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高氯酸μ-四硫代锑酸根双[（环胺）锌（II）]0.8水合物的合成、晶体结构及性质

Synthesis, crystal structure and properties of μ-tetra-thio-anti-monato-bis-[(cyclam)zinc(II)] perchlorate 0.8-hydrate.

作者信息

Näther Christian, Lühmann Henning, Bensch Wolfgang

机构信息

Institut für Anorganische Chemie, Universität Kiel, Max-Eyth.-Str. 2, D-24118 Kiel, Germany.

出版信息

Acta Crystallogr E Crystallogr Commun. 2024 Oct 11;80(Pt 11):1151-1156. doi: 10.1107/S2056989024009356. eCollection 2024 Oct 1.

DOI:10.1107/S2056989024009356
PMID:39712171
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC11660490/
Abstract

The reaction of Zn(ClO)·6HO with NaSbS·9HO in a water/aceto-nitrile mixture leads to the formation of the title compound, (μ-tetra-thio-anti-monato-κ :')bis-[(1,4,8,11-tetra-aza-cyclo-tetra-decane-κ )zinc(II)] perchlorate 0.8-hydrate, [Zn(SbS)(CHN)]ClO·0.8HO or [(Zn-cyclam)(SbS)][ClO]·0.8HO. The asymmetric unit consists of two crystallographically independent [SbS] anions, two independent perchlorate anions and two independent water mol-ecules as well as four crystallographically independent Zn(cyclam) cations that are located in general positions. Both perchlorate anions and one cyclam ligand are disordered and were refined with a split mode using restraints. The water mol-ecules are partially occupied. Two Zn(cyclam) cations are linked the [SbS] anions into [Zn(cyclam)SbS] cations that are charged-balanced by the [ClO] anions. The water mol-ecules of crystallization are hydrogen bonded to the [SbS] anions. The cations, anions and water mol-ecules are linked by N-H⋯O, N-H⋯S and O-H⋯S hydrogen bonds into a three-dimensional network. Powder X-ray diffraction proves that a pure sample had been obtained that was additionally investigated for its spectroscopic properties.

摘要

在水/乙腈混合溶剂中，Zn(ClO)₂·6H₂O与Na₃SbS₄·9H₂O反应生成标题化合物高氯酸（μ-四硫代锑酸根-κ⁴:S⁴）双[(1,4,8,11-四氮杂环十四烷-κ⁴)锌(II)]0.8水合物，[Zn₂(SbS₄)(C₁₂H₂₈N₄)]ClO₄·0.8H₂O或[(Zn-环胺)(SbS₄)][ClO₄]·0.8H₂O。不对称单元由两个晶体学独立的[SbS₄]阴离子、两个独立的高氯酸根阴离子、两个独立的水分子以及四个处于一般位置的晶体学独立的Zn(环胺)阳离子组成。两个高氯酸根阴离子和一个环胺配体无序，采用约束的分裂模式进行精修。水分子部分占据。两个Zn(环胺)阳离子通过[SbS₄]阴离子连接成[Zn(环胺)SbS₄]阳离子，由[ClO₄]阴离子进行电荷平衡。结晶水分子通过氢键与[SbS₄]阴离子相连。阳离子、阴离子和水分子通过N-H⋯O、N-H⋯S和O-H⋯S氢键连接成三维网络。粉末X射线衍射证明得到了纯样品，并对其光谱性质进行了进一步研究。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/1ab3925846e6/e-80-01151-fig7.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/9023c5dd6063/e-80-01151-fig1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/eed61b7dad97/e-80-01151-fig2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/1191f964cf8e/e-80-01151-fig3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/523a0813106a/e-80-01151-fig4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/f645a2911210/e-80-01151-fig5.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/5eddff0e4c3d/e-80-01151-fig6.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/1ab3925846e6/e-80-01151-fig7.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/9023c5dd6063/e-80-01151-fig1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/eed61b7dad97/e-80-01151-fig2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/1191f964cf8e/e-80-01151-fig3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/523a0813106a/e-80-01151-fig4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/f645a2911210/e-80-01151-fig5.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/5eddff0e4c3d/e-80-01151-fig6.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9e02/11660490/1ab3925846e6/e-80-01151-fig7.jpg

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