Synthetic studies for the preparation of phosphorus carbonyl rhenacycles with the selenoimidodiphosphinate ligand [N(SePPh 2) 2

Abstract

The synthesis of the rhenacycles [Re(CO) 3(PR 3){Ph 2P(Se)NP(Se)Ph 2-κ 2 Se}], PR 3 = PPh 3 ( 1), PMePh 2 ( 2), and PMe 2Ph ( 3) by a straightforward high yield procedure is described. Attempts at the preparation of the spiro [Re(CO) 2(Ph 2PCH 2CH 2PPh 2-κ 2P){Ph 2P(Se)NP(Se)Ph 2-κ 2 Se}] resulted in the formation of complexes [Re 2(CO) 6{Ph 2P(Se)NP(Se)Ph 2-κ 2 Se} 2(μ-Ph 2PCH 2CH 2PPh 2)] ( 4) and [Re(CO) 3(Ph 2PCH 2CH 2PPh 2-κ 2P){Ph 2P(Se)NP(Se)Ph 2-κ Se}] ( 5). All new inorganic rhenacycles 1– 5 were characterized in solution and in solid state. The X-ray diffraction analysis of [Re(CO) 3PPh 3{Ph 2P(Se)NP(Se)Ph 2-κ 2 Se}] showed that its MnSePNPSe ring conformation is sensitive to temperature.