Anisotropic NMR data acquisition with a prototype 400 MHz cryogen-free NMR spectrometer

• Published in: Magnetic resonance in chemistry 2023-09, Vol.61 (9-10), p.530-543
• Main Authors: Silva Elipe, Maria Victoria, Ndukwe, Ikenna Edward, Navarro-Vázquez, Armando
• Format: Article
• Language: English
• ISSN: 0749-1581; 1097-458X
• DOI: 10.1002/mrc.5380

High-temperature superconducting (HTS) materials have recently been incorporated into the construction of HTS cryogen-free magnets for nuclear magnetic resonance (NMR) spectroscopy. These HTS NMR spectrometers do not require liquid cryogens, thereby providing significant cost savings and facilitating easy integration into chemistry laboratories. However, the optimal performance of these HTS magnets against standard cryogen NMR magnets must be evaluated, especially with demanding modern NMR applications such as NMR in anisotropic media. The stability of the HTS magnets over time and their performance with complex pulse sequence experiments are the main unknown factors of this new technology. In this study, we evaluate the utility of our prototype 400 MHz cryogen-free power-driven HTS NMR spectrometer, installed in the fumehood of a chemistry laboratory, for stereochemical analysis of three commercial natural products (artemisinin, artemether, and dihydroartemisinin) via measurement of anisotropic NMR data, in particular, residual dipolar couplings. The accuracy of measurement of the anisotropic NMR data with the HTS magnet spectrometer is evaluated through the CASE-3D fitting protocol, as implemented in the Mestrenova-StereoFitter software program.