Structural Study of the Compounds Formed in the Reactions of FeCl·6HO with Ni(OH) in the Presence of Dithiolenes HSRSH (R = CHCl or CH).

In our attempts to prepare coordination polymers by reaction of FeCl·6HO and Ni(OH) in the presence of dithiolenes HSCHXSH (X = Cl or H), several ion pairs of compounds containing the anionic entity [Ni(SCHXS)] 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.