Synthesis and characterization of new alkoxotitanates of yttrium, barium and copper: Single crystal X-ray diffraction structures of Cl{sub 2}Y(Ti{sub 2}(OPr{sup i}){sub 9}), (Ti(OPr{sup i}){sub 5})Ba(Ti{sub 2}(OPr{sup i}){sub 9}), and ClCu(Ti{sub 2}(OPr{sup i}){sub 9})
- Univ. of Saarland, Saarbruecken (Germany)
The synthesis and characterization of new mixed-metal alkoxides of titanium with yttrium, barium, and copper, achieved via salt elimination and acid-base reactions, is described. The metathesis reactions of KTi{sub 2}(OPr{sup i}){sub 9} with anhydrous YCl{sub 3} (1:1 and 2:1) and CuCl{sub 2} (1:1) afford chloro-functionalized heterobimetallic alkoxides Cl{sub 2}Y(Ti{sub 2}(OPr{sup i}){sub 9}) (1), ClY(Ti{sub 2}(OPr{sup i}){sub 9}){sub 2} (2), and ClCu(Ti{sub 2}(OPr{sup i}){sub 9}) (3), respectively, in high yields. The barium - titanium derivatives [Ba(Ti{sub 2}(OPr{sup i}){sub 10})]{sub 2} (4), (Ti{sub 2}(OPr{sup i}){sub 9})Ba(Ti(OPr{sup i}){sub 5}) (5), and Ba(Ti{sub 2}(OPr{sup i}){sub 9}){sub 2} (6) result from the reaction between [Ba(OPr{sup i}){sub 2}]{sub n} and Ti(OPr{sup i}){sub 4} in 1:2, 1:3, and 1:4 molar ratios, respectively. All the new derivatives (1-6) have been characterized by elemental analyses, variable-temperature {sup 1}H and {sup 13}C NMR, infrared spectroscopy, cryoscopy, and single crystal X-ray diffraction studies for 1, 3, and 5. The crystallographic study of 1 reveals a mononuclear species where the yttrium atom, coordinated by four alkoxide oxygen atoms of the (Ti{sub 2}(OPr{sup i}){sub 9}){sup -} unit and two chloride ligands, is in a pseudo-octahedral arrangement. The NMR ({sup 1}H and {sup 13}C) and cryoscopic data for 1 indicate that the bioctahedral (Ti{sub 2}(OPr{sup i}){sub 9}) framework, as observed in the solid state structure, is retained in solution also. The X-ray structure of copper derivative 3 exhibits a triangular heterometallic core CuTi{sub 2}({mu}{sub 2}-OPr{sup i}){sub 3}({mu}{sub 3}-OPr{sup i}){sub 2} with chloride as a terminal ligand on copper. 46 refs., 3 figs., 4 tabs.
- OSTI ID:
- 563869
- Journal Information:
- Inorganic Chemistry, Vol. 36, Issue 11; Other Information: PBD: 21 May 1997
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
36 MATERIALS SCIENCE
ALKOXIDES
LIGANDS
SYNTHESIS
CRYSTAL STRUCTURE
MOLECULAR STRUCTURE
STRUCTURAL CHEMICAL ANALYSIS
NMR SPECTRA
SUPERCONDUCTIVITY
SOLUBILITY
BARIUM
COPPER
TITANIUM
YTTRIUM
REDOX REACTIONS
CHEMICAL REACTION YIELD
TERNARY ALLOY SYSTEMS
CHEMICAL BONDS
BOND ANGLE
BOND LENGTHS
CRYOSCOPY
X-RAY DIFFRACTION
NMR SPECTROMETERS
INFRARED SPECTROMETERS
CHELATING AGENTS