20.500.12556/DKUM-67646 Synthesis, crystal structure and magnetic properties of a new hydroxylammonium fluoroferrate 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. V prispevku poročamo o sintezi novega hidroksilamonijevega fluorometalata s formulo $(NH_3OH)_3FeF_6$. Spojino smo pripravili z reakcijo med trdnim $NH_3OHF$ in vodno raztopino železa v $HF$. Spojino smo karakterizirali s kemijsko in termično analizo, rentgensko difrakcijo na monokristalu in magnetnimi meritvami. Hidroksilamonijev fluoroferat kristalizira trigonalno, R3c, s parametri osnovne celice a = 11.4154(2) Å, c = 11.5720(2) Å, Z = 6. Strukturo sestavljajo kationi $NH_3OH^+$ in izolirani oktaedri $FeF_6^{3–}$, v katerih centralni atom leži na trištevni osi. Kisikovi in dušikovi atomi v hidroksilamonijevih kationih so donorji vodikovih vezi do fluoridnih anionov, kar povzroči nastanek mreže vodikovih vezi. Izračunani efektivni magnetni moment $µ_{eff}$ = 5.8 BM se odlično ujema s teoretično vrednostjo za visokospinske Fe(III) ione. Termični razkroj spojine smo preučevali s termogravimetrično metodo in rentgensko praškovno analizo. 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 anorganska kemija kristalografija koordinacijske spojine sinteza kristalna struktura karakterizacija spojin določitev strukture spojin rentgenska difrakcija magnetne meritve termična analiza TG DSC vodikova vez kovinski kompleksi hidroksilamonijev fluorometalat true false true Angleški jezik Slovenski jezik Znanstveno delo 2017-08-25 12:21:34 2017-08-25 12:22:47 2022-08-01 14:16:43 2019-07-11 16:26:41 2012 0 0 str. 789-794 št. 4 Letn. 59 2012 0000-00-00 Zaloznikova Objavljeno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 1318-0207 546.726.022.057:543.442.3:543.57 14086149 36480005 1318-0207 URN:SI:UM:DK:JL67D6WV Acta_Chimica_Slovenica_2012_Dojer_et_al._Synthesis,_Crystal_Structure_and_Magnetic_Properties_of_a_new_Hydroxylammonium_Fluoroferrate.pdf Acta_Chimica_Slovenica_2012_Dojer_et_al._Synthesis,_Crystal_Structure_and_Magnetic_Properties_of_a_new_Hydroxylammonium_Fluoroferrate.pdf 1 B5AE4B5C1191951D8367D0CD0095A1DF 4dc01fedb1e8e2099b92cfa3404e91a4b9fc65b3ad88b11f2b09087a5c9d5d72 90913958-7c0e-11eb-bb7a-00155d0001ca 20.500.12556/dkum/0dbe66c6-d7b1-4633-8a6c-1fd7823301b4 https://dk.um.si/Dokument.php?lang=slv&id=116064 http://acta-arhiv.chem-soc.si/59/59-4-789.pdf 1 https://dk.um.si/Dokument.php?lang=slv&id=116063 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0