118831-57-5Relevant articles and documents
Gold and silver hydrides: Synthesis of heterobimetallic Ir-M (M = Au, Ag) complexes and X-ray crystal structures of [(PPh3)Au(μ-H)IrH2(PPh3) 3](BF4) and [(PPh3)Ag(μ-H)IrH2(PPh3) 3](CF3SO3)
Albinati, Alberto,Anklin, Clemens,Janser, Philipp,Lehner, Hans,Matt, Dominique,Pregosin, Paul S.,Venanzi, Luigi M.
, p. 1105 - 1111 (2008/10/08)
The hydrido-bridged cationic complexes [(PR3)M(μ-H)IrH2(PPh3)3](CF 3SO3) (M = Au, Ag; R = Ph, Et) have been prepared and characterized by NMR (1H, 31P, and 109Ag) and crystallographic methods. The three PPh3 ligands on iridium have mer geometry. The complexes show dynamic behavior in solution, which exchanges the bridging hydride with the terminal hydride trans to PPh3. It is shown that the J(109Ag, 1H) values obtained from the two-dimensional 109Ag NMR spectra are useful in distinguishing bridging from terminal hydrides. The crystals of [(PPh3)Au(μ-H)IrH2(PPh3) 3](BF4)·CH2Cl2 (1b·CH2Cl2) belong to space group P1 with Z = 2, a = 17.482 (6) A?, b = 15.617 (5) A?, c = 13.218 (5) A?, α = 90.97 (4)°, β = 71.38 (3)°, γ = 103.89 (5)°, and V = 3312.9 (4) A?3. The structure was refined by block-diagonal least squares to R = 0.054 for the 3792 observed reflections. The crystals of [(PPh3)Ag(μ-H)IrH2(PPh3) 3](CF3SO3) (3), in the form of its benzene solvate, belong to the monoclinic space group Cc with Z = 4, a = 19.461 (4) A?, b = 19.458 (5) A?, c = 20.054 (4) A?, β = 96.16 (2)°, and V = 7550.3 (4) A?3. The structure was refined by full-matrix least squares to R = 0.049 for the 2842 observed reflections.
