Abstract

Single crystals of BaZr 2F 10 · 2H 2O were prepared from BaF 2ZrF 4 mixtures in aqueous HCl solution. The crystal structure has been solved in the orthorhombic Pnam space group: a = 7.8974(3)Å, b = 7.9076(3)Å, c = 14.7227(4)Å, R F = 0.017, and R I = 0.023 from a twinned crystal whose apparent space group was P4 22 12. The bidimensional structure is built up from infinite corner-sharing in the (001) plane of [Zr 2F 14] 6− bipolyhedra formed by edge-sharing of two [ZrF 8] 4− trigonal dodecahedra; between each [Zr 2F 10] 2− layer, Ba atoms and H 2O molecules ensure the cohesion of the structure. The dehydration process has been studied by TGA and X-ray thermodiffractometry; at 130°C the first H 2O molecule reversibly leaves without damaging the crystal structure which becomes isotypic to that of TlZrF 5; above 150°C the second H 2O molecule continuously leaves up to 210°C, where the crystal structure collapses.

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