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Synthesis, Crystal Structure, and Solid-State NMR Investigations of Heteronuclear Zn/Co Coordination Networks — A Comparative Study

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Universität Leipzig, Fakultät für Physik und Geowissenschaften, Linnéstr. 5, D-04103, Germany
Universität Leipzig, Fakultät für Chemie und Mineralogie, Johannisallee 29, D-04103, Germany
§ Universitè de Lyon, Centre de RMN à très hauts champs, CNRS/ENS Lyon/UCBL, 5 Rue de la Doua, 69100 Villeurbanne, France
Institut für Nichtklassische Chemie e. V., Permoserstr.15, D-04318, Germany
Department of Physics & Astronomy, University College London, Gower Street, London, United Kingdom
Cite this: Inorg. Chem. 2013, 52, 8, 4431–4442
Publication Date (Web):April 1, 2013
https://doi.org/10.1021/ic302643w
Copyright © 2013 American Chemical Society

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    Abstract

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    Synthesis and solid-state NMR characterization of two isomorphous series of zinc and cobalt coordination networks with 1,2,4-triazolyl benzoate ligands are reported. Both series consist of 3D diamondoid networks with four-fold interpenetration. Solid-state NMR identifies the metal coordination of the ligands, and assignment of all 1H and 13C shifts was enabled by the combination of 13C editing, FSLG-HETCOR spectra, and 2D 1H–1H back-to-back (BABA) spectra with results from NMR-CASTEP calculations. The incorporation of Co2+ replacing Zn2+ ions in the MOF over the full range of concentrations has significant influences on the NMR spectra. A uniform distribution of metal ions is documented based on the analysis of 1H T1 relaxation time measurements.

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    IR, thermogravimetric, and temperature-dependent PXRD data and atomic coordinates of 2 are given in the Supporting Information. It also contains various CP spectra using spectral editing techniques; tables for 13C and 1H assignments; and additional 1H 1D, 13C CPMAS, 2D HETCOR, and BABA spectra. This material is available free of charge via the Internet at http://pubs.acs.org. CCDC 852802 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.

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