Magic angle spinning (MAS) NMR is a powerful method for the study of pharmaceutical compounds, and probes with spinning frequencies above 100 kHz enable an atomic-resolution analysis of sub-micromole quantities of fully protonated solids. Here, we present an ultrafast NMR crystallography approach for structural characterization of organic solids at MAS frequencies of 100-111 kHz. We assess the efficiency of 1H-detected experiments in the solid state and demonstrate the utility of 2D and 3D homo- and heteronuclear correlation spectra for resonance assignments. These experiments are demonstrated for an amino acid, U-13C,15N-histidine, and also for the significantly larger, natural product Posaconazole, an antifungal compound investigated at natural abundance. Our results illustrate the power for characterizing organic molecules, enabled by exploiting the increased 1H resolution and sensitivity at MAS frequencies above 100 kHz.

中文翻译：

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天然丰度药物化合物的超快1H MAS NMR晶体学。

魔角旋转（MAS）NMR是研究药物化合物的有力方法，旋转频率高于100 kHz的探针可对亚微摩尔量的完全质子化固体进行原子分辨率分析。在这里，我们提出了一种用于在100-111 kHz的MAS频率下对有机固体进行结构表征的超快NMR晶体学方法。我们评估了固态下1H检测实验的效率，并证明了2D和3D同核和异核相关光谱用于共振分配的效用。这些实验针对氨基酸U-13C，15N-组氨酸进行了证明，还针对较大的天然产物Posaconazole（一种经自然丰度研究的抗真菌化合物）进行了证明。我们的结果说明了表征有机分子的能力，