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The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphosPh Complexes
Published on: April 10, 2015
Iridium Complexes of a Bis(N-pyrrolyl)boryl/Bis(phosphine) PBP Pincer Ligand
Samuel R Lee1, Nattamai Bhuvanesh1, Oleg V Ozerov1
1Department of Chemistry, Texas A&M University, College Station, Texas 77842, United States.
Abstract:
This work reports the synthesis of a bis(pyrrolylphosphino)phenyl borane (PBP)Ph (2) and its incorporation of Ir by metal insertion into B-Ph to afford the dipyrrolylboryl/bis(phosphine) pincer complex (PBP)Ir(Ph)Cl (3). Hydrogenolysis of 3 afforded (PBP)Ir(H)Cl (4). Compound 4 was converted into (PBP)IrCl2 (5a) via reaction with N-chlorosuccinimide, and exposure of 5a to CO produced (PBP)IrCl2(CO) (6a). Compounds 5a and 6a were converted into their analogs (PBP)IrI2 (5b) and (PBP)IrI2(CO) (6b) via metathesis with Me3SiI, respectively. Treatment of either 3 or 4 with Li[HAl(OtBu)3] under H2 resulted in the formation of (PBP)IrH4 (7), with traces of 4 as a persistent impurity. Attempts to access 7 via the reaction of 4 with NaBH4 in isopropanol led to the loss of boron from the pincer and isolation of L2IrH5 (8, L = 2-diisopropylphosphinopyrrole). Compounds 4, 7, and 8 were examined as catalysts for alkane transfer dehydrogenation but displayed only the modest activity. Solid-state structures of 6b and 7 were established by X-ray crystallography.
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