85185-49-5Relevant articles and documents
Crystal structures of (μ-trithio)bis[tricyclohexylgermanium(IV)] and (μ-trithio)bis[triphenylgermanium(IV)]
Brisse, Fran?ois,Vanier, Micheline,Olivier, Marc J.,Gareau, Yves,Steliou, Kosta
, p. 878 - 882 (2008/10/08)
Crystals of (μ-trithio)bis[tricyclohexylgermanium(IV)], [(C6H11)3Ge]2S3 (I), belong to the triclinic system of space group P1. The unit cell has the following dimensions: a = 9.004 (7) A?, b = 9.808 (4) A?, c = 11.815 (5) A?, α = 83.14 (3)°, β = 84.64 (5)°, γ = 66.92 (5)°, V = 951.8 A?3, Z = 1, dcalcd = 1.291 Mg m-3, F(000) = 394 Cu Kα radiation, μ(Cu Kα) = 3.59 mm-1. The structure, solved by direct methods, was refined by least squares to a final R value of 0.063 for 3185 observed reflections. [(C6H5)3Ge]2S3 (II), (μ-trithio)-bis[triphenylgermanium(IV)], is monoclinic of space group P21/n. The unit cell has the following dimensions: a = 11.969 (5) A?, b = 17.982 (6) A?, c = 16.741 (9) A?, β = 100.37 (4)°, V = 3543.9 A?3, dcalcd = 1.319 Mg m-3, Z = 4, F(000) = 1432, Mo Kα radiation, μ(Mo Kα) = 1.864 mm-1. The least-squares refinement of the atomic coordinates and temperature factors was concluded when R reached 0.096 for 1435 observed reflections. Both structures consist of a Ge-S-S-S-Ge sequence, in a coiled-type conformation, at the ends of which are bonded three cyclohexyl groups (I) or three phenyl groups (II). The two torsion angles describing the Ge-S-S-S-Ge part are both equal to 100.2 (3)° in I and to -96 (1) and -104 (1)° in II. The S-S, S-Ge and Ge-C distances respectively have average values of 2.009, 2.282, and 1.976 A? in I and 2.023, 2.260, and 1.90 A? in II. The S-S-S angle is 111.3 (3)° in I and 107.5 (7)° in II while S-S-Ge average 105.0° in I and 103.1° in II. Around Ge, the S-Ge-C and C-Ge-C angles have mean values of 106.7 and 112.1°, respectively, for I and 107.6 and 111.4°, respectively, for II. The substituents on Ge have a propeller-like arrangement. Looking down the Ge-Ge direction they adopt a staggered disposition.
