NMR study of the [VO(O2)2F]2- ion in solution: Synthesis, vibrational spectra and crystal structure of [NH3CH2CH2NH3][VO(O2)2F]
| Authors | |
|---|---|
| Year of publication | 2005 |
| Type | Article in Periodical |
| Magazine / Source | Journal of Fluorine Chemistry |
| MU Faculty or unit | |
| Citation | |
| Field | Inorganic chemistry |
| Keywords | Peroxovanadium complexes; X-ray structure determination; NMR spectrocopy |
| Description | The presence of the [VO(O2)2F]2- ion in an aqueous solution gives rise to a doublet (delta = -714 ppm, JVF = 163+/-3 Hz) in the 51V NMR, and a multiplet (delta = -160 ppm, Delta nu 1/2 = 1163 Hz) in the 19F NMR spectrum. The formation of this species is enhanced in formamide solutions. The ethane-1,2-diammonium(2+) fluorooxodiperoxovanadate, [NH3CH2CH2NH3][VO(O2)2F], was prepared from aqueous solution and characterized by elemental analysis, and IR and Raman spectroscopies. The complex crystallizes in the orthorhombic space group Pbca with eight formula units in a cell of dimensions: a = 9.2690(4), b = 8.8321(5) and c = 16.7605(8) A. The complex anion has a rare pentagonal pyramidal structure with a very weak intermolecular interaction d(V...O) = 2.8730(12) A between the vanadium atom and the double-bonded oxygen atom from the adjacent anion. |
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