Contributions to the stereochemistry of zirconium oxysalts—part VI: syntheses and crystal structures of K2Zr(SO4)3∙2.5H2O, K2Zr(SeO4)3, K2Zr2O(SeO4)4, and Zr(OH)2(SeO4)·H2O

Abstract

The compounds K2Zr(SO4)3·2.5H2O, K2Zr(SeO4)3, and K2Zr2O(SeO4)4 were synthesized at 200 °C by reaction of Zr2O2(CO3)(OH)2 and KHCO3 with the respective acids H2SeO4/H2SO4 and minor H2O. Zr(OH)2(SeO4)·H2O originates from an analogous experiment at 215 °C without KHCO3. All four phases form colorless crystals up to several tenths of a mm and were investigated by single crystal X-ray diffraction. K2Zr(SO4)3·2.5H2O is monoclinic, space group P21/c (No. 14), with a = 7.295(2) Å, b = 13.925(3) Å, c = 12.579(3) Å, β = 95.32(3)°, V = 1272.3(4) Å3, Z = 4, R1 = 0.025. K2Zr(SeO4)3 and K2Zr2O(SeO4)4 are both triclinic, space group P1¯\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$P\\overline{1}$$\\end{document} (No. 2), with a = 7.570(1) Å, b = 10.500(1) Å, c = 14.400(1) Å, α = 85.55(1)°, β = 88.04(1)°, γ = 87.82(1)°, V = 1139.7(2) Å3, Z = 4, R1 = 0.049, and a = 5.400(1) Å, b = 7.328(1) Å, c = 9.642(1) Å, α = 95.81(1)°, β = 95.20(1)°, γ = 94.27(1)°, V = 376.74(4) Å3, Z = 1, R1 = 0.020, respectively. Zr(OH)2(SeO4)·H2O crystallizes in the monoclinic space group C2/c (No. 15), with a = 6.684(1) Å, b = 12.998(2) Å, c = 6.792(1) Å, β = 97.37(1)°, V = 585.14(6) Å3, Z = 2, R1 = 0.013.Graphical abstract