Solid-State NMR of a Paramagnetic DIAD-FeII Catalyst: Sensitivity, Resolution Enhancement, and Structure-Based Assignments
| Autor: | Charbel Roukoss, Christophe Copéret, Lyndon Emsley, Eberhardt Herdtweck, Eric Oldfield, Emile Kuntz, Gwendal Kervern, Jean Marie Basset, Yong Zhang, Guido Pintacuda, Anne Lesage, Sylvian Cadars |
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| Přispěvatelé: | Laboratoire de Chimie - UMR5182 (LC), École normale supérieure de Lyon (ENS de Lyon)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Anorganisch-chemisches Institut, Technische Universität Munchen - Université Technique de Munich [Munich, Allemagne] (TUM), Laboratoire de Chimie, Catalyse, Polymères et Procédés, R 5265 (C2P2), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-École Supérieure de Chimie Physique Électronique de Lyon (CPE)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Conditions Extrêmes et Matériaux : Haute Température et Irradiation (CEMHTI), Université d'Orléans (UO)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratory for Inorganic, Eidgenössische Technische Hochschule - Swiss Federal Institute of Technology [Zürich] (ETH Zürich), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-École normale supérieure - Lyon (ENS Lyon)-Institut de Chimie du CNRS (INC), Centre National de la Recherche Scientifique (CNRS)-École supérieure de Chimie Physique Electronique de Lyon (CPE)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC) |
| Rok vydání: | 2006 |
| Předmět: |
Magnetic Resonance Spectroscopy
Magic angle Cations Divalent Carbon-13 NMR satellite Iron Analytical chemistry Fluorine-19 NMR Crystallography X-Ray 010402 general chemistry 01 natural sciences Biochemistry Catalysis Magnetics Colloid and Surface Chemistry Organometallic Compounds Magic angle spinning [CHIM]Chemical Sciences ComputingMilieux_MISCELLANEOUS Earth's field NMR Carbon Isotopes 010405 organic chemistry Chemistry General Chemistry Nuclear magnetic resonance spectroscopy Carbon-13 NMR Deuterium Carbon 0104 chemical sciences Solid-state nuclear magnetic resonance Anisotropy Quantum Theory Spin Labels Condensed Matter::Strongly Correlated Electrons Protons Algorithms |
| Zdroj: | Journal of the American Chemical Society Journal of the American Chemical Society, 2006, 128 (41), pp.13545-13552. ⟨10.1021/ja063510n⟩ Journal of the American Chemical Society, American Chemical Society, 2006, 128 (41), pp.13545-13552. ⟨10.1021/ja063510n⟩ |
| ISSN: | 1520-5126 0002-7863 |
| DOI: | 10.1021/ja063510n |
| Popis: | 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. |
| Databáze: | OpenAIRE |
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