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Updated: Aug 5, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
Published on: September 17, 2017
Direct 15N-13C Heteronuclear Correlation Spectroscopy Enhanced by Spin-Lock-Induced Crossing and Reversible
Danil A Markelov1,2, Alexey S Kiryutin1, Nikita V Chukanov1
1International Tomography Center, Siberian Branch of the Russian Academy of Science, Institutskaya 3A, Novosibirsk630090, Russia.
Abstract:
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.
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