PPh₄[Os(NS)(S₄)₂(H₂O)] wurde als rotbraune Kristalle durch Reaktion von PPh₄[OsNCl₄] mit einer Lösung von überschüssigem Dinatriumtetrasulfid in Dimethylformamid/H₂O hergestellt und durch das IR-Spektrum und eine Kristallstrukturanalyse charakterisiert. Raumgruppe P2₁/n, Z = 4, Strukturlösung mit 4162 unabhängigen Reflexen, R = 0,059 für Reflexe mit I > 2σ(I). Gitterabmessungen bei −40°C: a = 1138,9(5); b = 1301,4(4); c = 2092,7(7) pm, β = 104.74(3)º. Die Abstände OsN, OsO und OsS betragen 175,2(12), 219,8(12) und 237,5(4) − 239,1(4) pm. Die OsNS-Gruppe ist mit einem Bindungswinkel von 171,2(7)º annähernd linear.

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.

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Volume622, Issue8

August 1996

Pages 1306-1310

Synthese und Kristallstruktur von Tetraphenylphosphonium-Aquabis(tetrasulfido)thionitrosyl-Osmat, PPh₄[Os(NS)(S₄)₂(H₂O)]^†

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Synthese und Kristallstruktur von Tetraphenylphosphonium-Aquabis(tetrasulfido)thionitrosyl-Osmat, PPh4[Os(NS)(S4)2(H2O)]†

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Synthese und Kristallstruktur von Tetraphenylphosphonium-Aquabis(tetrasulfido)thionitrosyl-Osmat, PPh₄[Os(NS)(S₄)₂(H₂O)]^†