Syntheses and structural characterization of 2,2′-methylene-bis(6-t-butyl-4-methyl-phenoxide) complexes of titanium, zirconium and tantalum

Malcolm H. Chisholm, Jui Hsien Huang, John C. Huffman, William E. Streib, Darin Tiedtke

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Abstract

The reactions of M(NMe2)n (M = Ti, Zr, n = 4; Ta, n = 5) with 2,2′-methylene-bis(6-t-butyl-4-methylphenol), HO - CH2 - OH, in toluene produce Ti(O - CH2 - O)2 (1), Zr22-O - CH2 - O)2(μ,η1-O - CH2 - O)2 (2) and Ta(O - CH2 - O)(NMe2)3 (3). Compounds 1 and 2 can also be obtained via metathesis of MCl4 with Li2(O - CH2 - O). Reducing (O - CH2 - O)TiCl2 with 2 equiv. of Na/Hg also generates 1 by ligand redistribution. Reaction of Zr(NMe2)4 with 1 equiv. of HO - CH2 - OH yields (O - CH2 - O)Zr(NMe2)2 (4). Metathesis of TaCl5 with 1 equiv. of Li2(O - CH2 - O) produces (O - CH2 - O)TaCl3 (5). (O - CH2 - O)Ta(NMe2)2Cl (6) is formed from the reaction of 3 with 1 equiv. of trimethylsilylchloride in toluene. The dimethylamide groups of compounds 3 and 4 reveal dynamic behavior on the NMR time-scale. The compounds 1, 2 and 3 have been characterized by single-crystal X-ray crystallography.

Original languageEnglish
Pages (from-to)2941-2949
Number of pages9
JournalPolyhedron
Volume16
Issue number17
DOIs
Publication statusPublished - 1997 Jan 1

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All Science Journal Classification (ASJC) codes

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

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