الوصف: |
Chlorination of CS 2 leads to trichloromethanesulfenyl chloride, Cl 3 CSCl, in moderate yields. The oxidation of Cl 3 CSCl with H 2 O 2 gives Cl 3 CSO 2 Cl, the chloride of trichloromethanesulfonic acid. Cl 3 CSO 2 Cl is the crucial product for the preparation of trichloromethanesulfonates (“trichlates”) and has been characterized by IR spectroscopy, differential scanning calorimetry (DSC) and X‐ray diffraction measurements (P‐1, a =609.99(5) pm, b =727.45(6) pm, c =782.49(7) pm, α =80.644(3)°, β =85.175(3)°, γ= 88.311(3)°. The acid Cl 3 CSO 3 H can be gained in form of the hydrate (H 5 O 2 )[Cl 3 CSO 3 ] in two different modifications ( I : monoclinic, P 2 1 / n , Z=8, a =1292.47(7) pm, b =605.89(2) pm, c =2661.1(1) pm, β =98.708(4)°, V =1672.8(1) Å 3 ; II : monoclinic, Cc , Z=4, a =699.80(5) pm, b =1054.72(8) pm, c =1139.88(8) pm, β =95.303(3)°, V =837.7(1) Å 3 . Both modifications have been investigated by IR spectroscopy, thermal analyses and theoretical calculations. |