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Issue 7, 2018
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Hydrated and dehydrated Ca-coordination polymers based on benzene-dicarboxylates: mechanochemical synthesis, structure refinement, and spectroscopic characterization

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Abstract

A series of Ca-based coordination polymers were prepared mechanochemically by milling Ca(OH)2 with phthalic acid (H2oBDC), isophthalic acid (H2mBDC), and terephthalic acid (H2pBDC). The hydrated compounds [Ca(oBDC)(H2O)] (1), [Ca(mBDC)(H2O)3.4] (2), and [Ca(pBDC)(H2O)3] (3) were prepared for the first time via mechanochemical routes. The refined structures were validated by extended X-ray absorption data. The new dehydrated compound [Ca(oBDC)] (1-H2O), obtained after the thermal post-treatment of 1 in a reversible phase transition process, was determined ab initio based on the powder X-ray diffraction (PXRD) data. The materials were thoroughly characterized using elemental analysis, thermal analysis, and spectroscopic methods: magic-angle spinning NMR and attenuated total reflection-infrared spectroscopy. The specific surface areas and sorption properties of the hydrated and dehydrated samples were determined using the isotherms of gas sorption and dynamic vapor sorption measurements.

Graphical abstract: Hydrated and dehydrated Ca-coordination polymers based on benzene-dicarboxylates: mechanochemical synthesis, structure refinement, and spectroscopic characterization

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Publication details

The article was received on 02 Nov 2017, accepted on 27 Dec 2017 and first published on 27 Dec 2017


Article type: Paper
DOI: 10.1039/C7CE01906H
Citation: CrystEngComm, 2018,20, 946-961
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    Hydrated and dehydrated Ca-coordination polymers based on benzene-dicarboxylates: mechanochemical synthesis, structure refinement, and spectroscopic characterization

    A. Al-Terkawi, G. Scholz, C. Prinz, A. Zimathies, F. Emmerling and E. Kemnitz, CrystEngComm, 2018, 20, 946
    DOI: 10.1039/C7CE01906H

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