Ba2[Pd(HS2O7)2(S3O10)2]: A Heteroleptic Polysulfatopalladate |
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Authors: | Jörn Bruns Prof Dr Thorsten Klüner Prof Dr Mathias S Wickleder |
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Institution: | Carl von Ossietzky University of Oldenburg, Institute of Chemistry, Carl‐von‐Ossietzky‐Strasse 9–11, 26129 Oldenburg (Germany), Fax: (+49)?441‐798‐3352 |
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Abstract: | The oxidation of elemental palladium with oleum (65 % SO3) in the presence of barium carbonate in torch‐sealed glass ampoules at 180 °C leads to yellow single crystals of the heteroleptic palladate Ba2Pd(HS2O7)2(S3O10)2] (triclinic, P ; Z=1; a=884.18(3), b=927.68(3), c=938.77(4) pm; α=60.473(1), β=80.266(2), γ=87.746(2)°). The crystal structure shows the Pd2+ ions in a square‐planar coordination of oxygen atoms of two hydrogendisulfate as well as of two trisulfate anions. The compound is the first example of the rarely seen S3O102? and HS2O7? anions acting as ligands in a complex anion and, moreover, the first heteroleptic polysulfatometallate known so far. The complex formation leads to a stabilization of the trisulfate anion relative to its uncoordinated congener. Ba2Pd(HS2O7)2(S3O10)2] has been further characterized by vibrational spectroscopy and quantum chemical calculations. Thermal analyses by means of thermogravimetric/differential thermal analysis (TG/DTA) measurements show that the compound decomposes to yield elemental palladium and BaSO4. |
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Keywords: | palladium quantum chemistry thermal analysis sulfates vibrational spectroscopy |
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