Christian Näther , Henning Lühmann , Wolfgang Bensch
{"title":"高氯酸μ-四硫-抗单-双-[（环唑）锌（II）]的合成、晶体结构和性质","authors":"Christian Näther , Henning Lühmann , Wolfgang Bensch","doi":"10.1107/S2056989024009356","DOIUrl":null,"url":null,"abstract":"<div><div>In the title compound, the [SbS<sub>4</sub>]<sup>3–</sup> anions bridge two Zn(cyclam)<sup>2+</sup> cations into [Zn<sub>2</sub>(cyclam)<sub>2</sub>SbS<sub>4</sub>]<sup>+</sup> 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.</div></div><div><div>The reaction of Zn(ClO<sub>4</sub>)<sub>2</sub>·6H<sub>2</sub>O with Na<sub>3</sub>SbS<sub>4</sub>·9H<sub>2</sub>O in a water/acetonitrile mixture leads to the formation of the title compound, (μ-tetrathioantimonato-κ<sup>2</sup><em>S</em>:<em>S</em>′)bis[(1,4,8,11-tetraazacyclotetradecane-κ<sup>4</sup><em>N</em>)zinc(II)] perchlorate 0.8-hydrate, [Zn<sub>2</sub>(SbS<sub>4</sub>)(C<sub>10</sub>H<sub>24</sub>N<sub>4</sub>)<sub>2</sub>]ClO<sub>4</sub>·0.8H<sub>2</sub>O or [(Zn-cyclam)<sub>2</sub>(SbS<sub>4</sub>)]<sup>+</sup>[ClO<sub>4</sub>]<sup>−</sup>·0.8H<sub>2</sub>O. The asymmetric unit consists of two crystallographically independent [SbS<sub>4</sub>]<sup>3–</sup> anions, two independent perchlorate anions and two independent water molecules as well as four crystallographically independent Zn(cyclam)<sup>2+</sup> 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)<sup>2+</sup> cations are linked <em>via</em> the [SbS<sub>4</sub>]<sup>3–</sup> anions into [Zn<sub>2</sub>(cyclam)<sub>2</sub>SbS<sub>4</sub>]<sup>+</sup> cations that are charged-balanced by the [ClO<sub>4</sub>]<sup>−</sup> anions. The water molecules of crystallization are hydrogen bonded to the [SbS<sub>4</sub>]<sup>3–</sup> 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.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 11","pages":"Pages 1151-1156"},"PeriodicalIF":0.5000,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11660490/pdf/","citationCount":"0","resultStr":"{\"title\":\"Synthesis, crystal structure and properties of μ-tetrathioantimonato-bis[(cyclam)zinc(II)] perchlorate 0.8-hydrate\",\"authors\":\"Christian Näther , Henning Lühmann , Wolfgang Bensch\",\"doi\":\"10.1107/S2056989024009356\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>In the title compound, the [SbS<sub>4</sub>]<sup>3–</sup> anions bridge two Zn(cyclam)<sup>2+</sup> cations into [Zn<sub>2</sub>(cyclam)<sub>2</sub>SbS<sub>4</sub>]<sup>+</sup> 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.</div></div><div><div>The reaction of Zn(ClO<sub>4</sub>)<sub>2</sub>·6H<sub>2</sub>O with Na<sub>3</sub>SbS<sub>4</sub>·9H<sub>2</sub>O in a water/acetonitrile mixture leads to the formation of the title compound, (μ-tetrathioantimonato-κ<sup>2</sup><em>S</em>:<em>S</em>′)bis[(1,4,8,11-tetraazacyclotetradecane-κ<sup>4</sup><em>N</em>)zinc(II)] perchlorate 0.8-hydrate, [Zn<sub>2</sub>(SbS<sub>4</sub>)(C<sub>10</sub>H<sub>24</sub>N<sub>4</sub>)<sub>2</sub>]ClO<sub>4</sub>·0.8H<sub>2</sub>O or [(Zn-cyclam)<sub>2</sub>(SbS<sub>4</sub>)]<sup>+</sup>[ClO<sub>4</sub>]<sup>−</sup>·0.8H<sub>2</sub>O. The asymmetric unit consists of two crystallographically independent [SbS<sub>4</sub>]<sup>3–</sup> anions, two independent perchlorate anions and two independent water molecules as well as four crystallographically independent Zn(cyclam)<sup>2+</sup> 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)<sup>2+</sup> cations are linked <em>via</em> the [SbS<sub>4</sub>]<sup>3–</sup> anions into [Zn<sub>2</sub>(cyclam)<sub>2</sub>SbS<sub>4</sub>]<sup>+</sup> cations that are charged-balanced by the [ClO<sub>4</sub>]<sup>−</sup> anions. The water molecules of crystallization are hydrogen bonded to the [SbS<sub>4</sub>]<sup>3–</sup> 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.</div></div>\",\"PeriodicalId\":7367,\"journal\":{\"name\":\"Acta Crystallographica Section E: Crystallographic Communications\",\"volume\":\"80 11\",\"pages\":\"Pages 1151-1156\"},\"PeriodicalIF\":0.5000,\"publicationDate\":\"2024-10-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11660490/pdf/\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Acta Crystallographica Section E: Crystallographic Communications\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://www.sciencedirect.com/org/science/article/pii/S2056989024002561\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"CRYSTALLOGRAPHY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Acta Crystallographica Section E: Crystallographic Communications","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/org/science/article/pii/S2056989024002561","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CRYSTALLOGRAPHY","Score":null,"Total":0}
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.
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.
京公网安备 11010802042870号
京ICP备2023020795号-1
分享
求助内容：
应助结果提醒方式：
扫码关注我们
