Neutron diffraction study of fac-[IrH3(PPh2Me)3]·MeOH

Abstract
The structure of the methanol solvate of the facial isomer of [IrH3(PPh2Me)3] has been analysed by neutron diffraction. Data were obtained at 55 ± 0.1 K using a single crystal of volume 17.6 mm3 and the structure refined to final agreement factors of R(F2)= 0.053 and R′(F2)= 0.064 for 1615 reflections. The Ir atom is situated on a three-fold rotation axis. Distances and angles correspond well to those expected for a complex with normal terminal H atoms: Ir–H 1.627(4), Ir–P 2.314(2)Å; H–Ir–H 83.4(2), P–Ir–P 98.6(1), and H–Ir–P 88.5(2), 169.1(2)°. As expected, the overall geometry of the complex is distorted octahedral, with the hydrogen ligands compressed together by the steric bulk of the phosphines, as evidenced by the H–Ir–H (>90°) and P–Ir–P (>90°) angles. The compound crystallizes in the rhombohedral space group R3, with a= 10.367(1)Å and α= 108.19(6)° at T= 55 ± 0.1 K.

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