Synthesis and structural characterisation of the oxo-rhenium(V) complexes with spirophosphorane derived bidentate ligand (P similar to O-). Crystal structure of trans-ReOCl2[OCMe2CMe2OP(OCMe2CMe2O)](PPh3)

摘要

The reactions of ReO(OEt)Cl2L2. L = py, PPh3 or ReOCl3(Me2S)(OPPh3), with spirohydrophosphorane HP(OCMe2CMe2O)(2) - abbreviated here as HP similar to O - in toluene yield ReOCl2(P similar to O)L complexes, L = py (1), PPh3 (2) and OPPh3 (3), respectively. The encountered bidentate phosphite pinacolato (OCMe2CMe2O)POC Me2CMe2O ligand (P similar to O-) is afforded by means of a spirophosphorane ring-opening reaction. All the pink-violet compounds 1-3 were characterised by NMR. IR and UV-Vis spectroscopies. The structure of rrans-ReOCl2(P similar to O)PPh3 (2) was determined crystallographically. The rhenium atom adopts distorted octahedral geometry with a trans multiply bonded terminal oxo ligand (Re-O-t = 1.698(2) Angstrom) trans to pinacolate oxygen (Re-O = 1.880(2) Angstrom). Two phosphorus atoms as well as two chlorides are mutually in a trans arrangement. (C) 2000 Elsevier Science B.V. All rights reserved. [References: 53]