Nuclear Magnetic Resonance Studies of Compounds Related to Tetramethyldiphosphine Disulphide

Abstract

The proton n.m.r. spectra of tetramethyldiphosphine disulphide and a number of related compounds have been obtained, yielding values for the nuclear magnetic parameters. Brief commcnts are made on these parameters. D o~~b l e resonance experiments yielded the relative signs of the coupling constants for tetramethyldiphosphine sulphide ancl spectral analysis provided similar information for the disulphide. Con~parisons are made with published data.

Oxidative addition capability of triphosphine iron and ruthenium complexes with methyl iodide

“…In the same chemical shift region there are also the sharp resonances of the methyl protons. The methyl groups bonded to the terminal phosphorus atoms show higher-order splitting patterns as reported earlier [15][16][17]. As observed in the 1 H NMR, the non-equivalence of the -PMe 2 methyl groups is also recognizable in the 13 ppm) displaying broad signals except in the case of 2, where a quartet resonance was found at d 218.1 ppm.…”

The Reaction of Bunsen's Cacodyl Disulfide, Me2As(S)‐S‐AsMe2, with Iodine: Preparation and Properties of Dimethylarsinosulfenyl Iodide, Me2As‐S‐I

“…Under 1:1 molar ratio, the clear colorless solution, in 1 h, contained “protonated” Et 3 N and only 0.04 molecules of complexed 3 , 0.03 molecules of 2 , 0.02 molecules of an unknown species at 1.852 ppm, and 0.90 molecules of an unknown species at 1.299 ppm were seen. The later singlet is in‐between the singlets of cacodyl (Me 2 As–AsMe 2 ) at δ = 1.11 ppm38 and Me 2 As–S–AsMe 2 or 2 at 1.399 ppm 8. Working up gave a white, needle‐like solid, not suitable for X‐ray analysis, that was analyzed as 3Et 3 N · 2I 2 .…”

Preparation and Properties of Sodium Dimethyldithioarsinate Dihydrate, Me2AsS2Na·2H2O, and Palladium(II) Dimethyldithioarsinate, (Me2AsS2)2Pd

“…The highly reactive diarsine 8 shows a resonance at ca. 1.25 ppm (1.1 ppm in CDCl 3 35) and should give 13 and 14 by reaction with H 2 O 36. The dimethylarsane, being a strong reducing agent 37, must react with the dimethylarsinous acid ( 14 ) to give the anhydride 11 and hydrogen.…”