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The reaction of sulfur with MoOCI 4  in the presence of a large excess of ICl 3  in a sealed evacuated ampoule at 100 °C yields [SCl 3 ][MoOCl 4 ] in the form of yellow-brown, moisture sensitive crystals. The crystal structure determination (monoclinic space group P2 1 /n; lattice constants a - 971,1(1) pm, b = 926,9(1) pm. c = 1220,6(1) pm, β = 112,68(1)°, Z = 4) shows that the title compound consists of square pyramidal [MoOCl 4 ] -  anions and trigonal pyramidal [SCl 3 ] +  cations. Two [MoOCl 4 ] -  anions are linked by asymmetric chlorine bridges and form centrosymmetric dimers [Mo 2 O 2 CI 8 ] 2-  with the oxygen atoms located in the trans positions of the chlorine bridges. Two trigonal pyramidal [SCl 3 ] +  cations are connected by secondary sulfur chlorine interactions with the [Mo 2 O 2 CI 8 ] 2-  anion to form centrosymmetric dimers ([SCl 3 [MoOCl 4 ]) 2 . The coordination sphere for the sulfur atom is a strongly distorted octahedron with three S-Cl bonds of 199 pm and three weak S-Cl contacts of 304 pm in average length.

Darstellung und Kristallstruktur von [SCI 3 ][HM0OCl 4 ] / Preparation and Crystal Structure of [SCl 3 ][MoOCl 4 ]