Michaelis, Vladimir K., Eric G. Keeler, Salima Bahri, Ta-Chung Ong, Eugenio Daviso, Michael T. Colvin, and Robert G. Griffin. “Biradical Polarizing Agents at High Fields.” The Journal of Physical Chemistry B, October 4, 2022.
https://doi.org/10.1021/acs.jpcb.2c03985.
The sensitivity enhancements available from dynamic nuclear polarization (DNP) are rapidly reshaping the research landscape and expanding the field of nuclear magnetic resonance (NMR) spectroscopy as a tool for solving complex chemical and structural problems. The past decade has seen considerable advances in this burgeoning method, while efforts to further improve its capabilities continue along many avenues. In this report, we examine the influence of static magnetic field strength and temperature on the reported 1H DNP enhancements from three conventional organic biradicals: TOTAPOL, AMUPol, and SPIROPOL. In contrast to the conventional wisdom, our findings show that at liquid nitrogen temperatures and 700 MHz/460.5 GHz, these three bisnitroxides all provide similar 1H DNP enhancements, ε ≈ 60. Furthermore, we investigate the influence of temperature, microwave power, magnetic field strength, and protein sample deuteration on the NMR experimental results.