8 research outputs found
Synthetic studies and structural aspects of novel metallacyclic compoundsof titanium(IV) incorporating nitrogen, oxygen and sulphur: 1. Reactions of cis-dialkoxy-bis(acetylacetonato)titanium(IV) with alkoxyalkanols and the crystal structure of a new modification: di-μ-oxo-bis[diacetylacetonatotitanium(IV)]
Reactions of cis-dialkoxy-bis(acetylacetonato)titanium(IV), [(acac)2Ti(OR)2] (R = Et, Pr i ) with alkoxyalkanols (ROCH2CH2OH) (R = Me, Et, n-Bu) in 1:1 and 1:2 molar ratios in refluxing benzene under anhydrous conditions yield [(acac)2Ti(OR)2-n (OCH2CH2OR) n ] (n = 1 or 2) complexes, which were purified by distillation under reduced pressure. On the basis of i.r. and n.m.r. (1H- and 13C-) spectral studies, a cis-octahedral environment around TiIV is proposed. On keeping the distilled dark brown-red viscous liquid [(acac)2Ti(OEt)(OCH2CH2OBu)] for 2 weeks, orange yellow crystals of [(acac)2TiO]2 were obtained. A single crystal X-ray diffraction study suggests the product is a new modification of [(acac)2TiO]2
Fluorescent aluminum chelate complexes as modified precursors for nano-structured alumina
<p>A series of new mononuclear heteroleptic derivatives of aluminum(III), {[(CH<sub>3</sub>COCHCOCH<sub>3</sub>)AlL] (<b>1</b> and <b>4</b>)}, {[(C<sub>6</sub>H<sub>5</sub>COCHCOC<sub>6</sub>H<sub>5</sub>)AlL] (<b>2</b>, <b>5</b>, and <b>7</b>)}, and {[(C<sub>9</sub>H<sub>6</sub>NO)AlL] (<b>3</b> and <b>6</b>)}, have been synthesized by reacting Al(OPr<sup><i>i</i></sup>)<sub>3</sub> with tridentate Schiff base H<sub>2</sub>L<sup>x</sup> (H<sub>2</sub>L<sup>1</sup> = C<sub>13</sub>H<sub>10</sub>BrNO<sub>2</sub>; H<sub>2</sub>L<sup>2</sup> = C<sub>14</sub>H<sub>13</sub>NO<sub>3</sub>; H<sub>2</sub>L<sup>3</sup> = C<sub>17</sub>H<sub>13</sub>NO<sub>2</sub>) and β-diketone/8-hydroxyquinoline (β-diketone = acetylacetone/dibenzoylmethane) in 1 : 1 : 1 stoichiometry using anhydrous benzene and ethanol. All the complexes were characterized by elemental analysis, FTIR, and NMR (<sup>1</sup>H and <sup>13</sup>C) spectral studies. Molecular structures obtained from single-crystal XRD of aqua <b>1</b> (<b>1a</b>) and DMSO coordinated <b>2</b> (<b>2a</b>) authenticate their existence. Further, nanostructured α-alumina was synthesized from <b>1</b> by well-established sol–gel method and was characterized by powder XRD, TEM, and EDX analyses.</p
Synthesis, structural, and ε-caprolactone polymerization studies of heteroleptic derivatives of aluminum(III)
<div><p>A series of metallo-organic complexes of Al(III), [(CH<sub>3</sub>COCHCOCH<sub>3</sub>)<sub>2</sub>Al(OR)]<sub>2</sub> [where R = <i>o</i>-MeC<sub>6</sub>H<sub>4</sub> (<b>1</b>), <i>m</i>-MeC<sub>6</sub>H<sub>4</sub> (<b>2</b>), <i>p</i>-MeC<sub>6</sub>H<sub>4</sub> (<b>3</b>), C<sub>6</sub>H<sub>5</sub>CH<sub>2</sub> (<b>4</b>), <i>o</i>-ClC<sub>6</sub>H<sub>4</sub>CH<sub>2</sub> (<b>5</b>), <i>m</i>-ClC<sub>6</sub>H<sub>4</sub>CH<sub>2</sub> (<b>6</b>), and <i>p</i>-ClC<sub>6</sub>H<sub>4</sub>CH<sub>2</sub> (<b>7</b>), were synthesized quantitatively by treating Al(OPr<sup>i</sup>)<sub>3</sub> with CH<sub>3</sub>COCH<sub>2</sub>COCH<sub>3</sub> and the phenols (<i>o</i>-MeC<sub>6</sub>H<sub>4</sub>OH, <i>m</i>-MeC<sub>6</sub>H<sub>4</sub>OH, and <i>p</i>-MeC<sub>6</sub>H<sub>4</sub>OH) concerned as well as phenylmethanols (C<sub>6</sub>H<sub>5</sub>CH<sub>2</sub>OH, <i>o</i>-ClC<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>OH, <i>m</i>-ClC<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>OH, and <i>p</i>-ClC<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>OH) in suitable stoichiometry using benzene as solvent. All these complexes were soluble in common organic solvents, having sharp melting points, and they were characterized by elemental analysis, IR, and NMR (<sup>1</sup>H and <sup>13</sup>C) spectral studies. Single-crystal XRD followed by ORTEP diagram of solvated complex (<b>1a</b>) revealed its dimeric nature and the existence of six-coordinate aluminum. The complexes were studied in ring-opening polymerization of ε-caprolactone. The molecular weight and polydispersity index values of polycaprolactone were obtained by gel permeation chromatography analysis.</p></div