AbstractCyclooctadienefluorotriphenylphosphaneiridium(I) [IrF(C8H12)(PPh3)] (3) was prepared and its structure determined by single crystal X‐ray diffraction analysis. Complex 3 crystallises in the monoclinic space group P21/n. The lattice parameters are a = 931.9(3) pm, b = 1629.4(7) pm, c = 1592.9(7) pm, α = γ = 90°, β = 92.85(3)°. Number of molecules per unit cell is 4. The square planar iridium complex 3 exhibits an Ir−F bond length of 201.3(5) pm. 3 was obtained in Teflon tubes, whereas the use of glass vessels led to cyclooctadiene‐bis(triphenylphosphane)iridium(I)‐pentafluorosilicate(IV) ([Ir(C8H12)(PPh3)2][SiF5]) (4). The composition of 4 was confirmed by single crystal X‐ray diffraction analysis. 4 crystallises in the monoclinic space group P21/c. The lattice parameters are a = 1157.4(9) pm, b = 1864.4(9) pm, c = 1922.5(17) pm, α = γ = 90°, β = 96.16(7)°. The number of molecules per unit cell is 4. The square‐planar coordinated iridium cation [Ir(C8H12)(PPh3)2]+ is separated from the trigonal bipyramidal [SiF5]− anion by 461.1 pm (shortest Ir···F distance) and thus it is assumed that no interactions occur between the fluorine and iridium atoms. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004)
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