【摘要】 标题反应产生三个已知化合物2,3,4和两个新的化合物CH₃SCH₂CF₂CF₂H（5）和I（CF₂）₂O（CF₂）₂SO₃^-+S（CH₃）₃（6）。6的结构经X射线衍射测定得到验证。 6的晶体属单斜晶系,空间群为P2₁/c;晶胞参数a=9.399A,b=15.651A,C=10.934A,β=94.80°;V=1602.8A³;Z=4;D_m=2.072gcm^-3,D_c=2.073gcm^-3。结构由重原子法解出,经各向同性和各向异性块对角矩阵最小二乘修正,对1999个可观察衍射点,最终R值为0.054。三甲基锍中的三个S-C键形成三棱锥体,其键长分别为1.814,1.800,1.818A,三个C-S-C键角为101.06°,101.52°,102.53°。三甲基锍中的S原子与磺酸根中三个O原子的距离分别为3.79,3.64,3.43A,大大超过S-O共价键的键长范围。整个晶体是由[（CH₃）³S]⁺和[I（CF₂）₂O（CF₂）₂SO₃]^-组成的离子晶体。更多还原

【Abstract】 The title reaction gave three known compounds 2, 3,4 and two new compounds.CH₃SCH₂CF₂CF₂H （5） and I （CF₂）₂O （CF₂）₂SO₃S（CH₃）₃ （6）. The structure of 6 was con-firmed by X-ray diffraction analysis. The crystals of 6 are monoclinic. space groupP2₁/c, with a=9. 399, b=15. 651, c=10. 934A, β=94. 80°and Z=4. The structurewas solved by heavy-atom method and refined by block-diagonal matrix least-squaresprocedure to a final R=0. 054 for 1999 independent observed reflexions. The S-C bonds around the sulphur atom in trimethylsulphonium are pyramidalwith the bond lengths of 1.814A, 1.800 A and 1.818 A and the bond angles C-S-Cof 101.06°, 101.5O° and 102.53°. The distances of the sulphur atom in trimethyl-sulphonium to three oxygen atoms in the sulphonate radical are 3.79 A, 3.64 A and3.34A, respectively. These distances are out of the range of the normal S-O bondlength. The structure consists of trimethyl sulphonium cations and 5-iodo-3-oxaoctafluoropentanesulphonate anions.更多还原