Synthesis of a novel organoiridium(I) fluoro complex

Abstract

Cyclooctadienefluorotriphenylphosphaneiridium(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 P2(1)/n. The lattice parameters are alpha = 931.9(3) pm, b = 1629.4(7) pm, c = 1592.9(7) pm, alpha = gamma = 90degrees, beta = 92.85(3)degrees. 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 P2(1)/c. The lattice parameters are alpha = 1157.4(9) pm, b = 1864.4(9) pm, c = 1922.5(17) pm, alpha = 7 = 90degrees, beta = 96.16(7)degrees. 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 (IrF)-F-... distance) and thus it is assumed that no interactions occur between the fluorine and iridium atoms. ((C) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004).