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Hydroxylammonium fluorometalates: Synthesis and characterisation of a new fluorocuprate and fluorocobaltate
Authors:Matja? Kristl  Brina Dojer  Amalija Golobi?  Miha Drofenik
Affiliation:a University of Maribor, Faculty of Chemistry and Chemical Engineering, Smetanova 17, SI-2000 Maribor, Slovenia
b University of Ljubljana, Faculty of Chemistry and Chemical Technology, Ašker?eva 5, SI-1000 Ljubljana, Slovenia
c Institute of Mathematics, Physics and Mechanics and Faculty of Civil and Geodetic Engineering, University of Ljubljana, Jadranska 19, SI-1000 Ljubljana, Slovenia
d Jo?ef Stefan Institute, Jamova 39, SI-1000 Ljubljana, Slovenia
Abstract:The first layered hydroxylammonium fluorometalates, (NH3OH)2CuF4 and (NH3OH)2CoF4, were prepared by the reaction of solid NH3OHF and the aqueous solution of copper or cobalt in HF. Both compounds crystallize in monoclinic, P21/c, unit cell with parameters: a = 7.9617(2) Å, b = 5.9527(2) Å, c = 5.8060(2) Å, β = 95.226(2)° for (NH3OH)2CuF4 and a = 8.1764(3) Å, b = 5.8571(2) Å, c = 5.6662(2) Å, β = 94.675(3)° for (NH3OH)2CoF4, respectively. Magnetic susceptibility was measured between 2 K and 300 K giving the effective Bohr magneton number of 2.1 for Cu and 5.2 BM for Co. At low temperatures both complexes undergo a transition to magnetically ordered phase. The thermal decomposition of both compounds was studied by TG, DSC and X-ray powder diffraction. The thermal decomposition of (NH3OH)2CuF4 is a complex process, yielding NH4CuF3 as an intermediate product and impure Cu2O as the final residue, while (NH3OH)2CoF4 decomposes in two steps, obtaining CoF2 after the first step and CoO as the final product.
Keywords:Cuprate   Cobaltate   Fluorides   X-ray diffraction   Hydrogen bond
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