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By careful oxidation of the pure fluorochloroosmates(IV) with BrF 3  in dichloromethane the mixed pentavalent complex anions [OsF 5 Cl] -  and cis -[OsF 4 Cl 2 ] -  are formed. X-ray structure determinations on single crystals have been performed of (Ph 3 PNPPh 3 )[OsF 5 Cl]·CH 2 Cl 2  (1) (triclinic, space group P1̄, a = 12.153(5), b = 12.387(5), c = 14.229(5) Å , α = 70.07(1), β = 65.46(1), γ = 72.87(1)°, Z = 2) and cis-(Ph 3 PNPPh 3 )[OsF 4 Cl 2 ]·CH 2 Cl 2  (2) (triclinic, space group P1̄, a = 11.987(2) b = 13.083(2), c = 14.456(2) Å, α = 66.30(1), β = 65.47(1), γ = 71.22(1)°, Z = 2). Based on the molecular parameters of the X-ray determinations the IR and Raman spectra for the anions of 1 and 2 have been assigned by normal coordinate analysis. Due to the mutual trans influences the valence force constants of asymmetrically coordinated octahedral axes F • -Os-Cl′ differ from those of the symmetric F-Os-F axes. The data are for 1: f d (OsF • ) = 3.95, f d (OsF) = 4.07, f d (OsCl′) = 2.51 and for 2: f d (OsF • ) = 3.45, f d (OsF) = 3.97, f d (OsCl′) = 2.42 mdyn/Å

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Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalyse von (Ph 3 PNPPh 3 )[OsF 5 Cl]·CH 2 Cl 2  und cis-(Ph 3 PNPPh 3 )[OsF 4 Cl 2 ]·CH 2 Cl 2  / Crystal Structures, Vibrational Spectra and Normal Coordinate Analysis of (Ph 3 PNPPh 3 ) [OsF 5 Cl]·CH 2 Cl 2  and cis-(Ph 3 PNPPh 3  )[OsF 4 Cl 2 ]·CH 2 Cl 2