Structural Study of the Compounds Formed in the Reactions of FeCl(3)·6H(2)O with Ni(OH)(2) in the Presence of Dithiolenes HSRSH (R = C(6)H(2)Cl(2) or C(6)H(4))

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.