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Violet crystals of AsPh 4 [W(O)Cl 3 (HN 3 S 2 )] were obtained by partial hydrolysis of AsPh 4 [WCl 4 (N 3 S 2 )] in a saturated solution in CH 2 Cl 2 /CCl 4 . Its IR spectrum is reported. The crystal structure was determined by X-ray diffraction (2284 independent observed reflexions, R = 0.041). Crystal data: triclinic, space group P1̄, Z = 2, a = 812.2, b = 1268.4, c = 1343.9 pm, α = 88.58, β = 82.04 and γ = 88.26°. The compound consists of AsPh 4  ⊕  cations and [W(O)Cl 3 (HN 3 S 2 ) ⊖  anions in which the tungsten atoms have a distorted octahedral coordination with one oxo-ligand (171 pm), three chlorine atoms and two nitrogen atoms of the planar (HN 3 S 7 ) 2⊖  ligand. The WN bond lengths are 183 and 226 pm; the longer WN bond is due to the hydrogen atom attached to its N atom and to the trans influence of the oxo group. The crystal packing corresponds to one of the types frequently found among tetraphenylphosphonium compounds with cations stacked to parallel columns.

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AsPh 4 [W(O)Cl 3 (HN 3 S 2 )]; Synthese, IR-Spektrum und Kristallstruktur / AsPh 4 [W(O)Cl 3 (HN 3 S 2 )]; Synthesis, IR Spectrum and Crystal Structure