高氯酸μ-四硫-抗单-双-[（环唑）锌（II）]的合成、晶体结构和性质

IF 0.5 Q4 CRYSTALLOGRAPHY

Acta Crystallographica Section E: Crystallographic Communications Pub Date : 2024-10-01 DOI:10.1107/S2056989024009356

Christian Näther , Henning Lühmann , Wolfgang Bensch

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引用次数: 0

摘要

在水/乙腈混合物中，Zn(ClO4)2·6H2O与Na3SbS4·9H2O反应生成了（μ-四硫-抗单链-κ2 S:S’）双-[（1,4,8,11-四氮杂环-四癸烷-κ4 N）锌（II）]高氯酸盐0.8水合物，[Zn2(SbS4)(C10H24N4)2]ClO4·0.8H2O或[(Zn-cyclam)2(SbS4)]+[ClO4]- 0.8H2O。不对称单元由两个晶体独立的[SbS4]3-阴离子、两个独立的高氯酸盐阴离子和两个独立的水分子以及四个晶体独立的位于一般位置的Zn(cyclam)2+阳离子组成。高氯酸盐阴离子和环环配体都是无序的，并使用约束以分裂模式进行了精炼。水分子被部分占据。两个Zn(cyclam)2+阳离子通过[SbS4]3-阴离子连接成[Zn2(cyclam)2SbS4]+阳离子，由[ClO4]-阴离子电荷平衡。结晶的水分子与[SbS4]3-阴离子形成氢键。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射线衍射证明获得了纯净的样品，并对其光谱特性进行了进一步的研究。

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Synthesis, crystal structure and properties of μ-tetrathioantimonato-bis[(cyclam)zinc(II)] perchlorate 0.8-hydrate

In the title compound, the [SbS₄]^3– anions bridge two Zn(cyclam)²⁺ cations into [Zn₂(cyclam)₂SbS₄]⁺ cations, which are charged-balanced by perchlorate anions. The components are linked by N—H⋯O, N—H⋯S and O—H⋯S hydrogen bonds into a three-dimensional network.

The reaction of Zn(ClO₄)₂·6H₂O with Na₃SbS₄·9H₂O in a water/acetonitrile mixture leads to the formation of the title compound, (μ-tetrathioantimonato-κ²S:S′)bis[(1,4,8,11-tetraazacyclotetradecane-κ⁴N)zinc(II)] perchlorate 0.8-hydrate, [Zn₂(SbS₄)(C₁₀H₂₄N₄)₂]ClO₄·0.8H₂O or [(Zn-cyclam)₂(SbS₄)]⁺[ClO₄]⁻·0.8H₂O. The asymmetric unit consists of two crystallographically independent [SbS₄]^3– anions, two independent perchlorate anions and two independent water molecules as well as four crystallographically independent Zn(cyclam)²⁺ 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 molecules are partially occupied. Two Zn(cyclam)²⁺ cations are linked via the [SbS₄]^3– anions into [Zn₂(cyclam)₂SbS₄]⁺ cations that are charged-balanced by the [ClO₄]⁻ anions. The water molecules of crystallization are hydrogen bonded to the [SbS₄]^3– anions. The cations, anions and water molecules 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.

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来源期刊

Acta Crystallographica Section E: Crystallographic Communications Chemistry-Chemistry (all)

CiteScore

1.90

自引率

0.00%

发文量

351

审稿时长

3 weeks

期刊介绍： Acta Crystallographica Section E: Crystallographic Communications is the IUCr''s open-access structural communications journal. It provides a fast, simple and easily accessible publication mechanism for crystal structure determinations of inorganic, metal-organic and organic compounds. The electronic submission, validation, refereeing and publication facilities of the journal ensure rapid and high-quality publication of fully validated structures. The primary article category is Research Communications; these are peer-reviewed articles describing one or more structure determinations with appropriate discussion of the science.