Reactions of oximes and diethylhydroxylamine with titanium alkoxides

Singh, Ashita; Sharma, C. K.; K., A.; Gupta, Vandana; Mehrotra, R. C.

doi:10.1039/j19710002440

Cited by 24 publications

(7 citation statements)

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“…[7] Our results were different. Even when one molar equivalent of cyclopentanone oxime, acetoxime, or ethyl methyl ketoxime was treated with Ti(OiPr) 4 in dichloromethane solution, only the di-substituted derivatives [Ti(OiPr) 2 (ON= CRЈRЈЈ) 2 ] 2 (i.e., x = 2) crystallized from the reaction solution [Equation (2)].…”

Section: Resultscontrasting

confidence: 70%

“…Both the mono-and the di-substituted derivatives are alkoxo-bridged dimers (Figure 1), as found for Ti 2 (OiPr) 4 (pyridine-2-aldoximate) 4 (see above), contrary to monomeric compounds postulated from molecular weight measurements. [7] The structures can formally be derived from dimeric [Ti(OiPr) 4 ] 2 , [11] with one or two OiPr groups replaced by side-on coordinated oximate ligands. Figure 3 and Figure 4 show the molecular structures for 2 and 6, as examples for both isomers.…”

Section: Resultsmentioning

confidence: 99%

“…Several Ti(OR) 4-x -(ON=CRЈ 2 ) x or Ti(OR) 4-x (ON=CRЈRЈЈ) x (x = 1-4) derivatives were reported in the early literature, [7] but structural evidence was not provided. The reaction of Ti(OBu) 4 with acetoxime was recently repeated.…”

Section: M(or) X + Y Bl-h ǟ M(or)mentioning

confidence: 98%

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Ketoximate Derivatives of Titanium Alkoxides and Partial Hydrolysis Products Thereof

et al. 2009

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Crystalline oximate derivatives of titanium alkoxides [Ti(OR)2(ON=CR′R″)2]2 were obtained when Ti(OR)4 (R = iPr, Et) was treated with various oximes (cyclopentanone oxime, cyclohexanone oxime, acetoxime, ethyl methyl ketoxime or 2,4‐pentandione dioxime). Formation of bis‐substituted derivatives was favored in each case, and only one mono‐substituted derivative, [Ti(OiPr)3(ON=C6H10)]2, was isolated. Two isomers were observed for [Ti(OR)2(ON=CR′R″)2]2, differing by the mutual orientation of the oximate ligands. The NO groups of the oximate ligands are side‐on coordinated to one titanium atom in each case. Three partially hydrolyzed derivatives, viz. Ti6O6(OiPr)6(ON=CR2)6 (CR2 = CMe2 or C5H8) and Ti4O2(OiPr)8(ON=CMe–CH2–CMe=NO)2 were also structurally characterized. In these derivatives the NO groups bridge two titanium atoms.(© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009)

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Section: Resultscontrasting

confidence: 70%

Section: Resultsmentioning

confidence: 99%

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Ketoximate Derivatives of Titanium Alkoxides and Partial Hydrolysis Products Thereof

et al. 2009

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“…The hydrolysis is generally accelerated by the presence of high amounts of water which yields amorphous precipitates consisting of big aggregated particles with less defined sizes and shapes which can be converted into the metal oxides by a subsequent thermal treatment. Several strategies, involving the formation of thermodynamically stable complexes via the chemical modification of the alkoxide precursors with different compounds, such as amines, 29 alkoxy-and aminoalcohols, 30 oximes, 31 β-diketones, 30b,32 β-ketoesters 33 or carboxylic and phosphonic acids 34 have been proposed.…”

Section: Formation Of the Perovskite Colloidal Nanocrystalsmentioning

confidence: 99%

Solvothermal synthesis and controlled self-assembly of monodisperse titanium-based perovskite colloidal nanocrystals

et al. 2015

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The rational design of monodisperse ferroelectric nanocrystals with controlled size and shape and their organization into hierarchical structures has been a critical step for understanding the polar ordering in nanoscale ferroelectrics, as well as the design of nanocrystal-based functional materials which harness the properties of individual nanoparticles and the collective interactions between them. We report here on the synthesis and self-assembly of aggregate-free, single-crystalline titanium-based perovskite nanoparticles with controlled morphology and surface composition by using a simple, easily scalable and highly versatile colloidal route. Single-crystalline, non-aggregated BaTiO3 colloidal nanocrystals, used as a model system, have been prepared under solvothermal conditions at temperatures as low as 180 °C. The shape of the nanocrystals was tuned from spheroidal to cubic upon changing the polarity of the solvent, whereas their size was varied from 16 to 30 nm for spheres and 5 to 78 nm for cubes by changing the concentration of the precursors and the reaction time, respectively. The hydrophobic, oleic acid-passivated nanoparticles exhibit very good solubility in non-polar solvents and can be rendered dispersible in polar solvents by a simple process involving the oxidative cleavage of the double bond upon treating the nanopowders with the Lemieux-von Rudloff reagent. Lattice dynamic analysis indicated that regardless of their size, BaTiO3 nanocrystals present local disorder within the perovskite unit cell, associated with the existence of polar ordering. We also demonstrate for the first time that, in addition to being used for fabricating large area, crack-free, highly uniform films, BaTiO3 nanocubes can serve as building blocks for the design of 2D and 3D mesoscale structures, such as superlattices and superparticles. Interestingly, the type of superlattice structure (simple cubic or face centered cubic) appears to be determined by the type of solvent in which the nanocrystals were dispersed. This approach provides an excellent platform for the synthesis of other titanium-based perovskite colloidal nanocrystals with controlled chemical composition, surface structure and morphology and for their assembly into complex architectures, therefore opening the door for the design of novel mesoscale functional materials/nanocomposites with potential applications in energy conversion, data storage and the biomedical field.

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“…Both are ambidentate with the possibility of coordination (after deprotonation) through oxygen alone or through both nitrogen and oxygen. Although several derivatives Ti(OR) 42x L x (L = O-NLCR 2 or O-NR 2 ) were reported in the literature, 43 no structural information is available. Reaction of Ti(O i Pr) 2 (ONLCMe 2 ) 2 with acetylacetone (acac-H) gives Ti(O i Pr)(acac)(ONLCMe 2 ) 2 or Ti(acac) 2 (ONLCMe 2 ) 2 and shows that the oximate ligands are more strongly bonded than the OR groups.…”

Section: Reactions Of Titanium Alkoxides With Other No Ligandsmentioning

confidence: 99%