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Improved detection of long-range residual dipolar couplings in weakly aligned samples by Lee-Goldburg decoupling of homonuclear dipolar truncation

机译:Lee-Goldburg解耦同核偶极截断

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摘要

Homonuclear (1)H residual dipolar couplings (RDCs) truncate the evolution of transverse (1)H magnetization of weakly aligned molecules in high-resolution NMR experiments. This leads to losses in sensitivity or resolution in experiments that require extended (1)H evolution times. Lee-Goldburg decoupling schemes have been shown to remove the effects of homonuclear dipolar couplings, while preserving chemical shift evolution in a number of solid-state NMR applications. Here, it is shown that the Lee-Goldburg sequence can be effectively incorporated into INEPT- or HMQC-type transfer schemes in liquid state weak alignment experiments in order to increase the efficiency of the magnetization transfer. The method is applied to the sensitive detection of (1)H(N)-(13)C long-range RDCs in a three-dimensional HCN experiment. As compared to a conventional HCN experiment, an average sensitivity increase by a factor of 2.4 is obtained for a sample of weakly aligned protein G. This makes it possible to detect 170 long-range (1)H(N)-(13)C RDCs for distances up to 4.9 angstroms.
机译:在高分辨率NMR实验中,全核(1)H残留偶极耦合(RDC)截断了弱对齐分子的横向(1)H磁化的演化。这会导致需要延长(1)H进化时间的实验导致灵敏度或分辨率下降。 Lee-Goldburg解耦方案已显示出消除同核偶极偶合的影响,同时在许多固态NMR应用中保留了化学位移的演变。在此显示,在液态弱取向实验中,Lee-Goldburg序列可以有效地并入INEPT型或HMQC型转移方案中,以提高磁化转移的效率。该方法应用于三维HCN实验中灵敏检测(1)H(N)-(13)C远程RDC。与常规HCN实验相比,弱对齐的蛋白G样品的平均灵敏度提高了2.4倍。这使得检测170个远程(1)H(N)-(13)C成为可能RDC的最大距离为4.9埃。

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