Add time:07/31/2019         Source:sciencedirect.com

Reaction of [(η4-COD)Ir(μ2-Cl)]2 (1) with tin CH2CRCHCRCH2SnR′3 (R = H, Me; R' = Me, n-Bu) or lithium pentadienide reagents gives the corresponding acyclic pentadienyl sandwich compounds [(η4-COD)Ir(η5-CH2CMeCHCMeCH2) (2) and [(η4-COD)Ir(η5-CH2CHCHCHCH2) (3). Treatment of 1 with different phosphines affords the well-known mononuclear phosphine complexes [(η4-COD)IrClPR3] [R = Ph, 4; i-Pr, 5; Me, 6] which react with lithium pentadienide to give the exclusive formation of [(η4-COD)Ir(1-3-η-CH2CHCHCHCH2)PR3] [R = Ph, 7; P(i-Pr), 8], whereas the less steric trimethylphosphine shows an equilibrium mixture of the pseudo iridacyclic [(η4-COD)Ir(1,4-5′-η-CH2CHCHCHCH2)PMe3] (9a) and [(η4-COD)Ir(1-3-η-CH2CHCHCHCH2)PMe3] (9b) in a 2:1 ratio. Additionally, the addition reaction of phosphines to compound 2 gives the dimethyl-pentadienyl complexes [(η4-COD)Ir(1-3-η-CH2CMeCHCMeCH2)PPh3] (10) and the mixture of isomers [(η4-COD)Ir(1,4-5′-η-CH2CMeCHCMeCH2)PMe3] (11a) and [(η4-COD)Ir(1-3-η-CH2CMeCHCMeCH2)PMe3] (11b) in a 2:1 ratio. Compounds 2, 4, 5, 6, 7, 8, 9b, 10 and 11a have been structurally characterized by single-crystal X-ray diffraction studies. The influence of the electronic and steric effects of the different ligands, as well as the preference of the bonding modes in the pentadienyl ligands is analyzed and contrasting to pentadienyl electron rich complexes, derived from IrCl(PR3)3, previously described in the literature.

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