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On heating of [(C 2 H 5 ) 4 N][OsCl 6 ] for a short time at 240 °C , Cl 2  is lost and [(C 2 H 5 ) 4 N] 2 [Os 2 Cl 10 ] is formed quantitatively. Both complexes are connected by a temperature dependent redox equilibrium so that by treatment at 120 °C with Cl 2  gas the hexachloroosmate(V) is recovered from the decachlorodiosmate(IV). The crystal structures of salts of both an ions were determined from single crystal X -ray diffraction analyses. [(C 2 H 5 ) 4 N][OsCl 6 ] is monoclinic, space group P2  1  with a = 7 .020 (1), b = 10 .163 (2), c = 11.609 (2) Å , β = 103.91(1)° (at - 133 °C ). The strongly pseudocentrosymmetric structure shows a reversible phase transition at ca. 85 °C. The Os -Cl bond length (mean value 2.303 Å) in the regular [OsCl 6 ]-octahedra is significantly smaller than in [OsCl 6 ] 2−  , in accordance with vibrational spectra. [(n -C 4 H 9 ) 4 N] 2  [Os 2 Cl 10 ] crystallizes in the orthorhombic space group Pbca with a = 15 .496 (2), b = 15 .965 (3), c = 19 .431(3) Å and contains centrosymmetric [Os 2 Cl 10 ] 2−  ions with approximate D 2h  symmetry. Within the edge-sharing [OsCl 6 ] octahedra the mean terminal and bridging Os -Cl bond lengths are 2.307 and 2.411 Å , respectively.

zeitschrift für naturforschung b

Reaktionen und Strukturen von [(C 2 H 5 ) 4 N][OsCl 6 ] und [(n-C 4 H 9 ) 4 N] 2 [Os 2 Cl 10 ] / Reactions and Structures of [(C 2 H 5 ) 4 N][OsCl 6 ] and [(n-C 4 H 9 ) 4 N] 2 [Os 2 Cl 10 ]