Journal of Physical Chemistry, Vol.100, No.9, 3387-3394, 1996
A Practical Strategy for Determination of Proton Hyperfine Interaction Parameters in Paramagnetic Transition-Metal Ion Complexes by 2-Dimensional Hyscore Electron-Spin-Resonance Spectroscopy in Disordered-Systems
A practical strategy is outlined for the determination of proton hyperfine parameters in paramagnetic transition metal ion complexes in disordered systems from a single two-dimensional hyperfine sublevel correlation spectroscopy (2D HYSCORE) electron spin resonance experiment. Both dipolar and isotropic hyperfine interaction parameters can directly be determined from the cross peak ridges in the HYSCORE spectrum in the limit of the point dipole approximation. This approach is justified by spectral simulations for isotropic and axially symmetric g tensors. If the HYSCORE spectrum is measured at the gl spectral region of the electron spin resonance powder spectrum, the orientation of the hyperfine interaction tensor with respect to the g tensor frame can also be deduced from the shape of the cross peak ridges in many cases. Two experimental examples are presented. Using this approach, the hyperfine interaction parameters for protons in [CU(H2O)(6)](2+) and in [CU(C5H5N)(4)](2+) complexes, both incorporated into mesoporous (L)Cu-MCM-41 silica tube material, are determined from a single 2D HYSCORE spectrum; The parameters are in good agreement with independent measurements by electron spin echo modulation spectroscopy.
Keywords:ECHO ENVELOPE MODULATION