Krebs Christoph, Jess Inke, Näther Christian
Institute of Inorganic Chemistry, University of Kiel, Max-Eyth-Str. 2, 24118 Kiel, Germany.
Acta Crystallogr E Crystallogr Commun. 2023 Jan 1;79(Pt 1):14-18. doi: 10.1107/S2056989022011380.
Single crystals of the title compound, [Co(NCS)(CHBrN)(CHN)], were obtained by the reaction of Co(NCS) with 3-bromo-pyridine in aceto-nitrile. The Co cations lie on crystallographic inversion centers and are coordinated by two N-bonded thio-cyanate anions, two 3-bromo-pyridine and two aceto-nitrile ligands thereby forming slightly distorted CoN octa-hedra. In the crystal, these complexes are linked by C-H⋯S and C-H⋯N hydrogen bonds into a three-dimensional network. In the direction of the crystallographic -axis, the complexes are arranged into columns with neighboring 3-bromo-pyridine ligands stacked onto each other, indicating π-π inter-actions. The CN stretching vibration of the thio-cyanate anions is observed at 2066 cm, in agreement with the presence of only N-bonded anionic ligands. TG-DTA measurements reveal that in the first mass loss the aceto-nitrile ligands are removed and that in the second step, half of a 3-bromo-pyridine ligand is lost, leading to the formation of a polymeric compound with the composition [(Co(NCS))(CHBrN)] already reported in the literature.
通过将Co(NCS)与3-溴吡啶在乙腈中反应，得到了标题化合物[Co(NCS)(CHBrN)(CHN)]的单晶。Co阳离子位于晶体学反演中心，由两个N键合的硫氰酸根阴离子、两个3-溴吡啶和两个乙腈配体配位，从而形成略微扭曲的CoN八面体。在晶体中，这些配合物通过C-H⋯S和C-H⋯N氢键连接成三维网络。在晶体学c轴方向上，配合物排列成柱状，相邻的3-溴吡啶配体相互堆叠，表明存在π-π相互作用。硫氰酸根阴离子的CN伸缩振动在2066 cm处观察到，这与仅存在N键合的阴离子配体一致。热重-差示热分析测量表明，在第一次质量损失中，乙腈配体被除去，在第二步中，一半的3-溴吡啶配体损失，导致形成一种文献中已报道的组成为[(Co(NCS))(CHBrN)]的聚合化合物。
