Centre of Molecular and Macromolecular Studies , Polish Academy of Sciences , Sienkiewicza 112 , PL-90363 Łódź , Poland.
Department of Theoretical Physics, Faculty of Physics and Applied Informatics , University of Łódź , Pomorska 149/153 , PL-90236 Łódź , Poland.
J Phys Chem B. 2018 Aug 30;122(34):8146-8156. doi: 10.1021/acs.jpcb.8b04557. Epub 2018 Aug 20.
We report a new solid-state multidimensional NMR approach based on the cross-polarization with variable-contact pulse sequence [ Paluch , P. ; Pawlak , T. ; Amoureux , J.-P. ; Potrzebowski , M. J. J. Magn. Reson. 233 , 2013 , 56 ], with H inverse detection and very fast magic angle spinning (ν = 60 kHz), dedicated to the measurement of local molecular motions of H-N vectors. The introduced three-dimensional experiments, H-N-H and hCA(N)H, are particularly useful for the study of molecular dynamics of proteins and other complex structures. The applicability and power of this methodology have been revealed by employing as a model sample the GB-1 small protein doped with NaCuEDTA. The results clearly prove that the dispersion of H-N dipolar coupling constants well correlates with higher order structure of the protein. Our approach complements the conventional studies and offers a fast and reasonably simple method.
我们报告了一种新的基于交叉极化与可变接触脉冲序列（Paluch，P.；Pawlak，T.；Amoureux，J.-P.；Potrzebowski，M. J. J. Magn. Reson. 233，2013，56）的固态多维 NMR 方法，采用 H 反转检测和非常快速的魔角旋转（ν=60 kHz），专门用于测量 H-N 矢量的局部分子运动。所引入的三维实验 H-N-H 和 hCA（N）H 特别适用于研究蛋白质和其他复杂结构的分子动力学。通过使用掺杂有 NaCuEDTA 的 GB-1 小蛋白作为模型样品，证明了该方法的适用性和强大功能。结果清楚地证明了 H-N 偶极耦合常数的分散与蛋白质的高级结构很好地相关。我们的方法补充了传统研究，并提供了一种快速且相对简单的方法。
