Iron valence-to-core Fe Kβ X-ray emission spectroscopy (V2C XES) is established as a means to identify light atoms (C, N, O) within complex multimetallic frameworks. The ability to distinguish light atoms, particularly in the presence of heavier atoms, is a well-known limitation of both crystallography and EXAFS. Using the sensitivity of V2C XES to the ionization potential of the bound ligand, energetic shifts of ~10 eV in the ligand 2s ionization energies of bound C, N, and O may be observed. As V2C XES is a high-energy X-ray method, it is readily applicable to samples in any physical form. This method thus has great potential for application to multimetallic inorganic frameworks involved in both small molecule storage and activation.
© 2011 American Chemical Society