Synthesis and characterization of fac-tris(trimethylphosphino)iridium(III) silane complexes

Article abstract of DOI:10.1021/om00004a037

The synthesis and characterization of iridium(III) silyl complexes of the form IrHX(PMe₃)₃-SiRR′₂ (X = H or D; R = H, D, Cl, or Ph; R′ = Ph or t-Bu) are described. The complexes are prepared by the oxidative addition of SiXRR′₂ to IrH(PMe₃)₄ with the loss of PMe₃. Three of the complexes have been characterized by single-crystal X-ray diffraction techniques: IrH₂-(PMe₃)₃(SiHPh₂), triclinic, space group P1, a = 9.793(2) ?, b = 16.385(2) ?, c = 16.807(4) ?, α = 88.32(2)°, β = 99.70(2)°, γ = 94.72(2)°, V = 2649.0(10) ?³, Z = 4; IrH₂(PMe₃)₃(SiCl(t-Bu)₂), orthorhombic, space group Pbca, a = 18.519(3) ?, b = 15.264(2) ?, c = 18.982(3) ?, V = 5635.6(15) ?³, Z = 8; and IrH₂(PMe₃)₃(SiPh₃), C2/c, a = 34.011(7) ?, b = 9.779(2) ?, c = 18.733(4) ?, β = 105.46(3)°, V = 5998(2) ?³, Z = 8. Refinement to convergence gave the conventional and weighted agreement factors R = 0.038 and R_w = 0.042, R = 0.037 and R_w = 0.040, and R = 0.061 and R_w = 0.075 for each structure, respectively.