13C-13C旋转共振宽度距离测量在均标记的13C中
Ramesh Ramachandran1, Vladimir Ladizhansky, Vikram S Bajaj
1Francis Bitter Magnet Laboratory and Department of Chemistry, Massachusetts Institute of Technology, Cambridge, MA 02139-4307, USA.
Journal of the American Chemical Society
|December 11, 2003
概括
旋转共振宽度 (R2W) 实验准确地测量了生物固体中的距离. 这种方法克服了先前技术的局限性,使统一标记系统能够准确地进行特定地点的测量.
科学领域:
- 固态核磁共振 (NMR) 光谱学
- 结构生物学是结构生物学.
- 生物物理学的生物物理.
背景情况:
- 传统的旋转共振 (R2) 实验测量了随时间的磁化交换.
- 同时提取双极合和放松参数可能是具有挑战性的.
- 双极截断效应限制在均标记的固体中测量距离.
研究的目的:
- 介绍和验证旋转共振宽度 (R2W) 实验,用于测量固体中的距离.
- 为了证明R2W与2D 13C-13C化学转移相关性光谱学相结合的实用性.
- 通过克服二极截断,展示R2W在被统一标记的生物系统中的适用性.
主要方法:
- 使用恒定时间旋转共振宽度 (R2W) 实验.
- 测量磁化交换作为样品旋转频率的函数.
- 结合R2W与二维13C-13C化学转移相关性光谱.
主要成果:
- 独立且明确地提取了双极合和放松参数.
- 在R2W实验中减弱的二极截断效应.
- 在N-乙-[U-13C,15N]l-Val-l-Leu中精确测量了多个13C-13C距离 (3-6 Å),精度为+/-0.5 Å.
- 来自双旋转模型的距离约束与X射线晶体学数据有很好的一致性.
结论:
- R2W实验有利于提取结构和放松参数.
- R2W适用于均标记的生物系统,克服二极切断.
- 这种技术为固态结构分析提供了准确和特定地点的距离测量.
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