Untersuchungen an Polyhalogeniden, XIX [1] Bis(methyltriphenylphosphonium)oktaiodid (MePh3P)2I8, Cäsium(18-Krone-6)triiodid [Cs(C12H24O6)]I3, Iodoblei(18-Krone-6)triiodid [Pb(C12H24O6I]I3 und Diiodothallium(18-Krone-6)tetraiodothallat [Tl(C12H24O6)I2](TlI4) / Studies of Polyhalides, XIX [1] Bis(methyltriphenylphosphonium) Octaiodide (MePh3P)2I8, Cesium(18-crown-6) Triiodide [Cs(C12H24O6)]I3, Iodolead(18-crown-6) Triiodide [Pb(C12H24O6)I]I3 and Diiodothallium(18-crown-6) Tetraiodothallate [Tl(C12H24O6)I2](TlI4)

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Abstract
(MePh3P)2l8 has been prepared by the reaction of methyltriphenylphosphonium iodide with iodine in ethanol. It crystallizes in the monoclinic space group P21/n with a = 985.2(2), b = 1260.0(1), c = 1872.6(4) pm, β = 91.50(2)° and Z = 4. The crystal structure has been refined to R = 0.030 for 2882 reflections. It may be described as a layerlike packing of cations and anions. The anion with point symmetry 1̅ consists of two triiodide groups and a bridging iodine molecule forming a rather common nearly planar Z-shaped octaiodide ion I8 2-. [Cs(18-crown-6)]I3 has been prepared by the reaction of cesium iodide and 18-crown-6 with iodine in ethanol. It crystallizes in the triclinic space group P1̅ with a = 921.4(1), b = 1175.4(7), c = 1178.0(4) pm, a = 112.82(4), β = 94.24(7), γ = 98.60(3)° and Z = 2. The crystal structure has been refined to R = 0.038 for 3302 reflections. The geometry of the cation [Cs(18-crown-6)]+ and of the anion I3 - is quite normal. [Pb(18-crown-6)I]I3 has been prepared by the reaction of lead iodide and 18-crown-6 with iodine in dichloromethane. It crystallizes in the monoclinic space group P 21/n with a = 833.6(3), b = 1721.0(6), c = 1730.6(6) pm, β = 99.61(3)° and Z = 4. The crystal structure has been refined to R = 0.047 for 2772 reflections. It consists of complex cations [Pb(18-crown-6)I]+ and triiodide anions I3- forming weakly bonded ion pairs. [Tl(18-crown-6)I2](TlI4) has been prepared by the reaction of thallium(I)iodide and 18-crown-6 with iodine in dichloromethane. It crystallizes in the monoclinic space group P21/n with a = 1236.8(3), b = 1382.6(3), c = 1710.2(2) pm, β = 90.76(1)° and Z = 4. The crystal structure has been refined to R = 0.044 for 2916 reflections. It is composed of complex cations [Tl(18-crown-6)I2] + nd complex anions TlI4 - with their usual and expected geometry.

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