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Synthesis and crystal structure of a salicylatooxovanadium(V) complex of an aminebis(phenolate) ligand: Kinetic studies on its formation from corresponding alkoxo complexes
Authors:Dipankar Maity  W.S. Sheldrick  Bilwadal Bandyopadhyay
Affiliation:a Department of Chemistry, Jadavpur University, Kolkata 700 032, West Bengal, India
b Ruhr-Universitat Bochum, Lehrstuhl fur Analytischie Chemie, D-44 780 Bochum, Germany
c ECMP Division, NMR Laboratory, Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata 700 064, India
Abstract:Synthesis and single crystal X-ray structures of H2L1 and VO(L1)(HL) [H2L1 = N,N-bis(2-hydroxy-3,5-ditertiarybutyl)-N′,N′-dimethylethylendiamine) or simply aminebis(phenol) and H2L = salicylic acid) are reported here. The complex [VO(L1)(HL)] is in distorted octahedral geometry under O4N2 donor environment where the basal core is defined by O(1), O(3), O(2) and N(5) atoms and two axial coordinates are occupied by O(4), an alkoxo-group and N(1), an imino-nitrogen atom. The electron spray mass spectrometric study on [VO(L1)(HL)] in MeCN clearly points out the existence of single species in solution. Again, the 51V NMR of the bulk polycrystalline sample reveals that the complex [VO(L1)(HL)] mainly exists in three out of four possible isomers. The formation of [VO(L1)(HL)] from both [VO(L1)(OMe)] and [VO(L1)(OEt)] was followed kinetically by reacting with salicylic acid in MeCN. The presence of isosbestic point indicates a clean conversion of the reactants to product.
Keywords:Oxovanadium(V) complexes   Aminebis(phenolate) ligand   Distorted octahedral geometry   Solid state 51V NMR   Kinetics
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