Abstract
Addition of R′ 2PCl to anilines substituted with di- or trimethylcyclopentadienyl unit at ortho-position affords ortho-phenylene-bridged Me 2Cp or Me 3Cp/phosophinoamide ligands, 2-(RMe 2C 5H 2)C 6H 4NHPR′ 2 (R = Me or H; R′ = Ph, iPr, or Cyclohexyl). Successive addition of Ti(NMe 2) 4 and Me 2SiCl 2 to the ligands affords the desired dichlorotitanium complexes, [2-(η 5-RMe 2C 5H)C 6H 4NPR′ 2− κ 2 N, P]TiCl 2 (R = H, R′ = Ph, 9; R = Me, R′ = Ph, 10; R = H, R′ = iPr, 11; R = Me, R′ = iPr, 12; R = H, R′ = Cy, 13; R = Me, R′ = Cy, 14). By using Zr(NMe 2) 4 instead of Ti(NMe 2) 4, a zirconium complex, [2-(η 5-Me 3C 5H)C 6H 4NP(iPr) 2− κ 2 N, P]ZrCl 2 ( 15) is prepared. Molecular structures of 10, 14 and [2-(η 5-Me 2C 5H 2)C 6H 4NPPh 2− κN]Ti(NMe 2) 2 ( 16) were determined. The metric parameters determined on the X-ray crystallographic studies and the chemical shifts of the 31P NMR signal indicate that the phosphorous atom coordinates to the titanium in the dichloro-complexes 9– 15. The titanium and zirconium complexes show negligible activity in ethylene and ethylene/1-hexene (co)polymerization when activated with MAO or iBu 3Al/[Ph 3C][B(C 6F 5) 4].
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