Synthesis, characterization and the unpleasantly disordered crystal structure of Ir(OMe)(CO)(PPh3)2(SO4)

Article abstract of DOI:10.1016/0022-328X(88)80031-7

The adducts of O2 and SO2 with trans-MeOIr(CO)(PPh3)2 are formed in equilibria and have been characterized.Reaction of the SO2 adduct, Ir(OMe)(SO2)(CO)(PPh3)2 with dioxigen leads to the sulfato complex, Ir(OMe)(CO)(PPh3)2(SO4), the structure of which has been determined.Ir(OMe)(CO)(PPh3)2(SO4) crystallizes in the monoclinic system with a 11.958(2), b 14.163(3), c 12.231(2) Angstroem, β 118.365(12) deg, V 1822.7(6) Angstroem³ and Z=2.Diffraction data for 2θ=4.5-45.0 deg (Mo-K_α) were collected with a Syntex P2₁ diffractometer and the structure was solved (assuming space group P2₁/m and an unpleasant 2-fold disordered model) and refined to R=4.8percent for all 2512 independent data (R=3.5percent for those 2042 data with <*>F₀<*>>6?(<*>F₀<*>)).The iridium(III) atom has a distorted octahedral coordination sphere with trans PPh3 ligands and a cis-chelating bidentate O,O'-SO4 group; the structure is completed by mutually cis OMe and CO ligands.