Synthesis and characterization carbonyl-tungsten(0)complexes [n,n'-bis(ferrocenylmethylene) ethylenediamine]

Download

index.pdf

Date

2005

Author

Kavaklı, Cüneyt

Metadata

Show full item record

Item Usage Stats

147
views

59
downloads

In this study a bidentate ligand containing two ferrocenyl moieties, N,N'-bis(ferrocenylmethylene)ethylenediamine, was prepared by condensation reaction of ferrocenecarboxyaldehyde and ethylenediamine on refluxing in benzene. The molecule was identified by IR, Raman, UV-VIS, 1H-, 13C-NMR spectroscopies. Then, this bidentate ligand was reacted with pentacarbonylbis-(trimethyl)silylethyne)tungsten(0). The ligand substitution reaction in dichloromethane yielded the new complex, tetracarbonyl [N,N'-bis(ferrocenylmethylene)ethylenediamine]tungsten(0) (W(CO)4(BFEDA)). This new complex was isolated from the reaction solution in the form of orange crystals and fully characterized by elemental analysis, IR, UV-VIS, MS, 1H- and 13C-NMR spectroscopies. As a bidentate ligand, [N,N'-bis(ferrocenylmethylene)ethylenediamine] binds the metal atom in the two cis positions in the pseudooctahedral geometry of the tungsten-complex. Electrochemistry of the tetracarbonyl [N,N'-bis(ferrocenylmethylene)ethylenediamine]tungsten(0) was studied by cyclic voltammetry, and controlled potential electrolysis combined with the UV-VIS spectroscopy. One irreversible oxidation and three reversible oxidations were observed in the cyclic voltammogram. One of these reversible and the irreversible oxidations are attributed to tungsten and the other two reversible oxidations to iron centers. It is found that the two ferrocene groups started communication with each other after formation of tungsten-complex. N,N'-bis(ferrocenylmethylene)ethylenediamine was also reacted with photogenerated pentacarbonyl(tetrahydrofuran)tungsten(0) complex and the pentacarbonyl [N,N'-bis(ferrocenylmethylene)ethylenediamine]tungsten(0) (W(CO)5(BFEDA)) as an intermediate on the route to the tetracarbonyl[N,N'-bis(ferrocenylmethylene)ethylenediamine]tungsten(0) was isolated from the reaction medium in the form of red crystals and

Subject Keywords

Organometallic chemistry and compounds.

URI

http://etd.lib.metu.edu.tr/upload/12606101/index.pdf
https://hdl.handle.net/11511/15111

Collections

Graduate School of Natural and Applied Sciences, Thesis

Suggestions

OpenMETU
Core

Synthesis and characterization tetracarbonyl[n,n'-bis(ferrocenylmethylene ethylenediamine] molybdenum(0) complex Koçak, Fatma Sanem; Özkar, Saim; Department of Chemistry (2005) In this study a bidentate ligand containing two ferrocenyl moieties, N,N'-bis(ferrocenylmethylene)ethylenediamine, was prepared by condensation reaction of ferrocenecarboxyaldehyde and ethylenediamine on refluxing in benzene. The molecule was identified by IR, Raman, UV-Vis, 1H-, 13C-NMR spectroscopies. Then, this bidentate molecule was reacted with tetracarbonyl(bicyclo[2.1.1] hepta-2,5-diene)molybdenum(0). The ligand substitution reaction in toluene yielded the new complex, tetracarbonyl[N,Ń-bis(ferrocen...
Synthesis and characterization of tetracarbonyl(6-ferrocenyl-2.2'-bibyridine)tungsten(0) complex Edinç, Pelin; Özkar, Saim; Department of Chemistry (2005) In this study, a bidentate ligand, 6-ferrocenyl-2,2'-bipyridine, was prepared by the reaction of lithiated ferrocene with bipyridine. The ligand was identified by 1H, 13C- NMR and HMQC and UV-Vis spectroscopies. Then, bidentate molecule was reacted with pentacarbonylbis-(trimethylsilylethyne)tungsten(0). The ligand substitution reaction in CH2Cl2 yielded the new complex, tetracarbonyl(6-ferrocenyl-2,2'bipyridine)tungsten(0). The isolated and purified complex was fully characterized by elemental analysis, IR...
Synthesis and characterization of hyperbranched and air drying fatty acid based resins Bat, Erhan; Kisakurek, D; Akhmedov, IM (Elsevier BV, 2006-04-01) In this research four hyperbranched resins having fatty acid residues were synthesized. Dipentaerythritol, which was used as the core molecule of the resins, was twice esterified with dimethylol propionic acid. This resin was then esterified with the castor oil fatty acids. The hydroxyl group present in the ricinoleic acid which constitutes almost 87% of the castor oil fatty acids was then reacted with linseed oil fatty acids and benzoic acid. The linseed fatty acids were incorporated into the structure to ...
Synthesis of spiro-containing 1,4-oxazepines from N-propargylic beta-enaminones Karadeniz, Eda; Kelgökmen, Yılmaz; Zora, Metin (2018-03-18) An efficient and general method for the synthesis of spiro‐1,4‐oxazepines and 3,3‐dimethyl‐1,4‐oxazepines is reported. When treated with ZnI2 and AgSbF6 in refluxing DCE, cyclohexane‐embedded N‐propargylic β‐enaminones underwent 7‐exo‐dig cyclization to afford spiro‐1,4‐oxazepines, specifically 12‐methylene‐11‐oxa‐7‐azaspiro[5.6]dodeca‐7,9‐dienes, in good to high yields. Accordingly, N‐(1,1‐dimethyl)propargylic β‐enaminones produced 3,3‐dimethyl‐1,4‐oxazepines. Cyclization was found to be general for a dive...
Preparation of Gadolina Stabilized Bismuth Oxide Doped with Boron via Electrospinning Technique TUNÇ, TUNCAY; Uslu, Ibrahim; Durmusoglu, Senol; Keskin, Selda; Aytimur, Arda; Akdemir, Ahmet (Springer Science and Business Media LLC, 2012-01-01) In this study, boron doped and undoped poly (vinyl) alcohol/bismuth-gadolina acetate (PVA/Bi-Gd) nanofibers were prepared using electrospinning technique then calcinated at 800 degrees C for 2 h. The originality of this study is the addition of boron to metal acetates. The effects of boron doping were investigated in terms of solution properties, morphological changes and thermal characteristics. The characteristics of the fibers were investigated with FT-IR, XRD, SEM and BET. The addition of boron did not ...

Citation Formats

C. Kavaklı, “Synthesis and characterization carbonyl-tungsten(0)complexes [n,n’-bis(ferrocenylmethylene) ethylenediamine],” M.S. - Master of Science, Middle East Technical University, 2005.