Reaction of Diisobutylaluminum Hydride with Bis(Diphenylphosphinoyl)Ethane. Synthesis and Structure of [AI(C4H9)3]2[dppe]

Reaction of an excess of diisobutylaluminum hydride with bis(diphenylphosphinoyl)ethane (dppe-O2), the di-oxygen derivative of bis(diphenylphosphino)ethane (dppe), in heptane affords the crystalline product [AI(C4H9)3]2[dppe]. The title compound crystallizes in the triclinic space group PI with unit cell parameters a = 9.514(3), b = 10.417(4), c = 13.364(4) Å, α = 97.67(3), β = 102.09(2), Δ = 95.49(3)°, V= 1273.1(7)Å3, and D c = 1.04g cm−3 for Z= 1. Least-squares refinement based on 2455 observed reflections (I > 3σ (I)) converged at R = 0.059, R w = 0.070. The title compound results from a unique reaction wherein dppe and triisobutylaluminum were generated in situ from dppe-O2 and diisobutylaluminum hydride, respectively.