Crystal structure of caesium scandium bis(monohydrogenmonophosphate), CsSc(HPO4)2

Abstract

CsO 8H2P2Sc, monoclinic, P121/c1(no.14), a =5.3639(4)Å, b =9.1604(6) Å, c =14.705(1) Å, b =93.728(4)°, Source of materialSingle crystals of CsSc(HPO 4 ) 2 were obtained hydrothermally from acidic suspensions of scandium oxide, cesium hydroxide and phosphoric acid.According to the molar ratio of 1:1:6(Sc : Cs :P ), am ixutre of 0.5000 gS c 2 O 3 (Abcr, 99.9 %), 0.5435 g CsOH (Alfa Aesar, 99 %) and 2.5079 gH 3 PO 4 (Merck, 85 %) was homogenized in 10 ml of water.The suspension was concentrated by heating the open system at 373 Kfor two hours.The mixture was then transferred into a10mlTeflon-lined autoclave (filling degree 40 %) and heated under autogenous pressure at 443 Kfor 7 days.The reaction product contained crystals, which were washed with hot water, filtered, and washed again with acetone before drying in air at 333 K.The obtained transparent and colourless elongated prismatic crystals were up to 0.2 mm in length.The chemical composition was confirmed by ICP-AES analyses -found: Cs, 34.21 %; Sc, 12.54 %; P, 16.85 %; calculated for CsO 8H2P2Sc: Cs, 35.94 %; Sc, 12.16 %; P, 16.75 %.IR spectra and the loss of water during TG analyses confirm the presence of -OH groups.