Takegoshi K, Terao T
Department of Chemistry, Graduate School of Science, Kyoto University, Japan.
Solid State Nucl Magn Reson. 1999 May;13(4):203-12. doi: 10.1016/s0926-2040(99)00005-3.
A new solid-state NMR pulse sequence for recoupling 13C-1H dipolar interactions under magic-angle spinning is proposed, which works under a spinning speed of a few to several tens kilohertz. The sequence is composed of two different frequency switched Lee-Goldburg sequences, and the modulation of the spin part of the 13C-1H dipolar interaction is introduced by a virtual pulse sequence consisting of unitary operators connecting the rotating frame and the tilted rotating frame. When the cycle time of the spinning is equal to or twice the cycle time of the sequence, the 13C-1H dipolar interactions can be recoupled. The sequence is insensitive to experimental imperfections such as rf inhomogeneity or frequency offset, and the resulting lineshape can be represented by a simple analytical equation based on the zeroth-order average Hamiltonian. Experimental results for [2-(13)C] L-valine x HCl are reported.
提出了一种用于在魔角旋转下重新耦合¹³C-¹H偶极相互作用的新型固态核磁共振脉冲序列,该序列在几到几十千赫兹的旋转速度下工作。该序列由两个不同的频率切换李-戈德堡序列组成,¹³C-¹H偶极相互作用自旋部分的调制由一个由连接旋转坐标系和倾斜旋转坐标系的酉算符组成的虚拟脉冲序列引入。当旋转的循环时间等于或两倍于序列的循环时间时,¹³C-¹H偶极相互作用可以重新耦合。该序列对诸如射频不均匀性或频率偏移等实验缺陷不敏感,并且所得的线形可以由基于零阶平均哈密顿量的简单解析方程表示。报道了[2-(¹³)C]L-缬氨酸×HCl的实验结果。