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标题反应产生三个已知化合物2,3,4和两个新的化合物CH_3SCH_2CF_2CF_2H(5)和I(CF_2)_2O(CF_2)_2SO_3~(-+)S(CH_3)_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P2_1/c;晶胞参数a=9.399A,b=15.651A,C=10.934A,β=94.80°;V=1602.8A~3;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[(CH_3)~3S]~+和[I(CF_2)_2O(CF_2)_2SO_3]~-组成的离子晶体。
The title reaction yielded three known compounds 2,3,4 and two new compounds CH_3SCH_2CF_2CF_2H (5) and I (CF_2) _2O (CF_2) _2SO_3 - (-) S (CH_3) _3 (6). The structure of 6 was confirmed by X-ray diffraction. 6 is a monoclinic with space group P2_1 / c; cell parameters a = 9.399A, b = 15.651A, C = 10.934A, β = 94.80 °; V = 1602.8A ~ 3; D_m = 2.072gcm ~ (-3), D_c = 2.073gcm ~ (-3). The structure was solved by heavy atom method. The least squares correction of diagonal matrix of isotropic and anisotropic blocks was performed. For 1999 observable diffraction points, the final R value was 0.054. The three S-C bonds in trimethylsulfonium form a triangular pyramid with bond lengths of 1.814, 1.800 and 1.818A respectively. The three C-S-C bond angles are 101.06 °, 101.52 ° and 102.53 °. The distance between the S atom in trimethylsulfonium and the three O atoms in the sulfonate is 3.79, 3.64 and 3.43A respectively, which greatly exceeds the bond length range of the S-O covalent bond. The whole crystal is composed of [(CH_3) ~ 3S] ~ + and [I (CF_2) _2O (CF_2) _2SO_3] ~ -.