Syntheses, NMR Characterization and Semi-Empirical Structural Studies of Dithiaphospholane Derivatives

The preparation, properties and X-ray structures of gold(I) trithiophosphite complexes

“…The para carbons appear as broad singlets and the values of the J PC coupling constants especially for the ipso carbon ( 2 J PC 5-6 Hz), are lower than for the free ligand (13 Hz). With the bicyclic ligand, 1,2-bis(1,3,2-dithiaphospholan-2-ylthio)ethane, the doublet of doublets of the two bridging carbon atoms at higher field in the free ligand spectrum [18] is again reduced to a broad singlet in 6.…”

“…Calc. for C 18 The compound was prepared in an analogous manner to 2 employing (PhS) 3 P (0.145 g, 0.40 mmol) and (tht)AuC 6 A solution of (tht)AuCl (0.218 g, 0.68 mmol) and 1,2-bis(1,3,2-dithiaphospholan-2-ylthio)ethane (0.115 g, 0.34 mmol) in thf (15 mL) was stirred at r.t. A precipitate was observed and after 1.5 h the volatiles were removed in vacuo affording a yellowish solid (0.263 g, 96%). Only limited analytical data could be obtained due to the insolubility of the material, m.p.…”

“…Calc. for C 18 (7) (MeS) 3 P (0.139 g, 0.81 mmol) was dissolved in acetonitrile (10 mL) and (tht)AuCl (0.130 g, 0.41 mmol) was added which yielded a yellow precipitate. After 1 h thf (10 mL) was added which dissolved the precipitate affording a hazy yellowish solution.…”

New Synthetic Route for 2-Chloro-1,3,2-Dithiastibolane Involving a Skeletal Substitution Reaction

“…2-chloro-l,3,2-dithiaphospholane 1 was prepared from the corresponding dithiol with PC1 3 and the details can be found in [5]. Glassware was flame-dried in vacuum and solvents were dried, freshly distilled under dinitrogen, and degassed prior to use.…”