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A series of new ferrocene- and ruthenocene-containing iridium(III) heteroleptic complexes of the type [(ppy) 2 Ir(RCOCHCOR')], with ppy = 2-pyridylphenyl, R = Fc = Fe II (η 5 -C 5 H 4 )(η 5 -C 5 H 5 ) and R' = CH 3 ( 1 ) or Fc ( 2 ), as well as R = Rc = Ru II (η 5 -C 5 H 4 )(η 5 -C 5 H 5 ) and R' = CH 3 ( 3 ), Rc ( 4 ) or Fc ( 5 ) was synthesized via the reaction of appropriate metallocene-containing β -diketonato ligands with [(ppy) 2 (-Cl)Ir] 2 . The single crystal structure of 3 (monoclinic, P2 1 /n, Z = 4) is described. Complexes 1 - 5 absorb light strongly in the region 280-480 nm the metallocenyl -diketonato substituents quench phosphorescence in 1 - 5 . Cyclic and square wave voltammetric studies in CH 2 Cl 2 /[N( n Bu) 4 ][B(C 6 F 5 ) 4 ] allowed observation of a reversible Ir III/IV redox couple as well as well-resolved ferrocenyl (Fc) and ruthenocenyl (Rc) one-electron transfer steps in 1 - 5 . The sequence of redox events is in the order Fc oxidation, then Ir III oxidation and finally ruthenocene oxidation, all in one-electron transfer steps. Generation of Ir IV quenched phosphorescence in 6 , [(ppy) 2 Ir(H 3 CCOCHCOCH 3 )]. This study made it possible to predict the Ir III/IV formal reduction potential from Gordy scale group electronegativities, χ R and/or Σχ R  ' of -diketonato pendent side groups as well as from DFT-calculated energies of the highest occupied molecular orbital of the species involved in the Ir III/IV oxidation at a 98 % accuracy level.

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Synthesis, Spectroscopy and Electrochemistry in Relation to DFT Computed Energies of Ferrocene- and Ruthenocene-Containing -Diketonato Iridium(III) Heteroleptic Complexes. Structure of [(2-Pyridylphenyl)2Ir(RcCOCHCOCH3]