19 F-detected dual-optimized inverted 1 JCC 1,n-ADEQUATE

Ronald C Crouch; Jeffrey G Raab; Marius Pelmuş; Evgeny Tischenko; Michael Frey; Alexei V Buevich; Mikhail Reibarkh; R Thomas Williamson; Gary E Martin

doi:10.1002/mrc.5215

¹⁹ F-detected dual-optimized inverted ¹ J_CC 1,n-ADEQUATE

Magn Reson Chem. 2022 Feb;60(2):210-220. doi: 10.1002/mrc.5215. Epub 2021 Oct 6.

Authors

Ronald C Crouch¹, Jeffrey G Raab², Marius Pelmuş^{3

4}, Evgeny Tischenko¹, Michael Frey¹, Alexei V Buevich⁵, Mikhail Reibarkh⁵, R Thomas Williamson², Gary E Martin³

Affiliations

¹ Analytical Instruments, JEOL USA Inc., Peabody, MA, USA.
² Department of Chemistry and Biochemistry, University of North Carolina Wilmington, Wilmington, NC, USA.
³ Department of Chemistry, Seton Hall University, South Orange, NJ, USA.
⁴ Merck and Co., Inc., Kenilworth, NJ, USA.
⁵ Analytical Research and Development, Merck and Co., Inc., Rahway, NJ, USA.

PMID: 34469610
DOI: 10.1002/mrc.5215

Abstract

Modification of the recently reported ¹⁹ F-detected 1,1-ADEQUATE experiment that incorporates dual-optimization to selectively invert a wide range of ¹ J_CC correlations in a 1,n-ADEQUATE experiment is reported. Parameters for the dual-optimization segment of the pulse sequence were modified to accommodate the increased size of ¹ J_CC homonuclear coupling constants of poly- and perfluorinated molecules relative to protonated molecules to allow broadband inversion of the ¹ J_CC correlations. The observation and utility of isotope shifts are reported for the first time for 1,1- and 1,n-ADEQUATE correlations.

Keywords: 1,1-ADEQUATE; 1,n-ADEQUATE; 19F-detection; dual-optimization; isotope shifts.