NMR Crystallography of an Oxovanadium(V) Complex by an Approach Combining Multinuclear Magic Angle Spinning NMR,DFT, and Spin Dynamics Simulations |
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| Authors: | Dr. Frédérique Pourpoint Jenna Yehl Mingyue Li Dr. Rupal Gupta Dr. Julien Trébosc Prof. Olivier Lafon Prof. Jean‐Paul Amoureux Prof. Tatyana Polenova |
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| Affiliation: | 1. Unité de Catalyse et de Chimie du Solide (UCCS), ENSCL, Université de Lille, CNRS UMR 8181, 59652 Villeneuve d'Ascq (France);2. Department of Chemistry and Biochemistry, University of Delaware, DE 19716 (USA);3. Physics Department & Shanghai Key Laboratory of Magnetic Resonance, East China Normal University, Shanghai 200062 (China) |
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| Abstract: | Bioinorganic vanadium(V) solids are often challenging for structural analysis. Here, we explore an NMR crystallography approach involving multinuclear 13C/51V solid‐state NMR spectroscopy, density functional theory (DFT), and spin dynamics numerical simulations, for the spectral assignment and the 3D structural analysis of an isotopically unmodified oxovanadium(V) complex, containing 17 crystallographically inequivalent 13C sites. In particular, we report the first NMR determination of C–V distances. So far, the NMR observation of 13C–51V proximities has been precluded by the specification of commercial NMR probes, which cannot be tuned simultaneously to the close Larmor frequencies of these isotopes (100.6 and 105.2 MHz for 13C and 51V, respectively, at 9.4 T). By combining DFT calculations and 13C–51V NMR experiments, we propose a complete assignment of the 13C spectrum of this oxovanadium(V) complex. Furthermore, we show how 13C–51V distances can be quantitatively estimated. |
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| Keywords: | bioinorganic chemistry coordination chemistry density functional calculations NMR spectroscopy vanadium |
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