618891-15-9Relevant academic research and scientific papers
Synthesis of polymetallic Group 4 complexes bridged by benzenediolate and triolate ligands. X-ray crystal structure of [{Ti(C5 Me5)Cl2}2{μ-1,4-O(2,3-C6 H2Me2)O-}]
Arévalo, Silvia,Bonillo, M. Rufina,de Jesús, Ernesto,de la Mata, F. Javier,Flores, Juan C.,Gómez, Rafael,Gómez-Sal, Pilar,Ortega, Paula
, p. 228 - 236 (2003)
This paper reports the synthesis of polymetallic complexes in which two or three Group 4 metals are linked to a benzene core through oxo groups. Four methods have been evaluated for the synthesis of such derivatives: from the appropriated alcohol with (a) methyl complexes via methane elimination, (b) chloride compounds in the presence of a Lewis base, or (c) a zirconium hydride, and (d) from the lithium salt of the alcohol and chloride complexes. Method a has been used for the synthesis of bimetallic and trimetallic (pentamethylcyclopentadienyl)titanium(IV) complexes [{Ti(C5Me5)Cl2}2 {μ-1,4-O(C6H2XY)O-}] (X=Y=H (1); X = H, Y = Me (2); X=Y=Me (3)), [{Ti(C5Me5)Me2} 2{μ-1,4-O(C6H2Me2)O-}] (4), and [{Ti(C5Me5)X2}3 (μ3-1,3,5-C6H3O3-)] (X = Cl (7), Me (8)) from the corresponding hydroquinones 1,4-HO (2,3-C6H2XY)OH (X = Y = H, Me; X = H, Y = Me) or 1,3,5-trihydroxibenzene and [Ti(C5Me5) Cl2Me] or [Ti(C5Me5)Me3], respectively. Bis(cyclopentadienyl)titanium bimetallic complex [{Ti(C5H5)2Cl}2{μ-1,4-O (C6H2Me2)O-}] (5) is better prepared by method d by treatment of the dilithium salt Li2[1,4-O (2,3-C6H2Me2)O-] with [Ti(C5 H5)2Cl2] whereas the trimetallic compound [{Ti(C5H5)2Cl}3 (μ3-1,3,5-C6H3O3-)] (9) can be prepared directly from 1,3,5-trihidroxybenzene in the presence of NEt3 (method b). Finally, bis(cyclopentadienyl)zirconium complexes [{Zr(C5H5)2Cl}2 {μ-1,4-O(C6H2Me2)O-}] (6) and [{Zr(C5H5)2Cl}3 (μ3-1,3,5-C6H3O3-)] (10) are obtained from [Zr(C5H5)2ClH] (method c). The structure of complex 3 has been determined by X-ray diffraction methods.
