Mechanochemical Synthesis, Characterization, and Structure Determination of New Alkaline Earth Metal-Tetrafluoroterephthalate Frameworks: Ca(pBDC-F4)·4H2O, Sr(pBDC-F4)·4H2O, and Ba(pBDC-F4)

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• 作者：Abdal-Azim Al-Terkawi ; Gudrun Scholz ; Franziska Emmerling ; Erhard Kemnitz
• 刊名：Crystal Growth & Design
• 出版年：2016
• 出版时间：April 6, 2016
• 年：2016
• 卷：16
• 期：4
• 页码：1923-1933
• 全文大小：805K
• ISSN：1528-7505

文摘

New fluorinated alkaline earth metal–organic frameworks were successfully synthesized by milling of metal hydroxides M(OH)₂ with tetrafluoroterephthalic acid H₂pBDC-F₄. Both calcium- and strontium-tetrafluoroterephthalates are tetrahydrated, while the barium tetrafluoroterephthalate is free of coordinating water molecules. The two isomorphic structures Ca(pBDC-F₄)·4H₂O and Sr(pBDC-F₄)·4H₂O were solved from the powder diffraction data by ab initio structure determination and subsequent Rietveld refinement. The products were thoroughly characterized by elemental analysis, thermal analysis, magic-angle spinning NMR, Fourier transform infrared spectroscopy, scanning electron microscopy imaging, and Brunauer–Emmett–Teller measurements. Our findings suggest that the mechanochemical synthesis route is a promising approach for the preparation of new fluorinated alkaline earth metal–organic frameworks.