Premium
Synthesis, characterization and soft transformation of some bis(cyclopentadienyl) Ti(IV) and Zr(IV) complexes of Schiff's base ligands to nano‐sized titania or zirconia materials
Author(s) -
Sharma Namita,
Sharma Vinita,
Bohra Rakesh,
Raju V. S.
Publication year - 2007
Publication title -
applied organometallic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.53
H-Index - 71
eISSN - 1099-0739
pISSN - 0268-2605
DOI - 10.1002/aoc.1262
Subject(s) - chemistry , cyclopentadienyl complex , thermogravimetric analysis , denticity , schiff base , thermogravimetry , stoichiometry , nanocrystalline material , thermal stability , tetrahydrofuran , cubic zirconia , benzene , inorganic chemistry , crystallography , nuclear chemistry , crystal structure , solvent , organic chemistry , catalysis , ceramic
Some bis(cyclopentadienyl) complexes of Ti(IV)and Zr(IV) have been synthesized by the metathetical reactions of Cp 2 MCl 2 with the sodium salt of monofunctional bidentate Schiff's base ligands in 1:1 and 1:2 stoichiometry in anhydrous THF. All the derivatives of the types Cp 2 MCl 2− n {O(C 6 H 4 )CH 6 H 5 } n and Cp 2 MCl 2− n {OC(CH 3 )(R) 6 H 5 } n (where R = CH 3 or C 6 H 5 and n = 1 or 2) have been characterized by elemental analyses, molecular weight measurements, FT‐IR and ‐NMR [ 1 H and 13 C{ 1 H}] studies. The FAB mass spectra of a few representative complexes and the molecular weight measurements in freezing benzene indicate their monomeric nature in solution. Spectral studies appear to indicate mono‐ and bi‐dentate mode of attachment of the ligand in solution and in the solid state, respectively. Thermogravimetric analyses (TGA) of Cp 2 TiCl{O(C 6 H 4 )CH} ( 1 ) and Cp 2 ZrCl{O(C 6 H 4 )CH} ( 7 ) indicate their low thermal stability. Transformations of some of these complexes to pure titania (TiO 2 )/zirconia (ZrO 2 ) have been observed at relatively low sintering temperatures. Powder X‐ray diffraction (XRD) and scanning electron micrograph (SEM) studies suggest the nanocrystalline nature of these materials. Copyright © 2007 John Wiley & Sons, Ltd.