Titanium(IV) Neopentoxides. X-ray Structures of Ti3(μ3-O)(μ3-Cl)(μ-OCH2CMe3)3(OCH2CMe3)6and [Ti(μ-OCH2CMe3)(OCH2CMe3)3]2
Timothy J. BoyleTodd M. AlamEric R. MechenbierBrian L. ScottJoseph W. Ziller
Abstract
Attempts to synthesize titanium(IV) neopentoxide led to two unique products which were crystallographically characterized. A metathesis reaction between TiCl(4) and NaOCH(2)CMe(3) (NaONp) yielded Ti(3)(O)(Cl)(ONp)(9).C(7)H(8), 1, which adopts a standard M(3)(&mgr;(3)-X)(2)(&mgr;-X)(3)X(6) structure. The &mgr;(3) ligands are a Cl and an O atom, with the rest of ligands represented by bridging and terminal ONp ligands. [Ti(ONp)(4)](2), 2, was isolated in high yield by an alcoholysis exchange between Ti(OPr(i))(4) and HONp. 2 adopts a typical M(2)(&mgr;-X)(2)(X)(6) fused axial-equatorial edge-shared geometry, wherein each metal center is 5 coordinated. On the basis of molecular weight solution studies and (1)H, (13)C, (17)O (natural abundance), and (47,49)Ti solution and solid-state NMR investigations, 2 was determined to be a monomer in solution.
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