The new compound (MePh 3 P) 4 I 22 has been prepared by the reaction of Ph 3 MePI with iodine in a mixture of methanol and dichloromethane. It crystallizes in the triclinic space group P1̅ with a = 1018.4(3), b = 1333.0(4), c = 2042.9(6) pm, a = 88.56(2), β = 78.05(2), γ = 76.03(2)° and Z = 1. The crystal structure has been refined to R F = 0.0487 for 5525 reflections. It may be described as a layer-like packing of cations [CH 3 (C 6 H 3 ) 3 P] + and anions I 22 4- divided in one I 12 2- and two I 5 - groups. The central I 12 2- anion with point symmetry Q consisting of two L-shaped pentaiodide groups and a bridging iodine molecule is completed by two further end-on bonded pentaiodide ions with a rather short distance of 366.7(2) pm to the weakly bonded and nearly isolated docosaiodide ion.
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Tebbe et al. (1995) studied this question.