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Trimethylsulfonium sulfate, [(CH 3 ) 3 S+] 2 SO 4  2− , has been prepared and subjected to X-ray analysis. The crystals are monoclinic, space group  C 2/ c , with  a  = 10.38(1),  b  = 10.55(1),  c  = 10.50(1)Å,  β  = 90.55(8)° and  Z  = 4. The structure was solved by direct methods and refined by full-matrix anisotropic least squares with 745 observed CuKα film data to  R  = 0.101.

Preparation and X-ray analysis of trimethylsulfonium sulfate [(CH 3 ) 3 S + ] 2 SO 2− 4