The title compounds, R~PAuSC(=NP~)OR', R = Et, Ph or Cy and R' = Me, Et, Pr, pri or Cy, have been prepared and characterized by spectroscopic methods (i.r., 'H and 13c n.m.r. and f.a.b. m.s.) and, in the case of the R = Ph and R' = Me compound, by single-crystal X-ray diffraction methods. The spectroscopic data are consistent with the R3PAu moiety being coordinated by the sulfur atom of the thiolate ligand. This has been confirmed by an X-ray study on PhaPAuSC(=NPh)OMe which shows the gold atom to be linearly coordinated by the phosphorus and sulfur atoms; Au-P(1) 2.258 (1), Au-S(1) 2.301(1) A and P-Au-S 177.7(1)'. Crystals of PhsPAuSC(=NPh)OMe are triclinic, space group pi, with unit cell dimensions: a 10.825(1), b 12.553(2), c 8.914(2) a, a 97.86(2), , B 93.79(1), y 88.60(1)O, V 1197.1 fi3, Z 2. The structure was refined by a full-matrix least-squares procedure to R 0.028 for 4409 reflections with I > 2.5a(I). A J(P-H). N-Ph resonances overlap with P-Ph resonances. Obscured.1989, 1803.
A number of phosphinegold(I) thiolates where, generally, the thiolate is derived from a
thionucleobase, have been screened for anti-arthritic activity in Dark Agouti rats, a gold
sensitive model for arthritis. Potency and toxicity data showed that, generally, the Ph3P derivatives and species based on thiopurines were the most effective and that with other
complexes enhanced activity was accompanied by greater toxicity.
The crystal structures of the title compounds R 3 PAu(S 2 CO-c-C 6 H n ), R = Et, Ph and c-hexyl, have been determined at room temperature. Monoclinic crystals of the R = Et compound have space group C2/c with unit cell dimensions a = 26.754(4) A, b = 7.264(1) Â, c = 18.928(3) A, β = 102.04(1)°, Z= 8 and D x = 1.811 Mg_m" 3 . Crystals of the R = Ph structure are triclinic with space group Pi and unit cell dimensions a = 11.372(2) À, ¿> = 13.053(6) A, c = 9.488(3)Â; α = 109.45(3)°, β = 99.19(2)°, y = 106.28(3)°, Ζ = 2 and D x = 1.722 Mg m -3 . The R = c-hexyl compound crystallizes in the orthorhombic space group Ρ1χ2 χ 2 χ with unit cell dimensions a = 8.121(1) A, b = 11.108(4) A, c = 30.212(5) A, Ζ = 4 and D x = 1.591 Mgm" 3 . The structures were refined by a full-matrix leastsquares procedure on 1908 reflections to final Λ = 0.039 for the R = Et compound, 3664 reflections and R = 0.055 for R = Ph and 1501 reflections and R = 0.040 for R = c-hexyl. The Au atom in each of the structures is linearly coordinated by the S atom, derived from a monodentate xanthate ligand, and the Ρ atom. Different orientations of the xanthate ligands results in two structural forms. For the R = Et and Ph compounds the O atom is in close proximity of the Au atom whereas for the R = c-hexyl compound the S atom is orientated towards the Au atom. The different structures are rationalized in terms of the steric demands of the phosphine ligands. A close Au...Au interaction of 3.120(1) A is found in the R =
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