Michaelis Vladimir K, Ong Ta-Chung, Kiesewetter Matthew K, Frantz Derik K, Walish Joseph J, Ravera Enrico, Luchinat Claudio, Swager Timothy M, Griffin Robert G
Department of Chemistry, Massachusetts Institute of Technology, Cambridge, Massachusetts, 02139, USA.
Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, Massachusetts, 02139, USA.
Isr J Chem. 2014 Feb;54(1-2):207-221. doi: 10.1002/ijch.201300126. Epub 2014 Feb 13.
We report our recent efforts directed at improving high-field DNP experiments. We investigated a series of thiourea nitroxide radicals and the associated DNP enhancements ranging from ε = 25 to 82 that demonstrate the impact of molecular structure on performance. We directly polarized low-gamma nuclei including C, H, and O using trityl via the cross effect. We discuss a variety of sample preparation techniques for DNP with emphasis on the benefit of methods that do not use a glass-forming cryoprotecting matrix. Lastly, we describe a corrugated waveguide for use in a 700 MHz / 460 GHz DNP system that improves microwave delivery and increases enhancements up to 50%.
我们报告了近期在改进高场动态核极化(DNP)实验方面所做的努力。我们研究了一系列硫脲氮氧化物自由基以及相关的DNP增强因子,其范围从ε = 25到82,这展示了分子结构对性能的影响。我们通过交叉效应使用三苯甲基直接极化包括碳(C)、氢(H)和氧(O)在内的低γ核。我们讨论了多种用于DNP的样品制备技术,重点强调了不使用形成玻璃的冷冻保护基质的方法的优势。最后,我们描述了一种用于700 MHz / 460 GHz DNP系统的波纹波导,它改善了微波传输,并将增强因子提高了50%。