Solid-state NMR of a paramagnetic DIAD-FeII catalyst: sensitivity, resolution enhancement, and structure-based assignments |
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Authors: | Kervern Gwendal Pintacuda Guido Zhang Yong Oldfield Eric Roukoss Charbel Kuntz Emile Herdtweck Eberhardt Basset Jean-Marie Cadars Sylvian Lesage Anne Copéret Christophe Emsley Lyndon |
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Affiliation: | Laboratoire de Chimie, UMR 5182 CNRS-ENS Lyon, Ecole Normale Supérieure de Lyon, 46 Allée d'Italie, 69364 Lyon Cedex 07, France. |
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Abstract: | A general protocol for the structural characterization of paramagnetic molecular solids using solid-state NMR is provided and illustrated by the characterization of a high-spin Fe(II) catalyst precursor. We show how good NMR performance can be obtained on a molecular powder sample at natural abundance by using very fast (>30 kHz) magic angle spinning (MAS), even though the individual NMR resonances have highly anisotropic shifts and very short relaxation times. The results include the optimization of broadband heteronuclear (proton-carbon) recoupling sequences for polarization transfer; the observation of single or multiple quantum correlation spectra between coupled spins as a tool for removing the inhomogeneous bulk magnetic susceptibility (BMS) broadening; and the combination of NMR experiments and density functional theory calculations, to yield assignments. |
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