Abstract
The ESR spectra of a selection of molybdenum(V) and tungsten(V) compounds have been examined as a function of microwave frequency. In particular, reduced line widths at lower (S band: 2-4 GHz) microwave frequencies allow detection of 14N, 1H, 17O, 77Se, and 35,37Cl superhyperfine interactions in certain of the following complexes: [Mo(abt)3]- (abtH2 = o-aminobenzenethiol), [MO(XPh)4]- (M = Mo, W; X = S, Se), and cis-[MoO(qtl)2X] (X = Cl, Br; qtlH = quinoline-8-thiol). The redistribution of spectral information as a function of frequency, together with computer simulation, has allowed the determination of the hyperfine matrix and its relative orientation to the g matrix, in most cases. A dz2-based ground state is assigned to [Mo(abt)3]- in contrast to dxy-based ground states for the oxo-molybdenum(V) complexes. Axially symmetric sites are present in [MO(XPh)4]- and monoclinic (Cs) sites in trans-[MoOL(DMF)]+ (L = salen, salophen). The results provide strong motivation for a wider examination of transition metal species at lower microwave frequencies. © 1987 American Chemical Society.
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