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Durch oxydative Addition von Carbonsäuren an Aryliridium(I)‐Verbindungen Ir(Ar)(CO)(PPh3)2 konnten cis‐Arylhydridoiridium(III)‐Komplexe IrH(Ar)(O2CR)(CO)(PPh3)2 (R = Me: Ar = C6H5, 4‐MeC6H4; R = Et: Ar = 4‐MeC6H4, 2,4‐Me2C6H3) dargestellt werden. Reaktion aliphatischer Carbonsäuren mit Alkyliridium(I)‐Derivaten Ir(Alk)(CO)(PPh3)2 und Ir(Alk)[PhP(CH2CH2CH2PPh2)2] (Alk = CH2CMe3, CH2SiMe3) führte zu Dicarboxylatoiridium(III)‐Hydriden IrH(O2CR)2(CO)(PPh3)2 (R = Me, Et, i‐Pr) und IrH(O2CR)2[PhP(CH2CH2CH2PPh2)2] (R = Me, Et). Aus Ir(CH2SiMe3)(CO)(PPh3)2 und 4‐MeC6H4CO2H wurde Ir(4‐MeC6H4CO2)(CO)(PPh3)2 erhalten. Umsetzung von Organorhodiumkomplexen Rh(R′)(CO)(PPh3)2 (R′ = CH2SiMe3, 4‐MeC6H4) und Rh(R′)[PhP(CH2CH2CH2PPh2)2] (R′ = CH2CMe3, 4‐MeC6H4) mit aliphatischen und aromatischen Carbonsäuren ergab Carboxylatorhodium(I)‐verbindungen Rh(O2CR)(CO)(PPh3)2 (R = Me, t‐Bu, 4‐MeC6H4) und Rh(O2CR)[PhP(CH2CH2CH2PPh2)2] (R = Me, 4‐MeC6H4).

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A series of organorhodium and -iridium complexes M(R)(CO)(PPh3)2 (M = Rh: R = C6H5, 2-MeC6H4, 4-MeC6H4, 2,4,6-Me3C6H2, CH3, CH2SiMe3, CH2CMe3; M = Ir: R = CH3, CH2Ph, CH2SiMe3, CH2CMe3) has been prepared from MCl(CO)(PPh3)2 and the corresponding organolithium or Grignard reagents. Of these compounds, the mesitylrhodium complex Rh(2,4,6-Me3C6H2)(CO)(PPh3)2 as well as the iridium and rhodium alkyls with Me3SiCH2 and Me3CCH2 ligands show cis,trans-isomerism which is demonstrated on the basis of infrared and NMR spectroscopic evidence.

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