OUSL Journal (Dec 2022)
Synthesis of Tricarbonyl Re(I) Complexes of N and P Donor Ligands
Abstract
Reaction of 1,10-phenanthroline-5,6-dione V with 1,3-diphenyl propan-2-one afforded the keto-alcohol VI. Treatment of VI with alkynes, di(3-thienyl) acetylene and di(4-tert-butylphenyl) acetylene yielded 5,8-diphenyl-6,7-di(3-thienyl)-1,12-diaza-triphenylene L1 and 6,7-di(4-tert-butylphenyl)-5,8-diphenyl-1,12-diazatriphenylene L2, respectively. [ReCl(CO)5] reacted with N^N-donor ligands L1-L6 to produce fac-tricarbonylrhenium(I) complexes (20)-(25) in good yields as coloured solids. Treatment of [ReCl(CO)5] with the bulky P^N ligand L7 formed the neutral complex fac-[ReCl(CO)3(L7)] (26) whilst with the azine diphosphine Z,Z-L8 afforded the cationic complex fac-[Re(CO)3(E,Z-L8)]Cl (27a), where L8 is a tridentate ligand. The chloride anion of the complex (27a) was replaced by treating it with NH4PF6 into fac-[Re(CO)3(E,Z-L8)]PF6 (27b). Above complexes were characterized by a combination of elemental analysis, IR, Mass and NMR spectroscopy.
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