Jochim Aleksej, Radulovic Rastko, Jess Inke, Näther Christian
Institut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Str. 2, D-24118 Kiel, Germany.
Acta Crystallogr E Crystallogr Commun. 2020 Nov 17;76(Pt 12):1841-1845. doi: 10.1107/S2056989020015121. eCollection 2020 Dec 1.
In the course of our investigations regarding transition-metal thio-cyanates with thio-urea derivatives, the title compound, [Ni(NCS)(CHNS)], was obtained. The asymmetric unit consists of one thio-cyanate anion and one tetra-methyl-thio-urea mol-ecule on general positions, as well as one Ni cation that is located on a twofold rotational axis. In this compound, discrete complexes are formed in which the Ni cations are surrounded by two -N-bonding thio-cyanate anions as well as two -S-bonding tetra-methyl-thio-urea mol-ecules within a distorted square-planar coordination geometry. The discrete complexes are linked by pairs of weak C-H⋯S hydrogen bonds between the thio-cyanate S and one of the tetra-methyl-thio-urea methyl hydrogen atoms into chains along the crystallographic - and -axis directions, which are combined into layers parallel to the plane. X-ray powder diffraction proves that a pure crystalline phase was obtained and measurements using thermogravimetry and differential thermoanalysis reveal that the compound decomposes at about 408 K, where all tetra-methyl-thio-urea mol-ecules are lost.
在我们对过渡金属硫氰酸盐与硫脲衍生物的研究过程中，得到了标题化合物[Ni(NCS)(CHNS)]。不对称单元由一个处于一般位置的硫氰酸根阴离子和一个四甲基硫脲分子，以及一个位于二重旋转轴上的Ni阳离子组成。在该化合物中，形成了离散的配合物，其中Ni阳离子在扭曲的平面正方形配位几何结构中被两个通过-N键合的硫氰酸根阴离子以及两个通过-S键合的四甲基硫脲分子所包围。离散的配合物通过硫氰酸根S与四甲基硫脲甲基氢原子之一之间的成对弱C-H⋯S氢键沿晶体学a轴和b轴方向连接成链，这些链组合成平行于ab平面的层。X射线粉末衍射证明获得了纯晶相，热重分析和差示热分析测量表明该化合物在约408 K分解，此时所有四甲基硫脲分子均失去。
