Abstract
Hydrothermal methods for growing single crystals of alkali-metal trivanadates AV 3O 8 for A = K, Rb, Cs and their single-crystal structural studies are presented. Plate-shaped orange crystals were hydrothermally grown at 250 °C from V 2O 5 powders dispersed A(NO) 3 solutions. RbV 3O 8, the structure of which has remained undetermined, was found to be isostructural with KV 3O 8 and CsV 3O 8: the monoclinic system P2 1 m with a = 4.9864(8) A ̊ , b = 8.442(1) A ̊ , c = 7.8621(7) A ̊ , β = 96.064(9) °, and Z ≖ 2. The crystallographic data for KV 3O 8 and CsV 3O 8 have been revised; in particular, the data of KV 3O 8 has been greatly improved. AV 3O 8 adopts a layered structure with V 3O 8 layers consisting of VO 6 octahedra and VO 5 square pyramids. The oxygen coordination around interlayer A atom is AO 8 for A = Rb, Cs but is regarded as AO 6 for A = K from the anomalous variation of A − O distances with A + ionic radii.
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