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C 5 H 4 O 2 S 3 ,monoclinic, P 12 1 / c 1(no.14), a =3.9797(1)A, b =6.0394(2)A, c =31.1165(6)A, =91.868(1)°, V =747.5A 3 , Z =4, R gt (F) =0.119, wR ref (F 2 ) =0.324, T =200K. Source of material In the literature 4-methoxycarbonyl-1,3-dithiole-2-thione wasobtainedinthreesteps[1].Inthepresentone-potsynthesistheti-tlecompoundwasobtainedundersolventfreeconditionscata-lyzedbypotassiumcyanideinthepresenceofsilicaassolidsupportat200°C(85%yield).0.2mmolof4,5-bis(carbonyl-methoxy)-1,3-dithiole-2-thione,0.4mmolofpotassiumcyanideand0.2gofsilicaweremixedinamortar.Thispowderwasheatedfor1hat200°C.Thecolorofthemixturewasturnedfromyellowtolightbrown.Thepurecompoundwasobtainedbyfiltrationofthesolutionindichloromethane,followedbyevaporationofsol-ventandpreparativechromatographyoversilicagel.TheproductwascharacterizedbyIR, 1 HNMR,and 13 CNMRspectroscopy. Experimental details TheX-rayreflectionswereratherbroadanddiffuse,butthedataturnedouttobeuseable.Allhydrogenatomsweretreatedusingappropriateridingmodels.Thebadqualityofthecrystalsandthedatasetwerethereasonsforthelarge

Crystal structure of 4-methoxycarbonyl-1,3-dithiole-2-thione, C 5 H 4 O 2 S 3