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Syntheses,crystal structures and thermoanalyses of alkaline earth metal complexes derived from dinitropyridone
Abstract:Six new alkaline-earth metal compounds derived from dinitropyridone ligands (3,5-dinitropyrid-2-one, 2HDNP; 3,5-dinitropyrid-4-one, 4HDNP and 3,5-dinitropyrid-4-one-N-hydroxide, 4HDNPO) were synthesized and characterized by elemental analysis, FT-IR and partly by powder XRD, TG-DSC and X-ray single-crystal diffraction analysis. The structural determination revealed that one molecule of both magnesium salts (Mg(2DNP)2 ·?8H2O, (1), and Mg(4DNP)2 ·?6H2O (4)) comprise one cation [Mg(H2O)6]2+ and two anions displaying centro-symmetry with the Mg atom located at the center. Two anions (and crystalline water molecules) are joined by hydrogen bonds. The barium salt Ba(4DNP)2 ·?4H2O (5), is a centro-symmetric dimer with each Ba(II) being coordinated by one monodentate ligand anion, two bidentate ligand anions (different coordination pattern) and five water molecules. Another barium salt, Ba(4DNPO)2 ·?6H2O (6), is a coordination polymer, the ten-coordinate (BaO10) barium environment comprising four water molecules, a pair of 4DNPOs via the pyridine-N-oxide oxygen, and one 4DNPOs from an adjacent metal atom offering chelating nitro group oxygen, bridging adjacent bariums. Abundant intermolecular hydrogen bonds link the molecules of each complex into multi-dimensional chains. The X-ray powder diffraction analysis confirmed the phase homogeneity of the polycrystalline samples. The TG-DSC results revealed that Mg(2DNP)2 ·?8H2O and Ba(4DNP)2 ·?6H2O each has three main weight-loss stages. The first step is the loss of all water molecules and the last step is the loss of the nitro groups and/or decomposition of the pyridine rings with the release of heat.
Keywords:Alkaline-earth metal complex  Dinitropyridone  Crystal structure  Powder XRD  Thermoanalysis
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