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Insight into Magnesium Coordination Environments in Benzoate and Salicylate Complexes through 25Mg Solid-State NMR Spectroscopy
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    Insight into Magnesium Coordination Environments in Benzoate and Salicylate Complexes through 25Mg Solid-State NMR Spectroscopy
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    Department of Chemistry and Centre for Catalysis Research and Innovation, University of Ottawa, 10 Marie Curie Private, Ottawa, Ontario, Canada K1N 6N5
    *Tel: +1 613 562 5800 ext. 2018; fax: +1 613 562 5170; e-mail: [email protected]
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    The Journal of Physical Chemistry A

    Cite this: J. Phys. Chem. A 2013, 117, 30, 6561–6570
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    https://doi.org/10.1021/jp405145b
    Published July 8, 2013
    Copyright © 2013 American Chemical Society

    Abstract

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    We report on the 25Mg solid-state nuclear magnetic resonance (NMR) characterization of a series of magnesium complexes featuring Mg2+ ions in organic coordination environments. Six compounds have been synthesized with benzoate and salicylate ligands, which are typically used as linkers in metal organic frameworks (MOFs). The use of ultrahigh-field solid-state NMR has revealed a relatively large range of values for the 25Mg quadrupolar coupling constant, CQ(25Mg), in these compounds. In contrast to some previously studied inorganic Mg2+ complexes, the values of CQ(25Mg) in organic Mg2+ complexes are well rationalized by the degree of octahedral strain of the “MgO6” coordination polyhedra. 13C and 25Mg isotropic chemical shifts were also found to be sensitive to the binding mode of the carboxylate ligands. The experimental findings are corroborated by gauge-including projector-augmented-wave (GIPAW) density functional theory (DFT) computations, and these have allowed for an interpretation of the experimentally observed trend in the CQ(25Mg) values and for the visualization of the EFG tensor principal components with respect to the molecular structure. These new insights may prove to be valuable for the understanding and interpretation of 25Mg NMR data for Mg2+ ions in organic binding environments such as those found in MOFs and protein-divalent metal binding sites.

    Copyright © 2013 American Chemical Society

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    Supporting Information

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    X-ray diffractograms; additional experimental and computational details; additional spectra and figures; crystallographic information and cif for magnesium benzoate. This material is available free of charge via the Internet at http://pubs.acs.org.

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    Cited By

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    This article is cited by 11 publications.

    1. E. S. (Merijn) Blaakmeer, Giuseppe Antinucci, Vincenzo Busico, Ernst R. H. van Eck, and Arno P. M. Kentgens . Solid-State NMR Investigations of MgCl2 Catalyst Support. The Journal of Physical Chemistry C 2016, 120 (11) , 6063-6074. https://doi.org/10.1021/acs.jpcc.5b12606
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    The Journal of Physical Chemistry A

    Cite this: J. Phys. Chem. A 2013, 117, 30, 6561–6570
    Click to copy citationCitation copied!
    https://doi.org/10.1021/jp405145b
    Published July 8, 2013
    Copyright © 2013 American Chemical Society

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