Synthesis and characterization of oxo-rhenium(V) complexes with monodentate P(OCH3)3 and bidentate [OC(CH3)2C(CH3)2O]POC(CH3)2C(CH3)2 OP[OC(CH3)2C(CH3)2O] phosphite ligands

Abstract

The reactions of ReOCl3(Me2S)(OPPh3) with monodentate P(OMe)3 (P) and bidentate (OCMe2CMe2O)POCMe2CMe2OP(OCMe2CMe2O), (P–P) phosphites afford fac-ReOCl3P2 (1) and fac-ReOCl3(P–P) (2) respectively. Both blue–violet 1 and 2 have been characterized by NMR, IR and UV–Vis spectroscopies as well as by X-ray crystallography. Crystal data of ReOCl3P2 (1): crystal class triclinic, space group 1̄ (No 2), a=8.558(2), b=8.921(2), c=12.617(3) Å; α=74.42(3), β=81.81(3), γ=63.43(1)°; V=829.6(3) Å3, Z=2. Crystal data of ReOCl3(P–P) (2): monoclinic, space group P21⧹n, (P21⧹c No 14), a=9.615(2), b=16.424(3), c=17.395(3) Å; β=99.81(3); V=2706.8(9) Å3, Z=4. There is 72:28 orientational disorder in 2 between the mutually trans-oxo and chloride ligands. In both 1 and 2, the rhenium atoms are six coordinate with triply bonded terminal oxo ligands (1 Re–O=1.654(4) Å), (2 Re–O=1.692(15) Å) and chlorides in facial arrangements.