title: Solution Species and Crystal Structure of Zr(IV) Acetate.
abstract: Complex formation and the coordination of zirconium with acetic acid were investigated with Zr K-edge extended X-ray absorption fine structure spectroscopy (EXAFS) and single-crystal diffraction. Zr K-edge EXAFS spectra show that a stepwise increase of acetic acid in aqueous solution with 0.1 M Zr(IV) leads to a structural rearrangement from initial tetranuclear hydrolysis species [Zr4(OH)8(OH2)16]8+to a hexanuclear acetate species Zr6(O)4(OH)4(CH3COO)12. The solution species Zr6(O)4(OH)4(CH3COO)12was preserved in crystals by slow evaporation of the aqueous solution. Single-crystal diffraction reveals an uncharged hexanuclear cluster in solid Zr6(μ3-O)4(μ3-OH)4(CH3COO)12·8.5H2O. EXAFS measurements show that the structures of the hexanuclear zirconium acetate cluster in solution and the solid state are identical.
authors.affiliation: Helmholtz-Zentrum Dresden-Rossendorf, Institute of Resource Ecology , Bautzner Landstrasse 400, 01328 Dresden, Germany.|The Rossendorf Beamline at ESRF , BP 220, 38043 Grenoble, France.
authors.forename: Christoph
authors.identifier: http://orcid.org/0000-0001-6393-2778
authors.initials: C
authors.lastname: Hennig
authors.affiliation: Helmholtz-Zentrum Dresden-Rossendorf, Institute of Resource Ecology , Bautzner Landstrasse 400, 01328 Dresden, Germany.
authors.forename: Stephan
authors.initials: S
authors.lastname: Weiss
authors.affiliation: BAM Federal Institute for Materials Research and Testing , Richard-Willstätter-Strasse 11, D-12489 Berlin, Germany.
authors.forename: Werner
authors.initials: W
authors.lastname: Kraus
authors.affiliation: Helmholtz-Zentrum Dresden-Rossendorf, Institute of Resource Ecology , Bautzner Landstrasse 400, 01328 Dresden, Germany.
authors.forename: Jerome
authors.initials: J
authors.lastname: Kretzschmar
authors.affiliation: Helmholtz-Zentrum Dresden-Rossendorf, Institute of Resource Ecology , Bautzner Landstrasse 400, 01328 Dresden, Germany.|The Rossendorf Beamline at ESRF , BP 220, 38043 Grenoble, France.
authors.forename: Andreas C
authors.identifier: http://orcid.org/0000-0002-6608-5428
authors.initials: AC
authors.lastname: Scheinost