PREPARATION OF SPIRO-CYCLIC ORGANIC POLYSULFANES OF TYPE C6H10SN AND X-RAY STRUCTURAL-ANALYSIS OF C6H10S11, A DERIVATIVE OF CYCLO-DODECASULFUR

By reaction of (C5H5)(2)Ti(mu-S-2)(2)C6H10 3 with S2Cl2 7,8,9,10,11,12 -hexathiaspiro-[5.6]dodecane 4 is prepared (yield 51%) and characteriz ed by UV, IR, Raman, mass, and NMR spectra (H-1, C-13). The seven-memb ered CS6 ring undergoes pseudorotation in solution. With S7Cl2 the com plex 3 yields 12,13,14,15,16,17-undecathiaspiro[5.11]heptadecane 5 (yi eld 23%). The yellow, monoclinic crystals of 5 consist of spirocyclic C6H10S11 molecules with the C-6 ring in a chair-conformation while the CS11 ring is of the same conformation as cyclododecasulfur S-12. UV, IR, Raman, mass and NMR-spec tra of 5 are reported. A mixture of dichl orosulfanes SCl2 (n = 1-8) reacts with 3 to give the homologous series C6H10Sm which was characterized by reversed-phase HPLC for m = 5-14.