Probing Interactions of N-Donor Molecules with Open Metal Sites within Paramagnetic Cr-MIL-101: A Solid-State NMR Spectroscopic and Density Functional Theory Study.

Understanding host-guest interactions is one of the key requirements for adjusting properties in metal- organic frameworks (MOFs). In particular, systems with coordinatively unsaturated Lewis acidic metal sites feature highly selective adsorption processes. This is attributed to strong interactions...

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Published in:Journal of the American Chemical Society Vol. 140; no. 6; pp. 2135 - 2145
Main Authors: Wittmann, Thomas, Mondal, Arobendo, Tschense, Carsten B. L., Wittmann, Johannes J., Klimm, Ottokar, Siegel, Renée, Corzilius, Björn, Weber, Birgit, Kaupp, Martin, Senker, Juergen
Format: Article
Published: American Chemical Society 2/14/2018
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Online Access:View this record in EBSCOhost
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      dt: 2/14/2018
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      pub: American Chemical Society
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        10.1021/jacs.7b10148
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        atl: Probing Interactions of N-Donor Molecules with Open Metal Sites within Paramagnetic Cr-MIL-101: A Solid-State NMR Spectroscopic and Density Functional Theory Study.
      aug:
        au:
          Wittmann, Thomas
          Mondal, Arobendo
          Tschense, Carsten B. L.
          Wittmann, Johannes J.
          Klimm, Ottokar
          Siegel, Renée
          Corzilius, Björn
          Weber, Birgit
          Kaupp, Martin
          Senker, Juergen
        affil:
          Inorganic Chemistry III, University of Bayreuth, Universitätsstraße 30, 95447 Bayreuth, Germany
          Institute of Chemistry, Theoretical Chemistry/Quantum Chemistry, Technical University of Berlin, Sekr. C7, Straße des 17. Juni 135, 10623 Berlin, Germany
          Institute of Physical and Theoretical Chemistry and Institute of Biophysical Chemistry, Goethe University Frankfurt, Max-von-Laue-Straße 7-9, 60438 Frankfurt am Main, Germany
          Inorganic Chemistry II, University of Bayreuth, Universitätsstraße 30, 95447 Bayreuth, Germany
      su:
        Metal-organic frameworks
        Density functional theory
        Diethylamine
        Thermogravimetry
        Hyperfine coupling
        Nuclear magnetic resonance
      sug:
        subj:
          Metal-organic frameworks
          Density functional theory
          Diethylamine
          Thermogravimetry
          Hyperfine coupling
          Nuclear magnetic resonance
      ab: Understanding host-guest interactions is one of the key requirements for adjusting properties in metal- organic frameworks (MOFs). In particular, systems with coordinatively unsaturated Lewis acidic metal sites feature highly selective adsorption processes. This is attributed to strong interactions with Lewis basic guest molecules. Here we show that a combination of C MAS NMR spectroscopy with state-of-the-art density functional theory (DFT) calculations allows one to unravel the interactions of water, 2-aminopyridine, 3-aminopyridine, and diethylamine with the open metal sites in Cr-MIL-101. The C MAS NMR spectra, obtained with ultrafast magic-angle spinning, are well resolved, with resonances distributed over 1000 ppm. They present a clear signature for each guest at the open metal sites. Based on competition experiments this leads to the following binding preference: water < diethylamine ≈ 2-aminopyridine < 3-aminopyridine. Assignments were done by exploiting distance sum relations derived from spin-lattice relaxation data and C{¹H} REDOR spectral editing. The experimental data were used to validate NMR shifts computed for the Cr-MIL-101 derivatives, which contain CrO clusters with magnetically coupled metal centers. While both approaches provide an unequivocal assignment and the arrangement of the guests at the open metal sites, the NMR data offer additional information about the guest and framework dynamics. We expect that our strategy has the potential for probing the binding situation of adsorbate mixtures at the open metal sites of MOFs in general and thus accesses the microscopic interaction mechanisms for this important material class, which is essential for deriving structure-property relationships.
      pubtype: Academic Journal
      doctype: Article
      src: R
    language: English
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