Synthesis and x‐ray crystal structure of the TiMgCl5(OOCCH2Cl) · (ClCH2COOC2H5)3 Adduct

Abstract

AbstractThe synthesis of the TiMgCl5(OOCCH2Cl) · (ClCH2COOC2H5)3 adduct, obtained by reacting TiCl4 with a solution of MgCl2 in dry ClCH2COOC2H5, is reported together with its molecular and crystal structure as determined by x‐ray diffraction. The structure was solved by direct and Fourier methods and refined by least‐squares techniques to R = 0.057 for 1318 independent observed reflections. Crystals are monoclinic, space‐group P21/c, with 4 formula units in a unit‐cell of dimensions a = 10.480(4), b = 19.641(9), c = 16.597(6) Å, β = 120.21(5)°. The titanium(IV) atom is octahedrally coordinated by five chlorine atoms and an oxygen atom of a OOCCH2Cl residue. The magnesium atom is similarly coordinated by two chlorine atoms, the carbonyl oxygen atoms of three ClCH2COOC2H5 molecules and an oxygen atom of the OOCCH2Cl residue. The two octahedra share an edge by a double chlorine bridge between the magnesium and the titanium atoms and are also connected by the COO group of the OOCCH2Cl residue. Changes in the configurations and dimensions with respect to the free acceptor and donor molecules are discussed.