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A New Tool for NMR Crystallography: Complete C-13/N-15 Assignment of Organic Molecules at Natural Isotopic Abundance Using DNP-Enhanced Solid-State NMR

Katharina Marker 1 Morgane Pingret 2 Jean-Marie Mouesca 1 Didier Gasparutto 2 Sabine Hediger 1 Gael de Paepe 1
1 RM [?-2019] - Magnetic Resonance [?-2019]
MEM - Modélisation et Exploration des Matériaux : DRF/IRIG/MEM
2 LAN - Laboratoire Lésions des Acides Nucléiques
SCIB - UMR E3 - Service de Chimie Inorganique et Biologique : DSM/INAC/SCIB
Abstract : NMR crystallography of organic molecules at natural isotopic abundance (NA) strongly relies on the comparison of assigned experimental and computed NMR chemical shifts. However, a broad applicability of this approach is often hampered by the still limited H-1 resolution and/or difficulties in assigning C-13 and N-15 resonances without the use of structure-based chemical shift calculations. As shown here, such difficulties can be overcome by C-13-C-13 and for the first time N-15-C-13 correlation experiments, recorded with the help of dynamic nuclear polarization. We present the complete de novo C-13 and N-15 resonance assignment at NA of a self-assembled 2'-deoxyguanosine derivative presenting two different molecules in the asymmetric crystallographic unit cell. This de novo assignment method is exclusively based on aforementioned correlation spectra and is an important addition to the NMR crystallography approach, rendering firstly H-1 assignment straightforward, and being secondly a prerequisite for distance measurements with solid-state NMR.
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https://hal-cea.archives-ouvertes.fr/cea-01734607
Contributor : Jérôme Planès <>
Submitted on : Wednesday, March 14, 2018 - 6:04:09 PM
Last modification on : Monday, July 20, 2020 - 2:04:02 PM

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Katharina Marker, Morgane Pingret, Jean-Marie Mouesca, Didier Gasparutto, Sabine Hediger, et al.. A New Tool for NMR Crystallography: Complete C-13/N-15 Assignment of Organic Molecules at Natural Isotopic Abundance Using DNP-Enhanced Solid-State NMR. Journal of the American Chemical Society, American Chemical Society, 2015, 137 (43), pp.13796-13799. ⟨10.1021/jacs.5b09964⟩. ⟨cea-01734607⟩

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