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Molecular nitrides with titanium and rare-earth metals
Jorge Caballo1, María García-Castro, Avelino Martín
1Departamento de Química Inorgánica, Universidad de Alcalá, 28871 Alcalá de Henares-Madrid, Spain.
Inorganic Chemistry
|June 18, 2011
Summary
New titanium-group 3/lanthanide metal complexes were synthesized. These include cube-type adducts and double-cube nitrido compounds, with structures confirmed by X-ray crystallography and thermal decomposition studies.
Area of Science:
- Organometallic Chemistry
- Inorganic Chemistry
- Materials Science
Background:
- Titanium-group 3 and lanthanide metals are crucial in various catalytic and materials applications.
- The synthesis of novel multinuclear complexes offers opportunities for exploring unique reactivity and properties.
- Understanding the structural diversity and thermal stability of these complexes is key to their potential applications.
Purpose of the Study:
- To synthesize and characterize novel titanium-group 3/lanthanide metal complexes.
- To investigate the structural features of these complexes using X-ray crystallography.
- To evaluate the thermal decomposition behavior of the synthesized nitrido compounds.
Main Methods:
- Reaction of a titanium-containing precursor [{Ti(η(5)-C(5)Me(5))(μ-NH)}(3)(μ(3)-N)] (1) with various rare-earth metal derivatives (halides, triflates, amides).
- Isolation and characterization of cube-type adducts and double-cube nitrido compounds.
- X-ray crystallography for structural determination of selected complexes.
- Thermogravimetric analysis (TGA), differential thermal analysis (DTA), and pyrolysis experiments for thermal decomposition studies.
Main Results:
- Successful synthesis of cube-type adducts [X(3)M{(μ(3)-NH)(3)Ti(3)(η(5)-C(5)Me(5))(3)(μ(3)-N)}] and aryloxido complexes [(ArO)(3)M{(μ(3)-NH)(3)Ti(3)(η(5)-C(5)Me(5))(3)(μ(3)-N)}].
- Formation of corner-shared double-cube nitrido compounds [M(μ(3)-N)(3)(μ(3)-NH)(3){Ti(3)(η(5)-C(5)Me(5))(3)(μ(3)-N)}(2)] via NH(SiMe(3))(2) elimination.
- A single-cube intermediate [{(Me(3)Si)(2)N}Sc{(μ(3)-N)(2)(μ(3)-NH)Ti(3)(η(5)-C(5)Me(5))(3)(μ(3)-N)}] was isolated.
- X-ray crystal structures of six complexes were determined, elucidating their unique architectures.
- Thermal decomposition studies revealed insights into the stability and potential decomposition pathways of the nitrido complexes.
Conclusions:
- The synthetic strategy allows for the controlled assembly of complex titanium-group 3/lanthanide multinuclear structures.
- The characterized complexes exhibit diverse structural motifs, including cube-type and double-cube arrangements.
- The thermal stability investigations provide valuable data for potential applications in materials synthesis or catalysis.
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