Mechanochemical Synthesis of New Coordination Polymers with Acetylenedicarboxylate as Bridging Ligand

• Published in: ZAAC - Journal of Inorganic and General Chemistry Vol. 636; no. 2; pp. 400 - 404
• Main Authors: Stein, Irena, Ruschewitz, Uwe
• Format: Book Review Journal Article
• Language: English
• Published: Weinheim WILEY-VCH Verlag 01.02.2010; WILEY‐VCH Verlag; Wiley-VCH Verlag
• Subjects: Acetylenedicarboxylate; Alkaline earth metals; Coordination polymers; Mechanochemical synthesis; X-ray diffraction; Physical Sciences
• ISSN: 0044-2313; 1521-3749
• DOI: 10.1002/zaac.200900368

CaADC (1) and Mg(ADC)(H2O)2 (2) were synthesized by grinding Ca(CH3COO)2 and Mg(CH3COO)2·4H2O with acetylenedicarboxylic acid (H2ADC) in an agate mortar. After careful heating for two hours in an argon atmosphere at moderate temperatures, 50 °C and 70 °C, respectively, polycrystalline materials of good crystallinity were obtained. The crystal structures of 1 and 2 were solved and refined from X‐ray powder diffraction data. In the course of the structural refinement it turned out that 1 and 2 are isotypic to SrADC(I41/amd, Z = 4) and Mn(ADC)(H2O)2 (I2/a, Z = 4). In both compounds metal cations are connected by bridging ADC2– ligands to form a 3D coordination network. Thermoanalytical investigations show that CaADC decomposes above 50 °C, whereas for Mg(ADC)(H2O)2 a mass loss of approx. 33 % is observed above 150 °C. The loss of one water molecule as well as a decarboxylation is very likely. The remaining residue is amorphous to X‐rays.