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Synthesis and characterization of some oxovanadium(V) complexes with internally functionalized oximes: Crystal and molecular structures of heptacoordinated [VO{ONC(CH3)(C4H3O-2)}3] and [VO{ONC(CH3)(C4H3S-2)}3] · 0.5C6H6 |
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| Authors: | Vineet Sharma Rakesh Bohra John E Drake Mark E Light |
| Institution: | a Department of Chemistry, University of Rajasthan, Jaipur 302 004, Rajasthan, India b Department of Chemistry and Biochemistry, University of Windsor, Windsor, Ont., Canada N9B 3P4 c Department of Chemistry, University of Southampton, Highfield, Southampton, SO17 1BJ, UK |
| Abstract: | New oxovanadium(V) complexes with internally functionalized oximes of the type VO{OPri}3−n{ON C(CH3)(Ar)}n] (where Ar = C4H3O-2, C4H3S-2 and C5H4N-2 and n = 1-3) have been prepared in quantitative yields by the reaction of VO(OPri)3 with the corresponding oximes in various stoichiometric ratios in refluxing anhydrous benzene. The products have been characterized by elemental analyses and spectroscopic (FT IR, 1H, 13C{1H} and 51V NMR) studies. FAB mass spectral analysis of VO{OPri}{ONC(CH3)C4H3S}2] indicates the monomeric nature of the complex. 51V NMR values for these complexes suggest the formation of tetra-coordinate species in solution. However, the single crystal X-ray diffraction studies of VO{ONC(CH3)(C4H3O-2)}3] and VO{ONC(CH3)(C4H3S-2)}3] · 0.5C6H6 exhibit the presence of vanadium(V) atoms in a unique hepta-coordination state with distorted pentagonal bipyramidal geometry in the solid state. The oxo- atom occupies the axial position while the oximato ligands are bonded in a dihapto (η2-N,O) manner with the formation of three membered rings. |
| Keywords: | Oxovanadium(V) complexes Internally functionalized oximes 51V NMR Hepta-coordination Dihapto bonding |
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