6926-73-4Relevant articles and documents
CRYSTAL STRUCTURE, SOLID-STATE NMR, AND QUANTUM CHEMICAL MODEL CALCULATIONS OF BIS-(DIETHOXYTHIOPHOSPHORYL)-TRISULFANE
Grossmann, Gisbert,Schwab, Birgit,John, Andreas,Komber, Hartmut,Jeschke, Gunnar,Sieler, Joachim
, p. 297 - 308 (2007/10/02)
Crystals of (EtO)2P(S)SSSP(S)(OEt)2 are triclinic, P, with a = 8.388(1), b = 11.128(2), c = 12.518(1) Angstroem, α = 62.34(6), β = 71.93(2), γ = 84.97(5) deg, V = 981.6(6) Angstroem3, Z = 2, and Dc = 1.36 g/cm3.The final refinement using 3681 observed reflections for 252 variables gives R = 0.057.The two molecules in the elementar cell are conformation enantiomers.The 31P CP MAS spectra show two spinning sideband systems, because the two phosphorus atoms of one molecule are chemically nonequivalent in the crystal.The resolution in the 13C CP MAS spectrum allows to distinguish four lines for the methyl groups and three lines for the methylene groups.NDDO and INDO calculations show, that the conformations with dihedral angles PSSS of ca. 90 deg have the lowest energies and those with 180 or 0 deg have considerably higher energies.The relatively high coupling constants4JPP of bis-(dialkoxythiophosphoryl)-trisulfanes in solution are not caused by conformations with W-like or other plane positions of the PSSSP nuclei. Key words: Crystal structure; CP MAS NMR; chemical shift anisotropy; quantum chemical calculations; dithiophosphoric; thiophosphoryl trisulfane.
REDOX REACTIONS OF ANTIMONY(III) O,O-DISUBSTITUTED PHOSPHORODITHIOATES WITH FERRIC CHLORIDE
Woo, Edward J.,Kalbacher, Barbara J.,McEwen, William E.
, p. 269 - 278 (2007/10/02)
The reaction of antimony(III) tris-(O,O-diethylphosphorodithioate) with three equivalents of ferric chloride in ether solution has been found to give ferrous chloride, bis-(O,O-diethylthiophosphoryl) disulfide and dichloroantimony O,O-diethyl phosphorodithioate as the major products.However, a relatively low yield of bis-(O,O-diethylthiophosphoryl) trisulfide was also obtained.The structures of these products were established by independent syntheses.Several additional antimony(III) tris-(O,O-disubstituted phosphorodithioates) were prepared, and the major organic product obtained by reaction of each of these compounds with three equiva lents of ferric chloride was the corresponding bis-(O,O-disubstituted thiophosphoryl) disulfide.A mechanism for this reaction has been suggested, and evidence in support of the mechanism has been presented.The various antimony(III) tris-(O,O-dialkyl phosphorodithioates) are passivating agents in petroleum refining.The results reported in this and in our previous papers indicate that such compounds undergo a variety of reactions with components of crude petroleum prior to the ultimate pyrolysis reactions which occur in the fluid catalytic cracking process.
