Tj. Boyle et al., TITANIUM(IV) NEOPENTOXIDES - X-RAY STRUCTURES OF TI-3(MU(3)-CL)(MU-OCH2CME3)(3)(OCH2CME3)(6) AND [TI(MU-OCH2CME3)(OCH2CME3)(3)](2), Inorganic chemistry, 36(15), 1997, pp. 3293-3300
Attempts to synthesize titanium(IV) neopentoxide led to two unique pro
ducts which were crystallographically characterized. A metathesis reac
tion between TiCl4 and NaOCH2CMe3 (NaONp) yielded Ti-3(O)(Cl)(ONp)(9)
. C7H8, 1, which adopts a standard M-3(mu(3)-X)(2)(mu-X)(3)X-6 structu
re. The mu(3) ligands are a Cl and an O atom, with the lest 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(OPri
)(4) and HONp. 2 adopts a typical M-2(mu-X)(2)(X)(6) fused axial-equat
orial edge-shared geometry, wherein each metal center is 5 coordinated
. On the basis of molecular weight solution studies and H-1, C-13, O-1
7 (natural abundance), and Ti-47,Ti-49 solution and solid-state NMR in
vestigations, 2 was determined to be a monomer in solution.