Crystal-Structure of 0.53[Mer-(Pme2ph)3cl3iriii] 0.47[Mer-(Pme2ph)3- Trans-Cl2hiriii]

Abstract

Evaporation of a methanol solution containing both mer -(PMe₂Ph)₃Cl₃Ir^III (1) and mer -(Pme₂Ph)₃H-trans-Cl₂Ir^III (2) yields a new crystalline species (3) which is morphologically distinct from either (1) or (2). The structure of (3) has been determined by single-crystal X-ray diffraction analysis. Crystals are monoclinic, space group P2₁/c, with a 15.747(2), b 10.305(1), c 16.790(2)Ǻ, β 92.75(3)° and Z 4, and contain, in approximately equal amounts, discrete molecules of both (1) and (2) distributed randomly in common lattice sites. Site content differs only according to whether there is H or Cl trans to the unique phosphine ligand . Structure refinement by full-matrix least-squares analysis (6183 reflections, 413 parameters) converged with R = 0.026, Rw = 0.034, and site occupancy factor for the unique chlorine atom equal to 0.530(4). Molecules each exhibit the conformation observed for pure (1) [pure (2) differs]. Derived metal- ligand distances are very similar to the weighted averages [53% (1), 47% (2)] of the corresponding distances in (1) and (2).