Darstellung,Kristallstruktur, Schwingungsspektren und Normalkoordinatenanalyse von [Co(NH3)6][Os(SCN)6]

Synthesis, Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis of Co(NH₃)₆]Os(SCN)₆] From the mixture of the linkage isomers Os(NCS)_n(SCN)_6–n]^3–, n = 0–2, pure Os(SCN)₆]^3– has been isolated by ion exchange chromatography on diethylaminoethyl cellulose. The X‐ray structure determination on a single crystal of Co(NH₃)₆]Os(SCN)₆] (trigonal, space group R 3, a = 12.368(2), c = 11.830(2) Å, Z = 3) reveals that the thiocyanate ligands are exclusively S‐coordinated with the Os–S distance of 2.388 Å and the Os–S–C angle of 108.8°. The IR and Raman spectra of (n‐Bu₄N)₃Os(SCN)₆] are assigned by normal coordinate analysis based on the molecular parameters of the X‐ray determination. The valence force constant f_d(OsS) is 1.42 mdyn/Å.