Departamento de Química Inorgánica, Universidad Autónoma de Madrid, 28049 Madrid, Spain.
SCXRD Laboratory, SIdI, Universidad Autónoma de Madrid, 28049 Madrid, Spain.
Molecules. 2020 May 10;25(9):2240. doi: 10.3390/molecules25092240.
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.
在试图通过 FeCl·6HO 和 Ni(OH) 在二硫烯 HSCHXSH（X = Cl 或 H）存在下反应来制备配位聚合物时，我们得到了几个含有阴离子实体[Ni(SCHXS)]的化合物的离子对。我们还发现，这些反应中还形成了没有二硫烯配体的其他物种，导致形成了不同的离子对和四金属簇。对不同类型的结晶固体进行仔细分离，允许通过单晶 X 射线衍射（SCXRD）对所有生成的化合物进行表征。为了确定晶体中镍和铁的含量，进行了补充的全反射 X 射线荧光（TXRF）分析。描述了获得的八个不同结构类型，并与文献中发现的相关类型进行了比较。
