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Through careful acidification of the aqueous solution of [OsO 2 (OH) 4 ] 2-  in the presence of CN -  or  13 CN -  with acetic acid, [OsO 2 (CN) 4 ] 2-  or [OsO 2 ( 12 CN) 4 ] 2-  are formed, respectively. The reaction of Os 18 O 4  and tetrabutylammonium cyanide with glacial acetic acid in anhydrous methanol yields [Os 18 O 2 (CN) 4 ] 2-  . The shifts of the infrared and Raman bands of the isotopically labelled complexes are in good agreement with Teller-Redlich calculations. The degenerate E modes, expected for tetragonal symmetry, are split by approx. 15 cm -1 , indicating an orthorhombic distortion of the complex ion in the solid state. Therefore, all the observed IR- and Raman frequencies are assigned according to point group D 2h . For the complex containing an  18 O=Os= 18 O axis, the symmetry is lowered to C 2v , and the rule of mutual exclusion is restricted. This results in a weak absorption in the infrared spectrum of the Raman active symmetric OsO stretching vibration and vice versa a weak band in the Raman spectrum for the antisymmetric infrared active mode.

zeitschrift für naturforschung b

DarsteIlung und Schwingungsspektren des  13 C- und  18 O-Hiarkierten trans-Dioxotetracyanoosmats(VI), [OsO 2 (CN) 4 ] 2-  / Preparation and Vibrational Spectra of  13 C and  18 O Labelled trans-Dioxotetracyanoosmate(VI), [OsO 2 (CN) 4 ] 2-