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On the performance of Spin Diffusion NMR Techniques in Oriented Solids: Prospects for Resonance Assignments and Distance Measurements from Separated Local Field Experiments

机译：关于取向固体旋转扩散NMR技术的性能：共振分配的前景和分离的本地实地实验的距离

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NMR spin diffusion experiments have the potential to provide both resonance assignment and internuclear distances for protein structure determination in oriented solid-state NMR. In this paper, we compared the efficiencies of three common spin diffusion experiments: proton-driven spin diffusion (PDSD), cross-relaxation driven spin diffusion (CRDSD), and proton-mediated proton transfer (PMPT). As model systems for oriented proteins, we used single crystals of N-acetyl-L-15N-leucine (NAL) and N-acetyl-L-15N-valyl-L-15N-leucine (NAVL) to probe long- and short distances, respectively. We demonstrate that for short 15N/15N distances such as those found in NAVL (3.3 Å), the PDSD mechanism gives the most intense cross-peaks, while for longer distances (> 6.5 Å), the CRDSD and PMPT experiments are more efficient. The PDSD was highly inefficient for transferring magnetization across distances greater than 6.5 Å (NAL crystal sample), due to small 15N/15N dipolar couplings (< 4.5 Hz). Interestingly, the mismatched Hartmann-Hahn condition present in the PMPT experiment gave more intense cross-peaks for lower 1H and 15N spinlock field strengths (32 and 17 kHz, respectively) rather than higher values (55 and 50 kHz), suggesting a more complex magnetization transfer mechanism. Numerical simulations are in good agreement with the experimental findings, suggesting a combined PMPT and CRDSD effect. We conclude that in order to assign SLF spectra and measure short and long-range distances, the combined use of homonuclear correlation spectra, such as the ones surveyed in this work, are necessary.

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