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. 2022 Feb 3;78(Pt 3):264-269. doi: 10.1107/S2056989022001037. eCollection 2022 Feb 1.
The reaction of Co(NCS) with urotropine in ethanol leads to the formation of two different compounds, namely, bis-(ethanol-κ)bis-(hexa-methyl-ene-tetra-mine-κ)bis-(thio-cyanato-κ)cobalt(II)-di-aqua-κ -bis-(hexa-methyl-ene-tetra-mine-κ)bis-(thio-cyanato-κ)cobalt(II)-ethanol-hexa-methyl-ene-tetra-mine (1.2/0.8/1.6/4), [Co(NCS)(CHN)(CHO)]·[Co(NCS)(CHN)(HO)]·1.6CHO·4CHN, , and tris-(ethanol-κ)(hexa-methyl-ene-tetra-mine-κ)bis(thio-cyanato-κ)cobalt(II), [Co(NCS)(CHN)(CHO)], . In the crystal structure of compound , two crystallographically independent discrete complexes are observed that are located on centres of inversion. In one of them, the Co cation is octa-hedrally coordinated to two terminal N-bonded thio-cyanate anions, two urotropine ligands and two ethanol mol-ecules, whereas in the second complex 80% of the coordinating ethanol is exchanged by water. Formally, compound is a mixture of two different complexes, di-aqua-dithio-cyanato-bis-(urotropine)cobalt(II) and di-ethano-ldi-thio-cyanato-bis-(uro-trop-ine)cobalt(II), that contain additional ethanol and urotropine solvate mol-ecules leading to an overall composition of [Co(NCS)(urotropine)(ethanol)(HO)·0.8ethanol·4urotropine. Both discrete complexes are linked by inter-molecular O-H⋯O and O-H⋯N hydrogen bonding and additional urotropine solvate mol-ecules into chains, which are further connected into layers. These layers combine into a three-dimensional network by pairs of centrosymmetric inter-molecular C-H⋯S hydrogen bonds. In the crystal structure of compound , di-thio-cyanato-(urotropine)tri-ethano-lcobalt(II), the cobalt cation is octa-hedrally coordinated to two terminal N-bonded thio-cyanate anions, one urotropine ligand and three ethanol mol-ecules into discrete complexes, which are located in general positions. These complexes are linked by inter-molecular O-H⋯N hydrogen bonding into layers, which are further connected into a three-dimensional network by inter-molecular C-H⋯S hydrogen bonding.
Co(NCS)与乌洛托品在乙醇中反应生成两种不同的化合物，即双-(乙醇-κ)双-(六亚甲基四胺-κ)双-(硫氰酸根-κ)钴(II)-二水-κ -双-(六亚甲基四胺-κ)双-(硫氰酸根-κ)钴(II)-乙醇-六亚甲基四胺(1.2/0.8/1.6/4)，[Co(NCS)(CHN)(CHO)]·[Co(NCS)(CHN)(HO)]·1.6CHO·4CHN， ，以及三-(乙醇-κ)(六亚甲基四胺-κ)双(硫氰酸根-κ)钴(II)，[Co(NCS)(CHN)(CHO)]， 。在化合物 的晶体结构中，观察到两个晶体学独立的离散配合物位于对称中心上。其中一个中，Co阳离子八面体配位两个末端N键合硫氰酸根阴离子、两个乌洛托品配体和两个乙醇分子，而在第二个配合物中，80%配位的乙醇被水取代。形式上，化合物 是两种不同配合物的混合物，二水二硫氰酸根双-(乌洛托品)钴(II)和二乙醇二硫氰酸根双-(乌洛托品)钴(II)，它们含有额外的乙醇和乌洛托品溶剂化分子，导致总体组成为[Co(NCS)(乌洛托品)(乙醇)(HO)·0.8乙醇·4乌洛托品。两个离散配合物通过分子间O-H⋯O和O-H⋯N氢键以及额外的乌洛托品溶剂化分子连接成链，这些链进一步连接成层。这些层通过成对的中心对称分子间C-H⋯S氢键组合成三维网络。在化合物 二硫氰酸根-(乌洛托品)三乙醇钴(II)的晶体结构中，钴阳离子八面体配位两个末端N键合硫氰酸根阴离子、一个乌洛托品配体和三个乙醇分子形成离散配合物，它们位于一般位置。这些配合物通过分子间O-H⋯N氢键连接成层，这些层通过分子间C-H⋯S氢键进一步连接成三维网络。
