| Summary: | In our attempts to prepare coordination polymers by reaction of FeCl<sub>3</sub>·6H<sub>2</sub>O and Ni(OH)<sub>2</sub> in the presence of dithiolenes HSC<sub>6</sub>H<sub>2</sub>X<sub>2</sub>SH (X = Cl or H), several ion pairs of compounds containing the anionic entity [Ni(SC<sub>6</sub>H<sub>2</sub>X<sub>2</sub>S)<sub>2</sub>]<sup>−</sup> were obtained instead. It was also found that other species without dithiolene ligands were formed in these reactions, giving rise to different ion pairs and a tetrametallic cluster. The careful isolation of the different types of crystalline solids allowed the characterization of all of the resulting compounds by single crystal X-ray diffraction (SCXRD). In order to establish the amount of nickel and iron present in the crystals, complementary total reflection X-ray fluorescence (TXRF) analyses were performed. The eight different structural types that were obtained are described and compared with related ones found in the literature.
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