Reaction of organoaluminium species with bidentate phosphine ligands. Synthesis and molecular structure of [AlCl 3][(Ph 2P) 2CH 2][AlCl 2(CH 3)] and [AlCl 3] 2[(Ph 2P(O)) 2CH 2

Abstract

Reaction of methylaluminium sesquichloride with bis(diphenylphosphino) methane and bis(diphenylphosphinoyl)methane affords [AlCl 3][(Ph 2P) 2CH 2][AlCl 2(CH 3)] ( I) and [AlCl 3] 2[(Ph 2P(O)) 2CH 2] ( II), respectively. Compound I crystallizes in the triclinic space group P−1 with unit cell parameters a = 10.009(3), b = 10.748(4), c = 14.806(5) Å, α = 90.38(3), β = 103.36(2), γ = 96.89(3)°, V = 1537.5 Å 3 and ϱ = 1.36 for Z = 2. Compound II crystallizes in the monoclinic space group C2 with unit cell parameters a = 12.773(2), b = 13.028(3), c = 9.461(2) Å, β = 104.43(2)°, V = 1524.60 Å 3 and ϱ = 1.49 for Z = 2. Full-matrix least-squares refinement based on 3034 observed reflections for I converged at R = 0.047 ( R w = 0.066); full-matrix least-squares refinement based on 1565 observed reflections for II converged at R = 0.043 ( R w = 0.050). Both products result from reaction of the disproportionation products of methylaluminium sesquichloride, AlCl 3 and AlCl 2(CH 3).