Journal of Organometallic Chemistry p. 281 - 294 (1985)
Update date:2022-08-03
Topics:
Begley, Michael G.
Gaffney, Christine
Harrison, Philip G.
Steel, Andrew
The crystal and molecular structures of three organolead compounds containing lead-sulphur bonds are described.Crystals of triphenyllead benzenethiolate (I, C24H20Pbs) are in the monoclinic space group P21/c, with a 7.657, b 16.427, c 16.239 Angstroem, β 93.781 deg, Z=4; crystals of triphenyllead O,O'-diethyldithiophosphate (II, C22H25O2PPbS2), and diphenyllead bis(O,O'-dibenzyldithiophosphate) (III, C40H38O4PbS4) are both in triclinic space group P<*>, with a 9.579, b 10.602, c 12.710 Angstroem, α 101.623, β 99.554, γ 100.719 deg, Z=2, and a 11.760, b 12.532, c 16.263 Angstroem, α 80.14, β 111.46, γ 112.41 deg, Z=2, respectively.Structures were determined by the heavy atom method using 2820, 2752, and 3084 independent, non-zero reflections with I>3?(I) for compounds I, II and III, respectively, collected using an automated four-circle diffractometer using Mo-Kα radiation (λ 0.71069 Angstroem).The refinements converged at conventional R-values of 3.44percent, 7.40percent and 7.68percent for I, II, and III, respectively.Both Ph3PbSPh and Ph3PbS2(OEt)2 form lattices comprising non-interacting molecules with geometries at lead only slightly distorted from tetrahedral.The distortion in the dithiophosphate is somewhat greater than in the benzenethiolate, and is accompanied by a marginally longer lead-sulphur distance (2.554(6) Angstroem vs. 2.515(2) Angstroem).The lead in Ph2Pb
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