Columbia University, Department of Chemistry, 3000 Broadway, New York, NY 10027, USA.
J Magn Reson. 2012 Sep;222:74-80. doi: 10.1016/j.jmr.2012.05.019. Epub 2012 Jun 7.
A solid state NMR experiment is introduced for probing motions on the millisecond time scale, based on dephasing and refocusing (1)H-(13)C or (1)H-(15)N dipolar couplings. The method is related to the previously described Centerband-Only Detection of Exchange or CODEX experiment. The use of an R-type dipolar recoupling sequence takes advantage of the strong (1)H-(13)C or (1)H-(15)N dipolar coupling, while suppressing the effect of (1)H-(1)H homonuclear coupling. This approach paves the way to detect both the correlation time and reorientational angle of the dynamics in fully protonated samples. The performance of this pulse sequence is demonstrated using imidazole methyl sulfonate.
介绍了一种基于去相位和重聚焦(1)H-(13)C 或(1)H-(15)N 偶极耦合来探测毫秒时间尺度上运动的固态 NMR 实验。该方法与先前描述的仅中心带检测交换或 CODEX 实验有关。使用 R 型偶极重聚序列利用了强(1)H-(13)C 或(1)H-(15)N 偶极耦合,同时抑制了(1)H-(1)H 同核耦合的影响。这种方法为检测完全质子化样品中动力学的相关时间和重取向角铺平了道路。该脉冲序列的性能使用咪唑甲基磺酸酯进行了验证。