Reactions of TiCl4 or Ti(O-i-Pr)Cl3 with 2,4-pentanedione. The molecular structures of TiCl3(acac)(THF) and Ti(O-i-Pr)Cl2(acac)(THF)

Abstract

A series of titanium(IV) acetylacetonate (acac) complexes, Ti(acac)Cl3 (THF) (2), [Ti(acac)Cl2(THF)]2 (μ-O) (3), [Ti(O-i-Pr)Cl3(acac)](HNEt3+) (5), and Ti(O-i-Pr)Cl2 (acac)(THF) (6), were prepared from reactions of TiCl4 or Ti(O-i-Pr)Cl3 with 2,4-pentanedione (Hacac) in CH2Cl2 or THF with or without the presence of NEt3. The x-ray structural analyses were carried out on complexes 2 and 6. Complex 2 crystallizes in the monoclinic P21/n space group with a = 8.664(1) A°, b = 11.859(1) Å, c = 14.320(1) Å, β= 103.94(1)°, R = 0.0571, Rw = 0.0620, and Gof = 1.10. Complex 6 crystallizes also in the monoclinic P2t/n space group with a = 9.074(2) Å, b = 11.499(2) Å, c = 16.549(4) Å, β= 101.96(2)°, R = 0.0492, Rw = 0.0671, and Gof = 1.49. Based on the solid state structures of complexes 2 and 6, the relative bonding order of O-i-Pr > Cl > acac> THF is established.