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μ-四硫代锑酸三[(环胺)锌(II)]四硫代锑酸盐乙腈二溶剂合物二水合物的晶体结构,显示锌在环胺环平面上的无序状态(环胺=1,4,8,11-四氮杂环十四烷)

Crystal structure of μ-tetra-thio-anti-monato-tris[(cyclam)zinc(II)] tetra-thio-anti-monate aceto-nitrile disolvate dihydrate showing Zn disorder over the cyclam ring planes (cyclam = 1,4,8,11-tetra-aza-cyclo-tetra-deca-ne).

作者信息

Näther Christian, Danker Felix, Bensch Wolfgang

机构信息

Institut für Anorganische Chemie, Universität Kiel, Max-Eyth. Str. 2, 241128 Kiel, Germany.

出版信息

Acta Crystallogr E Crystallogr Commun. 2022 Apr 12;78(Pt 5):490-495. doi: 10.1107/S2056989022003759. eCollection 2022 May 1.

DOI:10.1107/S2056989022003759
PMID:35547801
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9069514/
Abstract

Reaction of Zn(ClO)·6HO with cyclam (cyclam = 1,4,8,11-tetra-aza-cyclo-tetra-decane, CHN) and NaSbS in an aceto-nitrile/water mixture led to the formation of crystals of the title compound, Zn(SbS)(CHN)·2CHCN·2HO or (Zn-cyclam)(SbS)(aceto-nitrile). The set-up of the crystal structure is similar to that of [(Zn-cyclam)(SbS)]8HO reported recently [Danker (2021 ▸). . , 18107-18117]. The crystal structure of the title compound consists of three crystallographically independent Zn cations (each disordered around centers of inversion), three centrosymmetric cyclam ligands, one SbS anion, one water and one aceto-nitrile mol-ecule occupying general positions. The aceto-nitrile mol-ecule is equally disordered over two sets of sites. Each Zn cation is bound to four nitro-gen atoms of a cyclam ligand and one sulfur atom of the SbS anion within a distorted square-pyramidal coordination. The cation disorder of the [Zn(cyclam)] complexes is discussed in detail and is also observed in other compounds, where identical ligands are located above and below the [Zn(cyclam)] plane. In the title compound, the building units are arranged in layers parallel to the plane forming pores in which the aceto-nitrile solvate mol-ecules are located. Inter-molecular C-H⋯S hydrogen bonding links these units to the SbS anions. Between the layers, additional water solvate mol-ecules are present that act as acceptor and donor groups for inter-molecular N-H⋯O and O-H⋯S hydrogen bonding.

摘要

Zn(ClO)·6HO与环胺(环胺=1,4,8,11-四氮杂环十四烷,CHN)和NaSbS在乙腈/水混合溶剂中反应,生成了标题化合物Zn(SbS)(CHN)·2CHCN·2HO或(Zn-环胺)(SbS)(乙腈)的晶体。其晶体结构的构建与最近报道的[(Zn-环胺)(SbS)]8HO相似[丹克(2021▸)……,18107 - 18117]。标题化合物的晶体结构由三个晶体学独立的Zn阳离子(每个在反演中心周围无序)、三个中心对称的环胺配体、一个SbS阴离子、一个水分子和一个占据一般位置的乙腈分子组成。乙腈分子在两组位置上同样无序。每个Zn阳离子在扭曲的四方锥配位中与一个环胺配体的四个氮原子和SbS阴离子的一个硫原子相连。详细讨论了[Zn(环胺)]配合物的阳离子无序现象,并且在其他化合物中也观察到相同的配体位于[Zn(环胺)]平面的上方和下方。在标题化合物中,结构单元平行于平面排列成层,形成了乙腈溶剂化分子所在的孔。分子间C-H⋯S氢键将这些单元与SbS阴离子相连。在层与层之间,存在额外的水溶剂化分子,它们作为分子间N-H⋯O和O-H⋯S氢键的受体和供体基团。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/eb5691f3788e/e-78-00490-fig5.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/46fdca14960e/e-78-00490-fig1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/a0be186b416a/e-78-00490-fig2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/facc37d9dcbf/e-78-00490-fig3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/172dd0e881f7/e-78-00490-fig4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/eb5691f3788e/e-78-00490-fig5.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/46fdca14960e/e-78-00490-fig1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/a0be186b416a/e-78-00490-fig2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/facc37d9dcbf/e-78-00490-fig3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/172dd0e881f7/e-78-00490-fig4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/be40/9069514/eb5691f3788e/e-78-00490-fig5.jpg

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