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BaF-benzenedicarboxylate: the first mechanochemical synthesis of a new coordination polymer with a direct Ba–F bond

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Abstract

A new barium coordination polymer, BaF-benzenedicarboxylate (BaF(p-BDC)0.5), with fluorine directly coordinated to the metal cation, was prepared by mechanochemical synthesis routes. Phase-pure BaF-benzenedicarboxylate was synthesized by milling starting either from barium hydroxide or from barium acetate as sources for barium cations. In both cases, the second reactant was 1,4-benzenedicarboxylic acid (H2(p-BDC)). Ammonium fluoride was used as fluorinating agent directly at milling. This is the first mechanochemical synthesis of coordination polymers where fluorine is directly coordinated to the metal cation. Following the second possibility, barium acetate fluoride (Ba(OAc)F) is formed as intermediate product after milling, and the new coordination polymer is accessible only after washing with water and dimethyl sulfoxide. The new compound BaF(p-BDC)0.5 was characterized by X-ray powder diffraction, FTIR-, and 19F, 1H-13C CP MAS NMR spectroscopies, DTA-TG, and elemental analysis.

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Acknowledgements

We thank Dr. M. Feist (HU Berlin) for DTA-TG measurements, Dr. K. Scheurell (HU Berlin) for her contribution in MAS NMR measurements, Ms. Bäßler (HU Berlin) for fluorine analysis and Ms. Odoj (HU Berlin) for elemental analysis. Furthermore, we acknowledge Voraksmy Ban and N. Casati for the synchrotron X-ray diffraction measurements (Swiss Light Source, Paul Scherrer Institut).

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Authors and Affiliations

  1. Department of Chemistry, Humboldt-Universität zu Berlin, Brook-Taylor-Str. 2, 12489, Berlin, Germany

    S. Breitfeld, G. Scholz & E. Kemnitz

  2. Federal Institute for Materials Research and Testing (BAM), Richard-Willstätter-Str. 11, 12489, Berlin, Germany

    S. Breitfeld & F. Emmerling

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  1. S. Breitfeld
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  2. G. Scholz
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  4. E. Kemnitz
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Correspondence to G. Scholz or E. Kemnitz.

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Breitfeld, S., Scholz, G., Emmerling, F. et al. BaF-benzenedicarboxylate: the first mechanochemical synthesis of a new coordination polymer with a direct Ba–F bond. J Mater Sci 53, 13682–13689 (2018). https://doi.org/10.1007/s10853-018-2331-3

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  • DOI: https://doi.org/10.1007/s10853-018-2331-3

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