Titanium(IV) Neopentoxides. X-ray Structures of Ti(3)(&mgr;(3)-O)(&mgr;(3)-Cl)(&mgr;-OCH(2)CMe(3))(3)(OCH(2)CMe(3))(6) and [Ti(&mgr;-OCH(2)CMe(3))(OCH(2)CMe(3))(3)](2).
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.
Boyle
Timothy J.
TJ
Department of Chemistry, X-ray Diffraction Laboratory, University of California-Irvine, Irvine, California 92717.
Alam
Todd M.
TM
Mechenbier
Eric R.
ER
Scott
Brian L.
BL
Ziller
Joseph W.
JW