One pot synthesis of chalcogenolato and phosphino bridged/ligated Mn(I)- and Re(I)-based mono- and dinuclear metallacycles

Abstract

A series of chalcogenolato and phosphino bridged/ligated Mn(I)- and Re(I)-based mononuclear and dinuclear metallacycles were synthesized in a single step under one pot reaction condition from rudimentary starting materials. Metallacycles 1−4 were synthesized by the reaction of diphenyl dichalcogenide (S/Se) and 1,4-bis(diphenylphosphino)butane (dppb) with dimetal decacarbonyl (Mn/Re). Two different shapes of metallacyclic compounds were synthesized using similar kind of metal precursors with different chalcogenolate ligands. Compounds 1 and 2 adapted dinuclear framework of general formula [{(CO)3M(μ-SC6H5)2M(CO)3}(μ-dppb)] (M = Mn/Re) when diphenyl disulfide was reacted with M2(CO)10 (Mn/Re) and dppb, whereas compounds 3 and 4 attained mononuclear structure of general formula [(CO)3M(SeC6H5)(η2-dppb)] (M = Mn/Re) while diphenyl diselenide was treated with M2(CO)10 (Mn/Re) and dppb. Compounds 1−4 were characterized using UV−Vis, IR and NMR spectroscopic techniques and elemental analysis. The molecular masses of metallacycles 1−4 were evaluated by electrospray ionization-mass spectrometry (ESI-MS). Solid-state structural elucidation of compound 3 was carried out using single-crystal X-ray diffraction methods.