Iron Complexes of 4,5-Bis(diorganophosphinomethyl)acridine Ligands

Inorg Chem. 2024 Oct 7;63(40):18655-18668. doi: 10.1021/acs.inorgchem.4c02409. Epub 2024 Sep 26.

Abstract

The search for an iron analog of the established ruthenium-based catalysts containing methylene-extended 4,5-bis(diorganophosphinomethyl)acridine ligands, [FeHCl(CO)(LR)], resulted in the discovery of a bidentate coordination mode of these usually tridentate pincer ligands toward iron. The acridines nitrogen atom does not coordinate to iron, leading to the formation of iron diphos-type complexes with unusually large cis bite angles of up to 124° as well as trans bite angles around 155°. The iron-containing complexes [FeCl22-LR)] (R = iPr, Ph), [FeX22-LCy)] (X = Cl, Br) and [Fe(CO)32-LR)] (R = iPr, Cy) have been isolated in crystalline form and characterized by spectroscopic methods and mass spectrometry. Their structures were verified unambiguously through X-ray diffraction. The stability of the iron(II) complexes decreased in the order Cy > Ph > iPr and Cl > Br > I, although all iron(II) complexes were found to be relatively stable enough for short-term handling in air in the solid state. Notably, no iron(0) complex of the phenyl derivative could be isolated. The iron(0) complex [Fe(CO)32-LCy)] was found to be significantly more stable toward hydrolysis and oxygen compared to [Fe(CO)32-LiPr)] and can be stored in air for months without significant decomposition in the solid state, while [Fe(CO)32-LiPr)] decomposes in air within seconds. The decomposition products [FeI22-O2LCy)], [{Fe(CO)32-HLR)}2] (R = iPr, Cy) and [FeCl2(CO)21-LCy)(κ1-OLCy)] were identified and characterized crystallographically. The iron(0) complex [Fe(CO)32-LCy)] is oxidized by [Fe(Cp)2](BPh4) to give the paramagnetic, low-spin iron(I) cation [Fe(CO)32-LCy)]+. The electron paramagnetic resonance spectrum of the highly sensitive cation as well as density functional theory calculations suggest a partial delocalization of the unpaired electron over the three carbonyl ligands and the acridines aromatic ring system. The catalytic activity and photophysical properties of the complexes have been preliminarily investigated.