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In our attempts to prepare coordination polymers by reaction of FeCl 3 ·6H 2 O and Ni(OH) 2 in the presence of dithiolenes HSC 6 H 2 X 2 SH (X = Cl or H), several ion pairs of compounds containing the anionic entity [Ni(SC 6 H 2 X 2 S) 2 ] - 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.

Structural Study of the Compounds Formed in the Reactions of FeCl3·6H2O with Ni(OH)2 in the Presence of Dithiolenes HSRSH (R = C6H2Cl2 or C6H4)