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In the reaction of K 2 [OsCl 6 ] with boiling water/acetylacetone (1:1) a mixture of different chloro-acetylacetonato complexes is formed, from which [Os(acac) 3 ] can be isolated by column chromatography with dichloromethane on silica gel. The crystal structure of [Os(acac) 3 ] (mo­noclinic, space group P2 1 /c,a = 13.968(5), b = 7.517(5), c = 16.455(5) Å ,β = 98.939(5)°, Z = 4) has been determined by single crystal X-ray diffraction analysis. High resolution IR and Raman spectra were measured at low temperature (10K). Based on the molecular parameters of the X-ray structure determination a normal coordinate analysis has been performed and the normal modes of vibration have been assigned. With a set of 32 force constants, taking into account the intraligand vibrations, a good agreement between observed and calculated frequencies has been achieved. The valence force constants are f d (OsO) = 3.19 and f d (OC) = 6.74 mdyn/Å.

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Darstellung, Kristallstruktur, Schwingungsspektren und Normalkoordinatenanalyse von [Os(acac) 3 ]/ Synthesis, Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis of [Os(acac) 3 ]