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Abstract From a comparison of the known molecular stoichiometry and x-ray photoemission spectroscopy, it is evident that the Fe(III) spin crossover salt [Fe(qsal)₂Ni(dmit)₂] has a preferential surface termination with the Ni(dmit)₂moiety, where qsal = N(8quinolyl)salicylaldimine, and dmit²⁻= 1,3-dithiol-2-thione-4,5-dithiolato. This preferential surface termination leads to a significant surface to bulk core level shift for the Ni 2p x-ray photoemission core level, not seen in the corresponding Fe 2p core level spectra. A similar surface to bulk core level shift is seen in Pd 3d in the related [Fe(qsal)₂]₂Pd(dmit)₂. Inverse photoemission spectroscopy, compared with the x-ray absorption spectra at the Ni-L3,2 edge provides some indication of the density of states resulting from the dmit²⁻= 1,3-dithiol-2-thione-4,5-dithiolato ligand unoccupied molecular orbitals and thus supports the evidence regarding surface termination in the Ni(dmit)₂moiety.