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The reaction of 2′ 2′ 3′ 3′-tetrafluoropropyl-5-iodo-3-oxaoctafluoropentane sulfonate with dimethylsulfoxide and determination of the crystal structure of one of the products
Authors:Li Zong-Zhen  Ni Chau-Zhou  Ma Yi-Lin
Institution:Shanghai Institute of Organic Chemistry Academia Sinica, Shanghai
Abstract:The title reaction gave three known compounds (2, 3 and 4) and two new compounds, CH3SCH2(CF2)2H (5) and I(CF2)2O(CF2)2SO3?S+(CH3)3 (6). The structure of 6 was confirmed by X-ray diffraction analysis. The crystals of 6 belong to monoclinic space group P21/C with a = 9.399, b = 15.651, c=10.934Å, β = 94.80° and z = 4. The structure was solved by heavy-atom method and refined by block-diagonal matrix least-squares procedure to a final R of 0.054 for 1999 independent observed reflexions. The S? C bonds around the sulphur atom in trimethylsulphonium are pyramidal with the bond lengths of 1.814 Å, 1.800Å and 1.818 Å and the bond angles C-S-C of 101.06°, 101.52° and 102.53°. The distances of the sulphur atom in trimethylsulphonium to three oxygen atoms in the sulphonate radical are 3.79 Å, 3.64 Å and 3.34 Å respectively. These distances are out of the range of the normal S-O bond length. The structure consists of trimethylsulphonium cations and 5-iodo-3-oxaoctafluoropentane-sulphonate anions.
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