By employing boronato instead of carboxylato bridges in the dication [Mn 2IV(μ‐O)‐(μ‐PhBO2)2L2]2+ (L = 1,4,7‐trimethyl‐1,4,7‐triazacyclononane), a Mn 2IV unit has been stabilized for the first time. Together with the di‐μ‐carboxylato‐μ‐oxodimanganese complexes of analogous structure, there is now an “isostructural series” available containing Mn 2II, MnIIMnIII, Mn 2III, MnIIIMnIV, Mn 2IV units. The Mn K‐edge energy of the corresponding complexes increases linearly with increasing oxidation level. This is of importance for EXAFS investigations of metalloproteins containing manganese.

A program package for XAFS data analysis, especially of liquid and amorphous samples, has been developed. For the first time a consequent error propagation is presented for all functions to be calculated in the course of the data analysis. The structural investigation of the Grignard compound CH3MgBr in diethyl ether is taken as an example for the various steps of the data analysis.

Structural investigations using EXAFS spectroscopy and standard analytical methods were performed on electrochemically synthesized tetrabutylammonium bromide stabilized Pd/Pt bimetallic clusters with different Pd/Pt ratios. The results of these investigations allow the determination of a detailed model concerning the structure of these 3.5 nm sized bimetallic clusters. The cores of the clusters are enriched in platinum metal, while the outer shell is enriched in palladium metal. The nanostructured particles are partially oxidized. The amounts of oxide in the outer shells are larger than in the cores of the clusters. Also, a small amount of the metal is present as metal bromide. The ammonium salt stabilizer forms a protective layer around the cluster.

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