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Heterometallic M/Mn (M=Cu, Co, Zn) acetate complexes as precursors for binary oxides
Authors:Valeriya G Makhankova  Oleksiy V Khavryuchenko  Vladimir N Kokozay  Oleg V Shishkin  Brian W Skelton
Institution:a Department of Inorganic Chemistry, Kyiv National Taras Shevchenko University, Volodymyrska street 64, Kyiv 01601, Ukraine
b STC “Institute for Single Crystals” National Academy of Sciences of Ukraine, 60 Lenina Avenue Khark?v 61001, Ukraine
c Department of Inorganic Chemistry, V.N. Karazin Kharkiv National University, 4 Svobody sq., Kharkiv 61077, Ukraine
d Chemistry M313, School of Biomedical, Biomolecular and Chemical Sciences, University of Western Australia, 6009, Australia
e Faculty of Chemistry, University of Wroclaw, 14 F. Joliot-Curie, 50-383 Wroclaw, Poland
Abstract:A facile one-pot procedure, or so-called “direct synthesis,” was used to prepare the novel heterometallic complexes M2Mn(OAc)6(bpy)2], where M=Cu (1), Co (2), Zn (3), bpy=2,2′-bipyridyl, with high yields via oxidative dissolution of pure metals in a liquid phase. The complexes were characterized by an elemental analysis, single crystal X-ray diffraction method and FTIR. These complexes are proposed as precursors, whose thermal degradation may lead to the formation of solids possessing nano- to microsize levels of dispersity. The thermal behavior of the complexes obtained was studied by thermal analysis (TG/DTA/DTG) in both air and N2 and also by TPD mass-spectrometry in vacuo. The FTIR, X-ray powder diffraction (PXRD) and thermoanalytical data were used for the identification of the solid products of thermal degradation. The morphology and microstructure of the solid residues were analyzed, using scanning electron microscopy with energy dispersive X-ray microanalysis (SEM/EDX) at mkm and sub-micro levels.
Keywords:Heterometallic complexes  X-ray crystallography  X-ray powder diffraction  Thermogravimetric analysis  Temperature programmed desorption mass-spectrometry  SEM/EDX analysis
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