Benjamin A. Mukda , Diane A. Dickie , Mark M. Turnbull
{"title":"2-氨基-5-碘吡啶盐。","authors":"Benjamin A. Mukda , Diane A. Dickie , Mark M. Turnbull","doi":"10.1107/S2056989024010259","DOIUrl":null,"url":null,"abstract":"<div><div>Compound <strong>1</strong> is the anhydrous form of the known crystal 2-amino-5-iodopyridinium bromide monohydrate and crystallizes in layers inclined ∼40° to the <em>ab</em> face. Hydrogen bonding between the amino and pyridinium ions to the bromide ion acceptor stabilizes the layers. Compound <strong>2</strong> is a salt of 2-amino-5-iodopyridium and a trihalidocobaltate(II) ion with one coordinated 2-amino-5-iodopyridine ligand. The halide ions are mixed Cl/Br with differing occupancies.</div></div><div><div>Reaction of 2-amino-5-iodopyridine (5IAP) with concentrated HBr at room temperature yielded 2-amino-5-iodopyridinium bromide, C<sub>5</sub>H<sub>6</sub>IN<sub>2</sub><sup>+</sup>·Br<sup>−</sup> or (5IAPH)Br. The complex formed pale-yellow crystals, which exhibit significant hydrogen bonding between the amino and pyridinium N—H donors and bromide ion acceptors. Halogen bonding is also observed. Similarly, reaction of 5IAP with cobalt(II) chloride in mixed HCl/HBr in 1-propanol yielded 2-amino-5-iodopyridinium (2-amino-5-iodopyridine-κ<em>N</em><sup>1</sup>)bromido/chlorido(0.51/2.48)cobalt(II), (C<sub>5</sub>H<sub>6</sub>IN<sub>2</sub>)[CoBr<sub>0.51</sub>Cl<sub>2.48</sub>(C<sub>5</sub>H<sub>5</sub>IN<sub>2</sub>)] or (5-IAPH)[(5IAP)CoCl<sub>2.48</sub>Br<sub>0.51</sub>], as blue block-shaped crystals. Two of the three halide positions exhibit mixed occupancy [Cl/Br = 0.797 (5):0.203 (5) and 0.689 (6):0.311 (6)], while the third position is occupied solely by a chloride ion. Extensive hydrogen and halogen bonding is observed.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 11","pages":"Pages 1230-1234"},"PeriodicalIF":0.5000,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11660468/pdf/","citationCount":"0","resultStr":"{\"title\":\"Salts of 2-amino-5-iodopyridinium\",\"authors\":\"Benjamin A. Mukda , Diane A. Dickie , Mark M. Turnbull\",\"doi\":\"10.1107/S2056989024010259\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>Compound <strong>1</strong> is the anhydrous form of the known crystal 2-amino-5-iodopyridinium bromide monohydrate and crystallizes in layers inclined ∼40° to the <em>ab</em> face. Hydrogen bonding between the amino and pyridinium ions to the bromide ion acceptor stabilizes the layers. Compound <strong>2</strong> is a salt of 2-amino-5-iodopyridium and a trihalidocobaltate(II) ion with one coordinated 2-amino-5-iodopyridine ligand. The halide ions are mixed Cl/Br with differing occupancies.</div></div><div><div>Reaction of 2-amino-5-iodopyridine (5IAP) with concentrated HBr at room temperature yielded 2-amino-5-iodopyridinium bromide, C<sub>5</sub>H<sub>6</sub>IN<sub>2</sub><sup>+</sup>·Br<sup>−</sup> or (5IAPH)Br. The complex formed pale-yellow crystals, which exhibit significant hydrogen bonding between the amino and pyridinium N—H donors and bromide ion acceptors. Halogen bonding is also observed. Similarly, reaction of 5IAP with cobalt(II) chloride in mixed HCl/HBr in 1-propanol yielded 2-amino-5-iodopyridinium (2-amino-5-iodopyridine-κ<em>N</em><sup>1</sup>)bromido/chlorido(0.51/2.48)cobalt(II), (C<sub>5</sub>H<sub>6</sub>IN<sub>2</sub>)[CoBr<sub>0.51</sub>Cl<sub>2.48</sub>(C<sub>5</sub>H<sub>5</sub>IN<sub>2</sub>)] or (5-IAPH)[(5IAP)CoCl<sub>2.48</sub>Br<sub>0.51</sub>], as blue block-shaped crystals. Two of the three halide positions exhibit mixed occupancy [Cl/Br = 0.797 (5):0.203 (5) and 0.689 (6):0.311 (6)], while the third position is occupied solely by a chloride ion. 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引用次数: 0
摘要
2-氨基-5-碘吡啶(5IAP)与浓HBr在室温下反应生成2-氨基-5-碘溴化吡啶C5H6IN2 +·Br-或(5IAPH)Br。该配合物形成淡黄色晶体,在氨基和吡啶N-H给体和溴离子受体之间表现出明显的氢键。卤素键也被观察到。同样,5IAP与氯化钴(II)在混合HCl/HBr中在1-丙醇中反应生成2-氨基-5-碘吡啶(2-氨基-5-碘吡啶-κ n 1)溴/氯-(0.51/2.48)钴(II), (C5H6IN2)[CoBr0.51Cl2.48(C5H5IN2)]或(5-IAPH)[(5IAP)CoCl2.48Br0.51],呈蓝色块状晶体。三个卤化物位置中有两个呈现混合占据[Cl/Br = 0.797(5):0.203(5)和0.689(6):0.311(6)],而第三个位置仅被氯离子占据。观察到广泛的氢和卤素成键。
Compound 1 is the anhydrous form of the known crystal 2-amino-5-iodopyridinium bromide monohydrate and crystallizes in layers inclined ∼40° to the ab face. Hydrogen bonding between the amino and pyridinium ions to the bromide ion acceptor stabilizes the layers. Compound 2 is a salt of 2-amino-5-iodopyridium and a trihalidocobaltate(II) ion with one coordinated 2-amino-5-iodopyridine ligand. The halide ions are mixed Cl/Br with differing occupancies.
Reaction of 2-amino-5-iodopyridine (5IAP) with concentrated HBr at room temperature yielded 2-amino-5-iodopyridinium bromide, C5H6IN2+·Br− or (5IAPH)Br. The complex formed pale-yellow crystals, which exhibit significant hydrogen bonding between the amino and pyridinium N—H donors and bromide ion acceptors. Halogen bonding is also observed. Similarly, reaction of 5IAP with cobalt(II) chloride in mixed HCl/HBr in 1-propanol yielded 2-amino-5-iodopyridinium (2-amino-5-iodopyridine-κN1)bromido/chlorido(0.51/2.48)cobalt(II), (C5H6IN2)[CoBr0.51Cl2.48(C5H5IN2)] or (5-IAPH)[(5IAP)CoCl2.48Br0.51], as blue block-shaped crystals. Two of the three halide positions exhibit mixed occupancy [Cl/Br = 0.797 (5):0.203 (5) and 0.689 (6):0.311 (6)], while the third position is occupied solely by a chloride ion. Extensive hydrogen and halogen bonding is observed.
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.