The compounds (Pn 4 P) 4 Sb 8 I 28 (1) and (Ph 4 P)Sb 3 I 10 (2) were prepared by the reaction of SbI 3 and Ph 4 PI in acetonitrile (molar ratios 2:1 and 3:1 respectively). The structures of 1 and 2 were determined from single crystal X-ray diffraction data. 1 crystallizes in the triclinic space group P1̄ with a - 1321.7(5). b = 1346.7(5), c = 2201.8(8) pm, α = 104.18(2). β = 99.92(2), γ = 100.33(2)°; 2: monoclinic, C2/c, a = 2371.1(2), b = 745.0(1), c = 2495.1(2) pm, β = 100.75(1)°. Whereas 1 exhibits isolated Sb 8 I 28 4- ions, the anions of 2 are built up of polymeric chains [Sb 3 I 10 - ] ∞ . In both compounds the distorted Sbl 6 octahedra are linked by common edges. The Sb-I distances are in the range between 277.4 and 354.8 pm (1) and between 277.4 and 342.4 pm (2). The observed structures do not only depend on stoichiometry, the nature of the counter cations, and the possibility of oligomerisation but also on the wide variety of the Sb-I bond strengths and the different bridges formed by iodine. The lone pair of Sb(III) seems to be predominantly 5 s 2 .
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Pohl et al. (1987) studied this question.