Direct 15N–13C Heteronuclear Correlation Spectroscopy Enhanced by Spin-Lock-Induced Crossing and Reversible Parahydrogen Exchange

Direct 15N–13C Heteronuclear Correlation Spectroscopy Enhanced by Spin-Lock-Induced Crossing and Reversible Parahydrogen Exchange Full article

Journal

The Journal of Physical Chemistry Letters
ISSN: 1948-7185

Output data

Year: 2026, Volume: 17, Number: 33, Pages: 9669-9676 Pages count : 8 DOI: 10.1021/acs.jpclett.6c01774

Authors

Markelov Danil A. ^1,2 , Kiryutin Alexey S. ¹ , Chukanov Nikita V. ¹ , Kireev Nikolay V. ³ , Sheberstov Kirill F. ² , Yurkovskaya Alexandra V. ¹

Affiliations

1	International Tomography Center, Siberian Branch of the Russian Academy of Science, Novosibirsk 630090, Russia;
2	Chimie Physique et Chimie du Vivant (CPCV, UMR 8228), Departement de Chimie, Ecole Normale Superieure, PSL University, Sorbonne Universite, Paris 75005, France
3	Nesmeyanov Institute of Organoelement Compounds of Russian Academy of Science, Moscow 119334, Russia

Direct observation of 15N–13C heteronuclear correlations by conventional thermal NMR is limited by the low sensitivity of both nuclei. To overcome this limitation, we use low-field spin-lock-induced crossing signal amplification by reversible exchange (SLIC-SABRE) hyperpolarization to perform 15N–13C correlation spectroscopy in 15N-labeled small molecules containing 13C at natural abundance (1.1%). In SLIC-SABRE, polarization is transferred from parahydrogen to the substrate during their reversible interactions with an Ir-based complex. By tailoring the hyperpolarized spin order generated by SLIC-SABRE and the subsequent detection pathway, complementary one- and two-dimensional experiments with 15N and 13C detection provide site-specific connectivities, resolved 15N–13C J-couplings, and 13C-induced isotope shifts of the 15N resonances. The approach is demonstrated for a selenadiazole derivative and metronidazole, with two-dimensional 15N–13C correlation spectra acquired in approximately 40 min. Together, these results demonstrate the potential of SLIC-SABRE for rapid, site-resolved heteronuclear correlation spectroscopy.

Markelov D.A. , Kiryutin A.S. , Chukanov N.V. , Kireev N.V. , Sheberstov K.F. , Yurkovskaya A.V.
Direct 15N–13C Heteronuclear Correlation Spectroscopy Enhanced by Spin-Lock-Induced Crossing and Reversible Parahydrogen Exchange
The Journal of Physical Chemistry Letters. 2026. V.17. N33. P.9669-9676. DOI: 10.1021/acs.jpclett.6c01774 WOS Scopus OpenAlex

Submitted:	May 29, 2026
Accepted:	Jul 28, 2026
Published online:	Jul 31, 2026

≡ Web of science:	WOS:001838492100001
≡ Scopus:	2-s2.0-105047888719
≡ OpenAlex:	W7172397847