Abstract

The structure of a transition metal complex may, in favourable cases, be determined by combining the information obtained from d–d spectroscopy, which indicates the nature of the ligand field, and metal (K)-edge EXAFS, from which the metal–ligand distances may be obtained; the approach is illustrated for tetragonally distorted, pseudo-octahedral NiIV complexes: [NiCl2{o-C6H4(PMe2)2}2]2+(Ni–Cl = 2.26, Ni–P = 2.22 Å), [NiCl2{o-C6H4(AsMe2)2}2]2+(Ni–Cl = 2.27, Ni–As = 2.36 Å).

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