Inorg. Chem. 1985, 24, 2453-2458
2453
Contribution from the Department of Chemistry, University of Calgary, Calgary, Alberta, Canada T 2 N 1 N 4
Reaction of Dimethylcyanamide with Sulfur Dichloride: X-ray Crystal Structures of the N,N'- (Chlorosulfoniumylidene)bis(N',N'-dimethylchloroformamidine) Complexes [(Me2NC(C1)N),SCl]+X- (X- = C1-, C13-) and the Hydrolysis Product [Me2NC(Cl)NH2]+Cl--H20 T. CHIVERS,* J. F. RICHARDSON, and N . R. M. S M I T H Recetived September 24, 1984
The reaction of dimethylcyanamide with SC12in carbon tetrachloride containing NH4CI produces [(Me,NC(CI)N),SCl]+X- (4 (X- = C13-)) and [(Me2NC(C1)N)3S]+C13-(8). The former is hydrolyzed in wet acetone to [Me2NC(CI)NH2]+CI--H20(7).In 1,2-dichloroethane,Me2NCN and SCI2react to give 4 (X-= Cl-). The structures of 4 (X- = CI-, C13-) and 7 have been determined by X-ray crystallography. Crystal data: [(Me2NC(C1)N)2SC1]+Cl 3 4 ) no. data used in final cycle no. variables in final cycle GOF residual electron density, e A-3 R, RWC
[(Me2NC(Cl)N)2SC1]tCI-.C2H4C12 [Me2NC(C1)NH2]tC1-.H20
+
+
'Graphite monochromator. bobserved data plus those for which IC > 3a(Z0). c R = GOF and R, for [(Me2NC(C1)N)2SCI]+C1
