An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.
Six complexes, rubidium and cesium 3,5-dinitropyrid-2-onate (2DNPO), 3,5-dinitropyrid-4-onate (4NDPO), 3,5-dinitropyrid-4-one-N-hydroxylate (4DNPNO), were synthesized and characterized by elemental analysis, FT-IR, TG-DTG and X-ray single-crystal diffraction analysis. All the complexes crystallized from water and one of them was a hydrate. Rubidium 3,5-dinitropyrid-4-one-N-hydroxylate was crystallized with the 1 : 2 stoichiometry as Rb[H(4DNPNO)2] upon absorption of carbon dioxide. The structural determinations showed that the coordination sphere around a metal centre is made up of oxygen atoms and nitrogen atoms, except for the 4DNPNO complexes, where the coordination sphere accommodates exclusively oxygen atoms. The coordination numbers of the metal centers vary from 8, 10, 11 to 12, while the ligands, each employing its pyridone tautomer, link with metal cations. Bridging oxygen atoms play an important role in construction of two- and/or three-dimensional networks of these complexes. Hydrogen bonding contributes to the connectivity within a given sheet in Rb[H(4DNPNO)2]; aromatic π–π stacking interactions exist only in Cs(4DNPNO). The interactions between metal atoms and ligands are generally very weak. The organization of all layer structures appears to be governed mainly by steric effects and electrostatic forces with very little directional influence of the cations. The thermogravimetric analyses of these complexes showed the following consecutive processes: loss of NO2 groups, collapse of the pyridyl ring backbones and finally inorganic residue formation. These complexes could be used as probes in template effects of heavy alkali-metal cations in the organization of biorelevant ligands and as environment-friendly energetic catalysts in solid propellants.
Three new energetic compounds, nickel(II) 3,5-dinitro-2-pyridonate (Ni(2DNPO)2(H2O)4, 1), copper(II) 3,5-dinitro-4-pyridonate (Cu(4DNPO)2(H2O)4, 2) and cobalt(II) 3,5-dinitro-4-pyridone-N-hydroxylate ([Co(4DNPOH)2(H2O)4] · 2DMF, 3 · 2DMF), were characterized by elemental analysis, FT–IR, TG-DSC and X-ray single crystal diffraction analysis. Complexes 1 and 2 are similar in structure with the metal ion coordinated by oxygen donors of four water molecules on the equatorial position and two nitrogen donors of the pyridone rings of two ligands in the axial positions. The cobalt(II) complex 3 · 2DMF is a heavily distorted octahedral geometry. The Co(II) has equatorial positions defined by oxygens of four water molecules. Its axial positions are filled with two oxygen atoms of the pyridone-N-hydroxylate of two ligands. The TG-DSC results reveal that 1 is the most stable, with higher initial thermal decomposition temperature and enthalpy. Based on the thermoanalyses, the nickel compound is a promising candidate as a component in catalyzed RDX-CMDB propellants in comparison with our earlier lead(II) analogs.
An efficient metal-free cyanoalkylation of 8-aminoquinoline and aniline-derived amides was achieved in the presence of K 2 S 2 O 8 . The method showed good substrate tolerance and also suitable for bromination and dimerization reactions.
The removal of Ni ion from an aqueous solution was carried out by solvent sublation of Ni-diacetyldioxime-sodium dodecylbenzensulphonic (sublate) into isopentanol. The ratio of surfactant to Ni-diacetyldioxime complex at 20:1 was most effective for the removal, with over 90% Ni ion removed from the aqueous solution within 1 h. The effects of electrolytes (e.g. NaCl), non-hydrophobic organics (e.g. ethanol) and pH of the solution upon the process were well studied. The removal rate was enhanced by higher airflow rates but almost independent on the volume of the organic solvent floating on the top of the aqueous column. The process of solvent sublation followed first order kinetics. A characteristic parameter, the apparent activation energy of attachment of the sublate to bubbles, was estimated to be 8.99 kJ/mol. Furthermore, the simulation of a mathematical model with the experiment data on the solvent sublation of Ni-diacetyldioxime-SDS was proved to be validated.
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