具有稳健性,提供了准确的 CST 参数,并且与单独记录单个核的 CST 所需的一对 RNCSA 实验相比,测量时间仅为其一半。DORNE-CSA 方法广泛适用于各种生物和无机系统。