Department for NMR-based Structural Biology, Max-Planck-Institute for Biophysical Chemistry, Am Fassberg 11, 37077 Göttingen, Germany.
J Am Chem Soc. 2010 Jan 13;132(1):223-33. doi: 10.1021/ja906283h.
We demonstrate the use of two-dimensional ((13)C,(13)C) double-quantum spectroscopy to detect molecular dynamics by solid-state NMR. Data collected on tyrosine-ethylester (TEE) are in line with previously determined ((1)H,(13)C) order parameters. Application of these experiments to microcrystalline ubiquitin reveals the presence of dynamics on millisecond or faster time scales and differences in local mobility depending on microcrystal preparation. In addition, solid-state NMR-based structure calculation indicates conformational variability of loop regions between different solid-phase ubiquitin preparations. Our data relate preparation-dependent changes observed in NMR spectral parameters such as chemical shifts and through-space correlations to differences in ubiquitin dynamics and conformation and suggest a prominent role of molecular mobility in microcrystalline ubiquitin.
我们展示了二维 ((13)C,(13)C) 双量子谱通过固态 NMR 来检测分子动力学的应用。在酪氨酸乙酯 (TEE) 上收集的数据与先前确定的 ((1)H,(13)C) 序参数一致。将这些实验应用于微结晶泛素揭示了毫秒或更快时间尺度上的动力学存在以及微结晶制备方式不同导致的局部流动性差异。此外，基于固态 NMR 的结构计算表明不同固相泛素制备物之间环区构象的可变性。我们的数据将 NMR 光谱参数（如化学位移和空间相关）中观察到的与泛素动力学和构象不同的依赖于制备的变化联系起来，并表明分子流动性在微结晶泛素中起着重要作用。
