Synthesis of 1-Methyl-3-aryl-substituted Titanocene and Zirconocene Dichlorides and Crystal Structure of Bis[η5-1-methyl-3-(α, α-dimethylbenzyl) cyclopentadienyl] titanium Dichloride

✍ Scribed by Yan-Long Qian; Xin-Rong Qin; Ji-Ling Huang; Albert Sun-Chi Chan; Shou-Shan Chen; Hong-Gen Wang

• Publisher: John Wiley and Sons
• Year: 2010
• Tongue: English
• Weight: 292 KB
• Volume: 19
• Category: Article
• ISSN: 0256-7660
• DOI: 10.1002/cjoc.20010190117

✦ Synopsis

Abstract

The syntheses of a series of l‐methyl‐3‐aryl‐substituted titanocene and zirconocene dichlorides are reported. These complexes are synthesized by the reaction of 2‐ and 3‐methyl‐6, 6‐dimethylfulvenes (1:4) with aryllithium, followed by the reaction with TiCl~4~·2THF, ZrCl~4~ and (CpTiCl~2~)~2~O respectively, to give complexes 1–5. The complex [η^5^‐1‐methyl‐3‐(α, α‐dimethylbenzyl) cyclopentadienyl] titanium dichloride has been studied by X‐ray diffraction. The red crystal of this complex is monoclinic, space group __P__2~t/C~ with unit cell parameters: a =6.973(6) × 10^−1^ nm, b =36.91(2) × 10^−1^ nm, c = 10.063(4) × 10^−1^ nm, α=β= γ = 93.35(5)°, V = 2584(5) × 10^−3^ nm^3^ and Z = 4. Refinement for 1004 observed reflections gives the final R of 0.088. There are four independent molecules per unit cell.