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Synthesis and Crystal Structure of the Palladium(IV) Polyoxomolybdate,K0.75Na3.75[PdMo6O24H3.5]·17H2O
Authors:Sarah Angus‐Dunne Prof. Dr.,Robert   C. Burns,Donald   C. Craig,Geoffrey   A. Lawrance
Affiliation:1. Department of Chemistry, M?lardalens University, Eskilstuna 63105, Sweden;2. School of Environmental and Life Sciences, Discipline of Chemistry, University of Newcastle, Callaghan 2308, New South Wales, Australia;3. School of Chemistry, University of New South Wales, Kensington 2033, New South Wales, Australia
Abstract:The first example of a heteropolyoxomolybdate containing palladium(IV) was isolated and characterized by X‐ray crystallography. The palladium(IV) hexamolybdate, K0.75Na3.75[PdMo6O24H3.5]·17H2O, was isolated from an aqueous solution at pH 4.5 in the space group Pbar{1} , a 10.790(2), b 12.244(3), c 14.086(3) Å, α 113.77(1), β 90.41(1),γ 107.86(1)°, and the structure was determined using X‐ray diffraction methods, refining to a residual of 0.0301 for 5334 reflections. A formal “[PdMo6O24H3]5–” subunit exhibits the basic Anderson structure, with two [PdMo6O24H3]5– cluster anions in the structure bridged by a hydrogen atom (formally an H+) situated on a center of symmetry to give a “[Pd2Mo12O48H7]9–” dimeric anion. The palladium(IV) atom occupies a slightly distorted octahedral environment, with Pd–O distances ranging from 1.968 to 2.009 Å.
Keywords:Palladium  Polyoxometalates  X‐ray diffraction  Sodium  Potassium
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