New perthiophosphonic acid anhydrides and the direct indication of the dimer‐monomer equilibrium. NMR and X‐Ray Studies

Abstract

New perthiophosphonic acid anhydrides (R-PSJ, with R = 2,4,6-tri-isopropyIphenyI and 2,4-di-tert-butyl-6-methylphenyl haw been prepared. For the latter case, the isolation of the monomer (n = I ) , the 2,4-di-tertbutyl-6-methyIphe~zyI-dithioxophosphorane, and both dimers (n = 2), cis-and trans-2,4-bis(2,4-di-tertbutyl-6-methylphenyl)-2,4-dithioxo-l, 3,2,4-dithiadiphosphetane, of one perthiophosphonic acid anhydride has been perfonned for the first time. The crystal structure of , !,4-di-tert-butyl-6-methylphenyl-di

Diselenadiphosphetandiselenide und Triselenadiphospholandiselenide - Synthese und Charakterisierung mittels31P- und77Se-Festkörper-NMRSpektroskopie

“…analog zu einigen Schwefelverbindungen [10,11] in monomeren Einheiten RP(=Se) 2 auftreten. Auûerdem ko È nnen Nebenprodukte, die den untersuchten Kern enthalten, leicht erkannt werden.…”

Preparation and 31P NMR study of some low‐coordinated organophosphorus compounds bearing the 2,4‐di‐t‐butyl‐6‐isopropylphenyl group

“…Similarly, the electronic-donating effect of the phosphorus-binding hydrogen atoms in Mes*PH 2 may not be so effective as those of PxPH 2 and DbtPH 2 . In the case of DbtP(‫ס‬S) 2 , the ‫מ‬P(‫ס‬S) 2 moiety is slightly deviated from planarity [30] and is less affected by the electron-withdrawing sulfur atoms, compared with the case of Mes*P(‫ס‬S) 2 , in which the ‫מ‬P(‫ס‬S) 2 moiety is planar [31]. In each case, the 2,4-di-t-butyl-6-isopropylphenyl-substituted derivatives showed their chemical shifts close to those of the corresponding 2,4-di-t-butyl-6-methylphenyl derivatives, indicating the unique character of the Mes* group.…”

Step-wise sulfurization of stable 1,2-bis(ferrocenyl)diphosphene

“…Since the 31 P NMR chemical shifts of dithioxophosphorane derivatives are observed in the characteristic lower fielded region (e.g. BbtPS 2 , δ P = 286.7 (11,16), such lower fielded chemical shift of 3 would be explained by the facile equilibrium between 3 and monomeric dithioxophosphorane 4 in solution (16).…”