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PubMed2002

Planar three-coordinate high-spin Fe(II) complexes with large orbital angular momentum: Mössbauer, electron paramagnetic resonance, and electronic structure studies.

Mössbauer spectra of [LFe(II)X](0) (L = beta-diketiminate; X = Cl(-), CH(3)(-), NHTol(-), NHtBu(-)), 1.X, were recorded between 4.2 and 200 K in applied magnetic fields up to 8.0 T. A spin Hamiltonian analysis of these data revealed a spin S = 2 system with uniaxial magnetization properties, arising from a quasi-degenerate M(S) = +/-2 doublet that is separated from the next magnetic sublevels by very large zero-field splittings (3/D/ > 150 cm(-1)). The ground levels give rise to positive magnetic hyperfine fields of unprecedented magnitudes, B(int) = +82, +78, +72, and +62 T for 1.CH(3), 1.NHTol, 1.NHtBu, and 1.Cl, respectively. Parallel-mode EPR measurements at X-band gave effective g values that are considerably larger than the spin-only value 8, namely g(eff) = 10.9 (1.Cl) and 11.4 (1.CH(3)), suggesting the presence of unquenched orbital angular momenta. A qualitative crystal field analysis of g(eff) shows that these momenta originate from spin-orbit coupling between energetically closely spaced yz and z(2) 3d-orbital states at iron and that the spin of the M(S) = +/-2 doublet is quantized along x, where x is along the Fe-X vector and z is normal to the molecular plane. A quantitative analysis of g(eff) provides the magnitude of the crystal field splitting of the lowest two orbitals, /epsilon(yz) - epsilon(2)(z)/ = 452 (1.Cl) and 135 cm(-1) (1.CH(3)). A determination of the sign of the crystal field splitting was attempted by analyzing the electric field gradient (EFG) at the (57)Fe nuclei, taking into account explicitly the influence of spin-orbit coupling on the valence term and ligand contributions. This analysis, however, led to ambiguous results for the sign of epsilon(yz) - epsilon(2)(z). The ambiguity was resolved by analyzing the splitting Delta of the M(S) = +/-2 doublet; Delta = 0.3 cm(-1) for 1.Cl and Delta = 0.03 cm(-)(1) for 1.CH(3). This approach showed that z(2) is the ground state in both complexes and that epsilon(yz) - epsilon(2)(z) approximately 3500 cm(-1) for 1.Cl and 6000 cm(-1) for 1.CH(3). The crystal field states and energies were compared with the results obtained from time-dependent density functional theory (TD-DFT). The isomer shifts and electric field gradients in 1.X exhibit a remarkably strong dependence on ligand X. The ligand contributions to the EFG, denoted W, were expressed by assigning ligand-specific parameters: W(X) to ligands X and W(N) to the diketiminate nitrogens. The additivity and transferability hypotheses underlying this model were confirmed by DFT calculations. The analysis of the EFG data for 1.X yields the ordering W(N(diketiminate)) < W(Cl) < W(N'HR), W(CH(3)) and indicates that the diketiminate nitrogens perturb the iron wave function to a considerably lesser extent than the monodentate nitrogen donors do. Finally, our study of these synthetic model complexes suggests an explanation for the unusual values for the electric hyperfine parameters of the iron sites in the Fe-Mo cofactor of nitrogenase in the M(N) state.

Electron Spin Resonance Spectroscopy↗
PubMed2003

Increased electron donor and electron acceptor characters enhance the adhesion between oil droplets and cells of Yarrowia lipolytica as evaluated by a new cytometric assay.

The adhesion of methyl ricinoleate droplets to cells of the yeast Yarrowia lipolytica was investigated. A new cytometric method, relying on the double staining of fatty globules with Nile Red and of cells with Calcofluor, enabled us to quantify methyl ricinoleate droplet adhesion to cells precultured on a hydrophilic or on a hydrophobic carbon source. In this last case, droplet adsorption was enhanced and a MATS (microbial adhesion to solvents) test revealed that this increase was due to Lewis acid-base interactions and not to an increase in the hydrophobic properties of the cell surface. These preliminary results demonstrate that the developed cytometric method is promising for various applications concerning the study of interactions between microorganisms and an emulsified hydrophobic substrates.

Adhesiveness↗