Synthesis of N-Silylated Diaminosulfanes from Functionally Substituted Sulfur Diimides and Hexachlorodisilane and Octachlorotrisilane - Multinuclear Magnetic Resonance Studies and X-Ray Structure Determination of a Non-Cyclic Diaminosulfane

Sulfur d iim ides R '(N S N )R 2 (1) w ith d ifferen t su b s titu en ts R 1 a n d /o r R 2 o r w ith fu n c tio n al g ro u p s reac t w ith h ex ach lo ro d is ilan e (2) o r o c ta ch lo ro tr is ila n e (3) to give the co rre sp o n d in g d iam in o su lfan es (4, 5) in q u a n tita tiv e yield. T he fo rm a tio n o f cyclic in te rm ed iates p rio r to the redox p rocess is d iscussed . T h e p ro d u c ts have been ch arac te rized by 'H , 13C, 15N an d 29Si N M R in so lu tio n as well as by 1:,N a n d 29Si C P /M A S N M R in the so lid s ta te (4a, 4f). T he crystal s tru c tu re o f C lM e2Si(C l3S i)N S N (S iC l3)S iM e2Cl (4f) has been determ ined: space g ro u p P 1 (no. 2) w ith a = 864.2(2), b = 1096.8(2), c = 1232.7(2) pm and Z = 2.