HNCO-based measurement of one-bond amide 15N-1H couplings with optimized precision.
HNCO-based measurement of one-bond amide 15N-1H couplings with optimized precision.
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DOI：
10.1007/s10858-009-9391-2
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发表时间：
2010-02
影响因子：
2.7
通讯作者：
Tolman JR
中科院分区：
文献类型：
--
作者：
Arbogast L;Majumdar A;Tolman JR
一对三维HNCO为基础的实验已经开发的目的是优化测量精度的1 JNH耦合。这两个脉冲序列记录了15 N磁化相对于直接键合的13 C ′核退相或再定相的整个恒定时间间隔内的1 JNH耦合演化，在13 C ′演化期间保持了15 N 13 C ′的多重量子相干性。第一个实验，设计用于较小的蛋白质，产生了明显的加倍的1 JNH耦合没有任何伴随的线宽增加。第二个实验是J标度的TROSY-HNCO实验，其中通过关于15 N偶极子的低场分量的位置对称偏移的谐振（即TROSY谐振）之间的频率差来测量1 JNH耦合。与现有的J标度TROSY-HNCO实验相比，该实验在1 JNH耦合测量的精度方面提供了显著的增益。与适当的选择的采集参数和足够的灵敏度，以获得一个3D TROSY-HNCO实验，它示出，1 JNH耦合可以测量的精度接近或超过的测量精度的TROSY共振本身的频率可以确定。
A pair of 3D HNCO-based experiments have been developed with the aim of optimizing the precision of measurement of 1JNH couplings. Both pulse sequences record 1JNH coupling evolution during the entire constant time interval that 15N magnetization is dephasing or rephasing with respect to the directly bonded 13C′ nucleus, with 15N13C′ multiple quantum coherence maintained during the 13C′ evolution period. The first experiment, designed for smaller proteins, produces an apparent doubling of the 1JNH coupling without any accompanying increases in line width. The second experiment is a J-scaled TROSY-HNCO experiment in which the 1JNH coupling is measured by frequency difference between resonances offset symmetrically about the position of the downfield component of the 15N doublet (i.e. the TROSY resonance). This experiment delivers significant gains in precision of 1JNH coupling measurement compared to existing J-scaled TROSY-HNCO experiments. With the proper choice of acquisition parameters and sufficient sensitivity to acquire a 3D TROSY-HNCO experiment, it is shown that 1JNH couplings can be measured with a precision which approaches or exceeds the precision of measurement with which the frequency of the TROSY resonance itself can be determined.
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影响因子：
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作者：
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