1. Synthesis, crystal structure and magnetic properties of a new hydroxylammonium fluoroferrateBrina Dojer, Matjaž Kristl, Zvonko Jagličić, Amalija Golobič, Marta Kasunič, Mihael Drofenik, 2012, izvirni znanstveni članek Opis: This paper reports on the synthesis of a new hydroxylammonium fluoroferrate, with the formula $(NH_3OH)_3FeF_6$, obtained after dissolving iron powder in hydrofluoric acid and adding solid $NH_3OHF$. This new compound has been characterized by chemical and thermal analysis, single-crystal X-ray diffraction, and magnetic measurements. The title compound crystallizes trigonal, R3c, with cell parameters a = 11.4154(2) Å, c = 11.5720(2) Å, Z = 6. The structure consists of $NH_3OH^+$ cations and isolated $FeF_6^{3–}$ octahedra in which the central ion lies on a threefold axis. The oxygen and nitrogen atoms of the hydroxylammonium cations are donors of hydrogen bonds to fluoride anions, resulting in a network of hydrogen bonds between counterions. The effective magnetic moment $µ_{eff}$ = 5.8 BM was calculated and perfectly matches the expected value of high-spin Fe(III) ions. The thermal decomposition of the compound was studied by TG, DSC, and X-ray powder diffraction.
Ključne besede: inorganic chemistry, crystallography, coordination compounds, synthesis, crystal structure, characterization of compounds, determination of the structure of compounds, X-ray diffraction, magnetic measurements, thermal analysis, TG, DSC, hydrogen bond, metal complexes, hydroxylammonium fluoromethalatehydroxylammonium, fluoroferrate
Objavljeno v DKUM: 25.08.2017; Ogledov: 2076; Prenosov: 70
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2. Synthesis and characterisation of hydroxylammonium fluorochromateMatjaž Kristl, Mihael Drofenik, Ljubo Golič, Amalija Golobič, 2003, izvirni znanstveni članek Opis: Reactions in the system $Cr – NH_3OHF – HF – H_2O$ were investigated. Green crystals of a new compound with the formula $(NH_3OH)_3CrF_6$ have been isolated from the water solution and characterized by chemical analysis. The compound crystallizes as triclinic, P-1, with cell parameters: a = 6.5461(2) Å, b = 6.9347(2) Å, c = 9.4072(3) Å, α = 86.772(1)°, β = 83.804(1)°, γ = 70.283(1)°. The effective magnetic moment, $µ_{eff}$ = 3.82 BM, was calculated from magnetic susceptibility measurements in the temperature range 80-290 K. The thermal decomposition of the compound was studied by TG and DSC analysis. $(NH_3OH)_3CrF_6$ decomposes above 125 °C in three steps and the residue has been identified by X-ray powder diffraction as $α – Cr_2O_3$.
Ključne besede: inorganic chemistry, structural chemistry, crystalline structure, coordination compounds, synthesis, inorganic reactions, thermal decomposition, characterization of compounds, TG, DSC, X-ray diffraction, chromium complexes, hydroxylammonium fluoro chromates, crystals
Objavljeno v DKUM: 25.08.2017; Ogledov: 1893; Prenosov: 115
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3. The crystal and molecular structures of two reaction products of geminal dicyano oxirane with thiohydantoine (compound I) and thioxobenzoxazole (compound II)Ivan Leban, Alenka Majcen Le Marechal, Albert Robert, 1993, izvirni znanstveni članek Opis: The crystal and molecular structures of two reaction products of geminal dicyano oxiranes with thiohydantoione and thioxobenzoxazole have been determinated from ▫$Mo-K_\alpha$▫ X-ray diffraction data. The two reaction products were: 2H-2-(p-tolyl)-imidazol[1,2-b]thiazole-3,6-dione (compound I) and Z-3-benzoxazole-3-phenyl-2-oxo-2-propanenitrile (compound II) with the following crystal data at 293(1) K: Compound I, ▫$C_{12}H_{10}N_2O_2S$▫, monoclinic ▫$P2_1/c$▫, a=15057(3), b=5.200(3), c=14.724(4) Å, ▫$\beta=104.24(3)°$▫, Z=4; final R and ▫$R_w$▫ values were 0.034 and 0.049 for1647 observed reflexions. Compound II, ▫$C_{16}H{10}N_2O_2$▫, monoclinic, ▫$P2_1/n$▫, a=14.396(3), b=4.326(1), c=21.335(4) Å, ▫$\beta-107.79(1)°$▫, Z=4;final R and ▫$R_w$▫ values 0.040 and 0.053 for 1516 observed reflections.
Ključne besede: organic chemistry, crystal structure, chemical reactions, oxiranes, coordination compounds, structural chemistry
Objavljeno v DKUM: 05.07.2017; Ogledov: 1572; Prenosov: 118
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