Metal ions are ubiquitous in biology and aid in facilitate many enzymatic transformations. For instance, high–valent iron–oxido and –hydroxido species are proposed to be key intermediates in oxidative processes catalyzed by non-heme iron proteins. A subclass of these proteins contains bimetallic sites that house either FeFe or FeM cores. To investigate the properties of both mono- and bimetallic cores, we have developed a symmetric tripodal ligand framework containing phosphinic amide groups, which can stabilize high–valent metal centers, as well as provide an auxiliary binding-site for a second metal ion. This presentation will describe our efforts to access high-valent homo-/hetero-bimetallic oxido and –hydroxido species by a variety of synthetic routes. Details of the structural and spectroscopic properties will be discussed that were obtained by X-ray diffraction methods, electrochemical techniques, and electronic absorbance, electronic paramagnetic resonance, Mössbauer, and vibrational spectroscopies.