Synthesis and Characterization of donor-functionalized ansa-Cyclopentadienyl-Indenyl and ansa-Indenyl-Indenyl Complexes of Yttrium, Samarium, Thulium, and Lutetium

✍ Scribed by Herbert Schumann; Frank Erbstein; Dirk F. Karasiak; Igor L. Fedushkin; Jörg Demtschuk; Frank Girgsdies

• Book ID: 101305098
• Publisher: John Wiley and Sons
• Year: 1999
• Tongue: German
• Weight: 222 KB
• Volume: 625
• Category: Article
• ISSN: 0372-7874
• DOI: 10.1002/(sici)1521-3749(199905)625:5<781::aid-zaac781>3.0.co;2-l

✦ Synopsis

The stepwise reaction of Me 2 SiCl 2 with K[C 5 H 3 t BuMe-3] or Li[C 9 H 7 ] and then with K[C 9 H 6 CH 2 CH 2 -NMe 2 -1] followed by double deprotonation with NaH or LiBu, yields the two dimethylsilicon bridged cyclopentadienyl-indenyl and indenyl-indenyl donor-functionalized ligand systems K 2 ), respectively. Treatment of 1 with YCl 3 (THF) 3 , SmCl 3 (THF) 1.77 , TmI 3 (DME) 3 , and LuCl 3 (THF) 3 gives the mixed ansa-metallocenes [(C 5 H 2 t Bu-3-Me-5)SiMe 2 (1-C 9 H 5 CH 2 CH 2 NMe 2 -3)]LnX (X = Cl, Ln = Y (3), Sm (4), Lu (5); X = I, Ln = Tm ( )), respectively. The reaction of 2 with LuCl 3 (THF) 3 yields [(1-C 9 H 6 )SiMe 2 (1-C 9 H 5 CH 2 CH 2 NMe 2 -3)]LuCl (7). Compound 4 reacts with LiMe to give the corresponding alkyl derivative [(C 5 H 2 t Bu-3-Me-5)SiMe 2 (1-C 9 H 5 CH 2 CH 2 NMe 2 -3)]Sm(CH 3 ) (8). The new complexes were characterized by elemental analyses, MS spectrometry, and NMR spectroscopy. The molecular structures of 5 and 6 were determined by single crystal Xray diffraction.