Cyclometallation reactions inortho-methyl substituted iridium arylsvia CO insertion and oxidative C-H addition. Characterization of the reported IrH[C6H2Me2-(4,6)-CH2-(2)][P(OMe)3]3 as the internally metallated benzoyl complexfac-IrH[C(O)C6H2Me2-(4,6)-H2(2)]-[P(OMe)3]3 by X-Ray diffraction(1)

TLDR: In this paper, the title compound of the iridaindanone type was characterized by x-ray analysis, which corresponds to a distorted octahedron with the phosphite ligands infac positions.

Abstract: The title compound, previously reported as , has been characterized as by x-ray analysis. The complex crystallizes in the triclinic space group P1 witha = 1029.2(4),b = 1192.7(7),c = 1216.6(7) pm, α = 105.42(4), β = 105.95(4), γ = 95.45(4)°, and Z = 2. With 3909 independent reflections for which F0 > 3 σ(F0,), the structure has been refined anisotropically to R = 0.048. The molecular geometry corresponds to a distorted octahedron with the phosphite ligands infac positions. The complex contains a five-membered metallocycle of the iridaindanone type, , in which the metal deviates slightly from the plane defined by the carbon atoms. Important bond distances are Ir-P = 230.1(3), 230.6(4), and 228.0(3) pm, Ir-C(O) = 207(1) pm, and Ir-CH2 = 213(1) pm. On the basis of the x-ray results and further i.r. and13C n.m.r. data, the structures of a series of related complexes, previously regarded as , have also been reformulated as .