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- Complex formation (1) (entfernen)
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)12 was 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.