Direct Electrochemical Synthesis and Crystallographic Characterization of Metal Diphenylphosphido and Diphenylthiophosphinato Compounds, and some Derivatives

DOI: 10.1039/DT9910000011

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 11 - 18 (1991)

Update date:2022-08-05

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Authors:

Annan, Theodore A.

Kumar, Rajesh

Tuck, Dennis G.

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Article abstract of DOI:10.1039/DT9910000011

The electrochemical oxidation of a number of metals in acetonitrile solutions of PPh2H gives rise to M(PPh2)n compounds (M = Co, Zn or Cd, n = 2; M = Cu, Ag or Au, n = 1).With anodic nickel the product is Ni(PPh2).PPh2H.In the presence of elemental sulphur such oxidation reactions yield (M = Co, Zn or Cd).The electrochemical processes involved have been identified.The crystal structure of the addition compound .4MeCN 1 has been determined by X-ray crystallography, which reveals a Cu4P4 ring, capped by Cu2PCP'2 rings.Crystal parameters: triclinic, space group P1, a = 14.719(4), b = 13.649(5). c= 17.112(5) Angstroem, α = 112.40(3), β = 106.22(2), γ = 115.39(2) deg and Z = 1; R = 0.0632 for 3622 observed reflections = 3?(l)>.The compound Ni)PPh2).PPh2H is oxidized by elemental oxygen, sulphur or selenium to give (E = O, S or Se), and also reacts with PhNCS to yield 2>. 2.Crystal parameters: triclinic, space group P1, a= 8.950(6), b = 9.745(4), c = 10.366(7) Angstroem, α = 112,28(4), β = 99.09(5), γ = 90.88(4) deg, and Z = 1.Disorder prevented this structure from being refined beyond R = 0.1612, but the essential features of the square-planar NiS2P2 core were identified.The crystal parameters of 3 are monoclinic, space group P2,/c, a = 12.420(5), b = 9.737(7), c = 20.729(16) Angstroem, β = 100.29(5) deg, and Z = 2.The nickel atom is co-ordinated by two monodentate Ph2PO(O)^- ligands and two monodentate Ph2P(O)OH ligands which are hydrogen-bonded to their anionic analogues, and by two MeCN molecules, to give a NiO2O'2N2 core.

Full text of DOI:10.1039/DT9910000011

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