Synthesis of mer-trichlorotris(tetrahydrofuran)tungsten (III) by intermetal chlorine atom transfer

Article abstract of DOI:10.1016/S0020-1693(97)06157-4

The three-coordinate titanium(III) complex Ti(N[R]Ar)₃ (R = C(CD₃)₂CH₃, Ar = 3,5-C₆H₃Me₂) abstracts chlorine from WCl₄(DME) (DME = 1,2-dimethoxyethane) in tetrahydrofuran (THF) to give yellow crystalline WCl₃(THF)₃ in 65% isolated yield. Orange TiCl(N[R]Ar)₃, which can be recycled to Ti(N[R]Ar)₃ in 73% yield by reduction with sodium amalgam, was recovered in 71% yield. WCl₃(THF)₃ was characterized by elemental analysis, SQUID magnetic susceptibility measurements, ¹H NMR spectroscopy and single crystal X-ray crystallography. WCl₃(THF)₃ was found to be an octahedral complex possessing a meridional arrangement of ligands, as has been seen for other MCl₃(THF)₃ complexes (M = Sc, Ti, V, Cr, Mo).