Restoring Resolution in Biological Solid-State NMR under Conditions of Off-Magic-Angle Spinning

被引:11
作者
Sarkar, Riddhiman [1 ,2 ]
Camargo, Diana C. Rodriguez [1 ,2 ]
Pintacuda, Guido [3 ]
Reif, Bernd [1 ,2 ]
机构
[1] Deutsch Forschungszentrum Gesundheit & Umwelt, Helmholtz Zentrum Munchen HMGU, D-85764 Neuherberg, Germany
[2] Tech Univ Munich, Dept Chem, Munich Ctr Integrated Prot Sci CIPS M, D-85747 Garching, Germany
[3] Univ Lyon, Inst Sci Analyt, Ctr RMN Tres Hauts Champs, F-69100 Villeurbanne, France
关键词
RESIDUAL DIPOLAR COUPLINGS; MAGNETIC-RESONANCE SPECTRA; SOLUBLE-PROTEIN COMPLEXES; CHEMICAL-SHIFT; ROTATING SOLIDS; T-2; RELAXATION; SPECTROSCOPY; DYNAMICS; INTERFERENCE; PERSPECTIVES;
D O I
10.1021/acs.jpclett.5b02467
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
Spin-state-selective excitation (S3E) experiments allow the selection of individual transitions in a coupled two spin system. We show that in the solid state, the dipole-dipole interaction (DD) between N-15 and H-1 in a H-1-N-15 bond and the chemical shift anisotropy (CSA) of 15N in an amide moiety mutually cancel each other for a particular multiplet component at high field, when the sample is spun off the magic angle (Arctan [root 2] = 54.74 degrees). The accuracy of the adjustment of the spinning angle is crucial in conventional experiments. We demonstrate that for S3E experiments, the requirement to spin the sample exactly at the magic angle is not mandatory. Applications of solid state NMR in narrow bore magnets will be facilitated where the adjustment of the magic angle is often difficult. The method opens new perspectives for the development of schemes to determine distances and to quantify dynamics in the solid state.
引用
收藏
页码:5040 / 5044
页数:5
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