Abstract: | Preparation and Crystal Structure of β-[SeCl3][MoOCl4] The reaction of Se4[MoOCl4] and Te4[MoOCl4] with SOCl2 as solvent at 150 °C and 80 °C yields [SeCl3][MoOCl4] and [TeCl3][MoOCl4] respectively within 3 to 6 days as yellow-brown, moisture-sensitive crystals. [TeCl3][MoOCl4] was obtained in the already known monoclinic form, while β-[SeCl3][MoOCl4] crystallizes in a new polymorphic triclinic form (P1¯, Z = 2, a = 752.7(2), b = 812.8(2), c = 956.9(3) pm, α = 92.55(3)°, β = 111.63(2)°, γ = 107.39(3)°). The structure contains centrosymmetric tetranuclear units ([SeCl3]2[Mo2O2Cl8]) which are analogous to the entities found in the structure of [SCl3][MoOCl4]. The packing of the molecules in β-[SeCl3][MoOCl4] and [SCl3][MoOCl4] is distinctely different. |