Abstract: | On the Preparation of Bis(triphenylsilyl)sulfanes (C6H5)3Si? Sx? Si(C6H5)3 (x = 3, 4) and the Crystal Structure of (C6H5)3Si? S4? Si(C6H5)3 The preparation of the bis(triphenylsilyl)sulfanes Ph3Si? Sx? SiPh3 (x = 3, 4) from Ph3SiSNa and SCl2 resp. S2Cl2 is reported. They are characterized by vibrational, NMR and UV-VIS spectroscopic measurements. Ph3Si? S4? SiPh3 crystallizes in space group P1 with a = 943.6(6) pm, b = 945.7(5) pm, c = 1 881.7(12) pm, α = 82.11(5)°, β = 78.95(5)°, γ = 83.15(5)° and Z = 2. |