35Cl NQR spectra of group 1 and silver dichloromethanesulfonates

Abstract

The dichloromethanesulfonates of silver and other +1-charged cations, M + (Cl 2 CHSO − 3 ) (M = Ag, Tl, Li, Na, K, Rb, Cs) were synthesized and studied by 35 Cl NQR. Dichloromethanesulfonic acid was prepared by the methanolysis of dichloromethanesulfonyl chloride, and was then neutralized with the carbonates of the +1-charged cations to produce the corresponding dichloromethanesulfonate salt. This NQR study completed the investigation of the chloroacetates and chloromethanesulfonates of silver, Ag + (Cl x CH 3−x SO − 3 ) and Ag + (Cl x CH 3−x CO − 2 ), and suggests (1) that the ability of organochlorine atoms to coordinate to silver decreases as the number of electron-withdrawing groups (Cl, SO − 3 , CO − 2 ) attached to the carbon atom increases; (2) that the unusually large NQR spectral width found among M + (Cl 2 CHCO − 2 ) salts is not present among M + (Cl 2 CHSO − 3 ) salts, and therefore is not generally characteristic of the dichloromethyl group in salts.

Synthesis and Characterization of the Trichlates [N(CH3)4][Cl3CSO3], [NH4][Cl3CSO3], and the Dichlate [NH4][Cl2CHSO3]

“…In a hydrothermal reaction in sealed glass ampoules at elevated temperatures, the reaction of barium hydroxide and Cl 3 CSO 2 Cl in the presence of NH 4 OH leads to single crystals of (NH 4 )[Cl 2 CHSO 3 ]. Although dihalido-and monohalido methanesulfonates have already been investigated roughly 20 years ago, [24][25][26] structure elucidations are scarce. For the [ClCH 2 SO 3 ] À anion the silver compound is known as the only example, [24] while no structure determinations of the [Cl 2 CHSO 3 ] À anion are known so far.…”