Synthese, Molekül- und Kristallstruktur eines neuen tricyclischen B3N4S2Si2-Systems

Abstract

Acyclische Schwefeldiimide 1 ergeben rnit 1,2,4,3,5-Trithiadiborolanen 2 das cyclische 1,4,2,6,3,5-Dithiadiazadiborinansystem 3['.*]. 1 2 3Das difunktionelle 2,6-Bis(chlordimethylsilyl)-3,5-dimethylderivat 3a reagiert mit Bis(methy1amino)phenylboran 4 nicht zum zuniichst formulierbaren Produkt 5, sondern es entsteht das durch RBntgen-Strukturanalyse gesicherte tricyclische System 6@l. Die Struktur 6 (und 5) wird durch die Koordination von Schwefel an Bor begunstigt; ob 6 ein Umlagerungsprodukt von 5 ist, bleibt unklar. CI ICl I YgH5 6 (H3CI2Si, ,S, ,Si(CH3)2 / '

Contributions to the chemistry of boron. Part 194. Synthesis and characterization of mono, bi-, and tri-cyclic boron–nitrogen–sulphur ring systems. Crystal structure of 2,7,9,14-tetrakis(diethylamino)-3,5,6,10,12,13-hexathia-1,8-diaza-2,4,7,9,11,14-hexaboratricyclo[9.3.0.04,8]tetradecane

“…Most of these pairs can be considered equal in terms of the 30 criterion. The largest deviations result for the pair N(4)-B( 14)/N(8)-B( 7) and connected therewith for the bond angles B(3)-N(4)-B( 14)/B(9)-N(8)-B (7).…”

“…After the addition of half of the disulphane derivative a very pale powdery precipitate formed in the yellow solution. After complete addition the mixture was allowed to warm to room temperature and was stirred for a further 48 h. (7).-A solution of compound (2) (0.41 g, 2.5 mmol) in toluene ( 5 cm3) was added to a solution of (4b) (0.33 g, 1.0 mmol) in toluene (10 cm3) at ambient temperature with stirring. After warming the mixture to 70 "C for 36 h, the yellow solution was separated from a small amount of solid which had formed.…”

“…After proloned pumping, sublimation of (4b) was performed at 110 "C (1.3 Pa). Compound (7), m.p. 100-1 10 "C (decomp.…”