Rusanova Julia A, Semenaka Valentyna V, Omelchenko Irina V
Department of Chemistry, Taras Shevchenko National University of Kyiv, 64/13, Volodymyrska Street, Kyiv 01601, Ukraine.
SSI "Institute for Single Crystals", National Academy of Sciences of Ukraine, 60 Lenina ave., Kharkiv 61072, Ukraine.
Acta Crystallogr E Crystallogr Commun. 2016 Mar 11;72(Pt 4):489-91. doi: 10.1107/S2056989016003996. eCollection 2016 Apr 1.
The tetra-nuclear complex cation of the title compound, Cr2Pb2(NCS)2(OH)2(C4H10NO)42·CH3CN, lies on an inversion centre. The main structural feature of the cation is a distorted seco-norcubane Pb2Cr2O6 cage with a central four-membered Cr2O2 ring. The Cr(III) ion is coordinated in a distorted octa-hedron, which involves two N atoms of one bidentate ligand and one thio-cyanate anion, two μ2-O atoms of 2-(di-methyl-amino)-ethano-late ligands and two μ3-O atoms of hydroxide ions. The coordination geometry of the Pb(II) ion is a distorted disphenoid, which involves one N atom, two μ2-O atoms and one μ3-O atom. In addition, weak Pb⋯S inter-actions involving the coordinating and non-coordinating thio-cyanate anions are observed. In the crystal, the complex cations are linked through the thio-cyanate anions via the Pb⋯S inter-actions and O-H⋯N hydrogen bonds into chains along the c axis. The chains are further linked together via S⋯S contacts. The contribution of the disordered solvent aceto-nitrile mol-ecule was removed with the SQUEEZE [Spek (2015 ▸). Acta Cryst. C71, 9-18] procedure in PLATON. The solvent is included in the reported mol-ecular formula, weight and density.
标题化合物Cr₂Pb₂(NCS)₂(OH)₂(C₄H₁₀NO)₄₂·CH₃CN的四核络合阳离子位于一个对称中心上。阳离子的主要结构特征是一个扭曲的类降冰片烷Pb₂Cr₂O₆笼，带有一个中心四元Cr₂O₂环。Cr(III)离子以扭曲的八面体配位，涉及一个双齿配体的两个N原子和一个硫氰酸根阴离子、2-(二甲基氨基)乙醇酸酯配体的两个μ₂-O原子以及氢氧根离子的两个μ₃-O原子。Pb(II)离子的配位几何形状是一个扭曲的双楔体，涉及一个N原子、两个μ₂-O原子和一个μ₃-O原子。此外，还观察到涉及配位和非配位硫氰酸根阴离子的弱Pb⋯S相互作用。在晶体中，络合阳离子通过硫氰酸根阴离子经由Pb⋯S相互作用和O-H⋯N氢键沿c轴连接成链。这些链通过S⋯S接触进一步连接在一起。在PLATON中使用SQUEEZE [Spek (2015 ▸). Acta Cryst. C71, 9 - 18]程序去除了无序溶剂乙腈分子的贡献。溶剂包含在报道的分子式、分子量和密度中。
