Hydrated and dehydrated Ca-coordination polymers based on benzene-dicarboxylates: mechanochemical synthesis, structure refinement, and spectroscopic characterization. Issue 7 (25th January 2018)

• Record Type: Journal Article
• Authors: Al-Terkawi, Abdal-Azim; Scholz, Gudrun; Prinz, Carsten; Zimathies, Annett; Emmerling, Franziska; Kemnitz, Erhard
• Is Part Of: CrystEngComm. Volume 20:Issue 7(2018)
• Page Start: 946
• Page End: 961
• Publication Date: 2018-01-25
• Subjects: Crystals -- Periodicals; Crystal growth -- Periodicals; Crystallography -- Periodicals; Cristaux -- Périodiques; Cristaux -- Croissance -- Périodiques; Cristallographie -- Périodiques; 548
• DOI: 10.1039/c7ce01906h
• Languages: English
• ISSNs: 1466-8033

Abstract

Abstract : Hydrated Ca-CPs were synthesized by milling. Dehydrated phases were obtained by thermal treatments in reversible processes. Abstract : A series of Ca-based coordination polymers were prepared mechanochemically by milling Ca(OH)2 with phthalic acid (H2 o BDC), isophthalic acid (H2 m BDC), and terephthalic acid (H2 p BDC). The hydrated compounds [Ca( o BDC)(H2 O)] (1 ), [Ca( m BDC)(H2 O)3.4 ] (2 ), and [Ca( p BDC)(H2 O)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( o BDC)] (1 -H 2 O ), obtained after the thermal post-treatment of1 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.