| Abstract: | Synthesis and Crystal Structure of Tetraphenylphosphonium Aqua-bis(tetrasulfido)thionitrosyl Osmate, PPh4[Os(NS)(S4)2(H2O)] PPh4[Os(NS)(S4)2(H2O)] has been prepared as redbrown crystals by reacting PPh4[OsNCl4] with a solution of excess disodium tetrasulfide in dimethylformamide/H2O and characterized by IR spectroscopy and by a crystal structure determination. Space group P21/n, Z = 4, structure solution with 4162 independent reflections, R = 0.059 for reflections with I > 2σ(I). Lattice dimensions at ?40°C: a = 1138.9(5), b = 1301.4(4), c = 2092.7(7) pm, β = 104.74(3)º. Os? N, Os? O, and Os? S distances are 175.2(12), 219.8(12), and 237.5(4)?239.1(4) pm, respectively. The Os?N?S moiety is approximately linear, with an OsNS angle of 171.2(7)º. |
