Organometallics p. 2179 - 2185 (1985)
Update date:2022-07-30
Topics:
Rees, Wayne M.
Churchill, Melvyn Rowen
Fettinger, James C.
Atwood, Jim D.
The preparation of iridium alkoxide complexes trans-ROIr(CO)(PPh3)2 and their carbonylation to carboalkoxy complexes ROC(O)Ir(CO)2(PPh3)2 are described for R = Me, n-Pr, t-Bu, and Ph. The preparations involve metathetical reactions between trans-Ir(CO)(PPh3)2Cl and NaOR. In the carbonylation an intermediate can be identified by infrared and conductivity studies as [Ir(CO)3(PPh3)2+][OR-]. Thus a mechanism involving alkoxide displacement by CO and subsequent nucleophilic attack of alkoxide on a CO of the cation is indicated. The complex trans-PhOIr(CO)(PPh3)2 crystallizes in the centrosymmetric monoclinic space group P21/c (no. 14) with a = 15.790 (3) ?, b = 11.461 (3), c = 19.986 (5) ?, β = 100.326 (18)°, V = 3558 (2) ?3, and Z = 4. Diffraction data (Mo Kα, 2θ = 5-55°) were collected with a Syntex P21 automated four-circle diffractometer, and the structure was solved and refined to RF = 6.2% and RwF = 4.6% for all 8220 reflections (RF = 3.8% and RwF = 4.1% for those 5981 reflections with |F0| > 6σ(|F0|)). The iridium atom has the expected square-planar geometry with Ir-P(1) = 2.328 (1) ?, Ir-P(2) = 2.344 (1) ?, Ir-CO = 1.795 (5) ?, and Ir-OPh = 2.049 (4) ?. The phenoxide ligand is "bent" with 〈Ir-O-C(ipso) = 126.5 (3)°.
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Doi:10.1021/jo00225a056
(1985)Doi:10.1021/jo971046m
(1997)Doi:10.1246/cl.1997.399
(1997)Doi:10.1016/0022-328X(85)87264-8
(1985)Doi:10.1002/chem.201403357
(2014)Doi:10.1016/S0040-4020(01)93219-3
(1964)