Pub Date : 2024-09-30eCollection Date: 2024-09-01DOI: 10.1107/S2056989024008272
Susan A Bourne, Delia A Haynes, Michele Zema
This virtual collection is a celebration. It is a celebration of crystallography in Africa, and a celebration of the international crystallography community. It commemorates the founding of the African Crystallographic Association (AfCA), which was accepted as the newest Regional Associate of the International Union of Crystallography (IUCr) in 2023, the year of the 75th anniversary of the first IUCr Congress and General Assembly. The collection contains research articles authored by scientists across the African continent, as well as a selection of articles giving context to crystallography in Africa. These discuss history, collaboration between scientists and between associations, and various educational and outreach initiatives.
{"title":"Foreword to the AfCA collection: celebrating work published by African researchers in IUCr journals.","authors":"Susan A Bourne, Delia A Haynes, Michele Zema","doi":"10.1107/S2056989024008272","DOIUrl":"10.1107/S2056989024008272","url":null,"abstract":"<p><p>This virtual collection is a celebration. It is a celebration of crystallography in Africa, and a celebration of the international crystallography community. It commemorates the founding of the African Crystallographic Association (AfCA), which was accepted as the newest Regional Associate of the International Union of Crystallography (IUCr) in 2023, the year of the 75th anniversary of the first IUCr Congress and General Assembly. The collection contains research articles authored by scientists across the African continent, as well as a selection of articles giving context to crystallography in Africa. These discuss history, collaboration between scientists and between associations, and various educational and outreach initiatives.</p>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 Pt 10","pages":"997-998"},"PeriodicalIF":0.5,"publicationDate":"2024-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11451496/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142379777","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The structures of Orn-free Gramicidin S with cis/trans-isomers of Hyp were solved, and the puckering of Hyp was unexpectedly down in both isomers.
The cyclic peptide cyclo(Val-Leu-Leu-d-Phe-Pro)2 (peptide 1) was specifically designed for structural chemistry investigations, drawing inspiration from Gramicidin S (GS). Previous studies have shown that Pro residues within 1 adopt a down-puckering conformation of the pyrrolidine ring. By incorporating fluoride-Pro with 4-trans/cis-isomers into 1, an up-puckering conformation was successfully induced. In the current investigation, introducing hydroxyprolines with 4-trans/cis-isomer configurations (tHyp/cHyp) into 1 gave cyclo(Val-Leu-Leu-d-Phe-tHyp)2 methanol disolvate monohydrate, C62H94N10O12·2CH4O·H2O (4), and cyclo(Val-Leu-Leu-d-Phe-cHyp)2 monohydrate, C62H94N10O12·H2O (5), respectively. However, the puckering of 4 and 5 remained in the down conformation, regardless of the geometric position of the hydroxyl group. Although the backbone structure of 4 with trans-substitution was asymmetric, the asymmetric backbone of 5 with cis-substitution was unexpected. It is speculated that the anticipated influence of stress from the geometric positioning, which was expected to affect the puckering, may have been mitigated by interactions between the hydroxyl groups of hydroxyproline, the solvent molecules, and peptides.
{"title":"Puckering effects of 4-hydroxy-l-proline isomers on the conformation of ornithine-free Gramicidin S","authors":"Akiko Asano , Kanako Nakayama , Sakura Okada , Takuma Kato , Mitsunobu Doi","doi":"10.1107/S2056989024007771","DOIUrl":"10.1107/S2056989024007771","url":null,"abstract":"<div><p>The structures of Orn-free Gramicidin S with <em>cis/trans</em>-isomers of Hyp were solved, and the puckering of Hyp was unexpectedly down in both isomers.</p></div><div><p>The cyclic peptide <em>cyclo</em>(Val-Leu-Leu-<span>d</span>-Phe-Pro)<sub>2</sub> (peptide <strong>1</strong>) was specifically designed for structural chemistry investigations, drawing inspiration from Gramicidin S (GS). Previous studies have shown that Pro residues within <strong>1</strong> adopt a down-puckering conformation of the pyrrolidine ring. By incorporating fluoride-Pro with 4-<em>trans</em>/<em>cis</em>-isomers into <strong>1</strong>, an up-puckering conformation was successfully induced. In the current investigation, introducing hydroxyprolines with 4-<em>trans</em>/<em>cis</em>-isomer configurations (tHyp/cHyp) into <strong>1</strong> gave <em>cyclo</em>(Val-Leu-Leu-<span>d</span>-Phe-tHyp)<sub>2</sub> methanol disolvate monohydrate, C<sub>62</sub>H<sub>94</sub>N<sub>10</sub>O<sub>12</sub>·2CH<sub>4</sub>O·H<sub>2</sub>O (<strong>4</strong>), and <em>cyclo</em>(Val-Leu-Leu-<span>d</span>-Phe-cHyp)<sub>2</sub> monohydrate, C<sub>62</sub>H<sub>94</sub>N<sub>10</sub>O<sub>12</sub>·H<sub>2</sub>O (<strong>5</strong>), respectively. However, the puckering of <strong>4</strong> and <strong>5</strong> remained in the down conformation, regardless of the geometric position of the hydroxyl group. Although the backbone structure of <strong>4</strong> with <em>trans</em>-substitution was asymmetric, the asymmetric backbone of <strong>5</strong> with <em>cis</em>-substitution was unexpected. It is speculated that the anticipated influence of stress from the geometric positioning, which was expected to affect the puckering, may have been mitigated by interactions between the hydroxyl groups of hydroxyproline, the solvent molecules, and peptides.</p></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 9","pages":"Pages 942-946"},"PeriodicalIF":0.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141923887","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The title compound, which was obtained by the reaction between 1,10-phenanthroline and phenyltin trichloride in methanol, exhibits intramolecular interactions involving the chlorine and hydrogen atoms. Crystal cohesion is ensured by intermolecular C—H⋯Cl hydrogen bonds, as well as Y—X⋯π and π-stacking interactions
The title compound, [Sn(C6H5)Cl3(C12H8N2)], which was obtained by the reaction between 1,10-phenanthroline and phenyltin trichloride in methanol, exhibits intramolecular hydrogen-bonding interactions involving the chlorine and hydrogen atoms. Crystal cohesion is ensured by intermolecular C—H⋯Cl hydrogen bonds, as well as Y—X⋯π and π-stacking interactions involving three different aromatic rings with centroid–centroid distances of 3.6605 (13), 3.9327 (14) and 3.6938 (12) Å]. Hirshfeld surface analysis and the associated two-dimensional fingerprint plots reveal significant contributions from H⋯H (30.7%), Cl⋯H/H⋯Cl (32.4%), and C⋯H/H⋯C (24.0%) contacts to the crystal packing while the C⋯C (6.2%), C⋯Cl/Cl⋯C (4.1%), and N⋯H/H⋯N (1.7%) interactions make smaller contributions.
{"title":"Crystal structure and Hirshfeld surface analysis of trichlorido(1,10-phenanthroline-κ2N,N′)phenyltin(IV)","authors":"Tarek Benlatreche , Mohamed Abdellatif Bensegueni , Georges Dénès , Stéphane Golhen , Hocine Merazig","doi":"10.1107/S2056989024009150","DOIUrl":"10.1107/S2056989024009150","url":null,"abstract":"<div><div>The title compound, which was obtained by the reaction between 1,10-phenanthroline and phenyltin trichloride in methanol, exhibits intramolecular interactions involving the chlorine and hydrogen atoms. Crystal cohesion is ensured by intermolecular C—H⋯Cl hydrogen bonds, as well as <em>Y</em>—<em>X</em>⋯π and π-stacking interactions</div></div><div><div>The title compound, [Sn(C<sub>6</sub>H<sub>5</sub>)Cl<sub>3</sub>(C<sub>12</sub>H<sub>8</sub>N<sub>2</sub>)], which was obtained by the reaction between 1,10-phenanthroline and phenyltin trichloride in methanol, exhibits intramolecular hydrogen-bonding interactions involving the chlorine and hydrogen atoms. Crystal cohesion is ensured by intermolecular C—H⋯Cl hydrogen bonds, as well as <em>Y</em>—<em>X</em>⋯π and π-stacking interactions involving three different aromatic rings with centroid–centroid distances of 3.6605 (13), 3.9327 (14) and 3.6938 (12) Å]. Hirshfeld surface analysis and the associated two-dimensional fingerprint plots reveal significant contributions from H⋯H (30.7%), Cl⋯H/H⋯Cl (32.4%), and C⋯H/H⋯C (24.0%) contacts to the crystal packing while the C⋯C (6.2%), C⋯Cl/Cl⋯C (4.1%), and N⋯H/H⋯N (1.7%) interactions make smaller contributions.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 10","pages":"Pages 1039-1043"},"PeriodicalIF":0.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11451494/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142379772","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-01DOI: 10.1107/S205698902400882X
Betty Fuhrmann , Eric Meier , Monika Mazik
An analysis of the complex structure obtained by crystallization of 5-nonanoyl-8-hydroxyquinoline and InCl3 in acetonitrile is reported.
Crystallization of 5-nonanoyl-8-hydroxyquinoline in the presence of InCl3 in acetonitrile yields a dinuclear InIII complex crystallizing in the space group P
. In this complex, [In2(C18H22NO2)2Cl4(H2O)2], each indium ion is sixfold coordinated by two chloride ions, one water molecule and two 8-quinolinolate ions. The crystal of the title complex is composed of two-dimensional supramolecular aggregates, resulting from the linkage of the Owater—H⋯O=C and Owater—H⋯Cl hydrogen bonds as well as bifurcated Carene—H⋯Cl contacts.
{"title":"Crystal structure of bis(μ2-5-nonanoylquinolin-8-olato)bis[aquadichloridoindium(III)]","authors":"Betty Fuhrmann , Eric Meier , Monika Mazik","doi":"10.1107/S205698902400882X","DOIUrl":"10.1107/S205698902400882X","url":null,"abstract":"<div><div>An analysis of the complex structure obtained by crystallization of 5-nonanoyl-8-hydroxyquinoline and InCl<sub>3</sub> in acetonitrile is reported.</div></div><div><div>Crystallization of 5-nonanoyl-8-hydroxyquinoline in the presence of InCl<sub>3</sub> in acetonitrile yields a dinuclear In<sup>III</sup> complex crystallizing in the space group <em>P</em><blockquote><div><figure><img></figure></div></blockquote>. In this complex, [In<sub>2</sub>(C<sub>18</sub>H<sub>22</sub>NO<sub>2</sub>)<sub>2</sub>Cl<sub>4</sub>(H<sub>2</sub>O)<sub>2</sub>], each indium ion is sixfold coordinated by two chloride ions, one water molecule and two 8-quinolinolate ions. The crystal of the title complex is composed of two-dimensional supramolecular aggregates, resulting from the linkage of the O<sub>water</sub>—H⋯O=C and O<sub>water</sub>—H⋯Cl hydrogen bonds as well as bifurcated C<sub>arene</sub>—H⋯Cl contacts.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 10","pages":"Pages 1020-1023"},"PeriodicalIF":0.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11451490/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142383290","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-01DOI: 10.1107/S2056989024009058
Christian Näther , Inke Jess
In the crystal structure of the title compound, the CoII cations are octahedrally coordinated by two bridging and one terminal thiocyanate anions, two bridging 4-methylpyridine N-oxide coligands and one ethanol molecule and linked into chains by single μ-1,3-bridging anionic ligands that are further connected into layers by pairs of μ-1,1(O,O)-bridging 4-methylpyridine N-oxide coligands.
Reaction of 4-methylpyridine N-oxide and Co(NCS)2 in ethanol as solvent accidentally leads to the formation of single crystals of Co(NCS)2(4-methylpyridine N-oxide)(ethanol) or [Co(NCS)2(C6H7NO)(C2H6O)]n. The asymmetric unit of the title compound consists of one CoII cation, two crystallographically independent thiocyanate anions, one 4-methylpyridine N-oxide coligand and one ethanol molecule on general positions. The cobalt cations are sixfold coordinated by one terminal and two bridging thiocyanate anions, two bridging 4-methylpyridine N-oxide coligands and one ethanol molecule, with a slightly distorted octahedral geometry. The cobalt cations are linked by single μ-1,3(N,S)-bridging thiocyanate anions into corrugated chains, that are further connected into layers by pairs of μ-1,1(O,O)-bridging 4-methylpyridine N-oxide coligands. The layers are parallel to the bc plane and are separated by the methyl groups of the 4-methylpyridine N-oxide coligands. Within the layers, intralayer hydrogen bonding is observed.
{"title":"Synthesis and crystal structure of poly[ethanol(μ-4-methylpyridine N-oxide)di-μ-thiocyanato-cobalt(II)]","authors":"Christian Näther , Inke Jess","doi":"10.1107/S2056989024009058","DOIUrl":"10.1107/S2056989024009058","url":null,"abstract":"<div><div>In the crystal structure of the title compound, the Co<sup>II</sup> cations are octahedrally coordinated by two bridging and one terminal thiocyanate anions, two bridging 4-methylpyridine <em>N</em>-oxide coligands and one ethanol molecule and linked into chains by single μ-1,3-bridging anionic ligands that are further connected into layers by pairs of μ-1,1(<em>O</em>,<em>O</em>)-bridging 4-methylpyridine <em>N</em>-oxide coligands.</div></div><div><div>Reaction of 4-methylpyridine <em>N</em>-oxide and Co(NCS)<sub>2</sub> in ethanol as solvent accidentally leads to the formation of single crystals of Co(NCS)<sub>2</sub>(4-methylpyridine <em>N</em>-oxide)(ethanol) or [Co(NCS)<sub>2</sub>(C<sub>6</sub>H<sub>7</sub>NO)(C<sub>2</sub>H<sub>6</sub>O)]<sub>n</sub>. The asymmetric unit of the title compound consists of one Co<sup>II</sup> cation, two crystallographically independent thiocyanate anions, one 4-methylpyridine <em>N</em>-oxide coligand and one ethanol molecule on general positions. The cobalt cations are sixfold coordinated by one terminal and two bridging thiocyanate anions, two bridging 4-methylpyridine <em>N</em>-oxide coligands and one ethanol molecule, with a slightly distorted octahedral geometry. The cobalt cations are linked by single μ-1,3(<em>N</em>,<em>S</em>)-bridging thiocyanate anions into corrugated chains, that are further connected into layers by pairs of μ-1,1(<em>O</em>,<em>O</em>)-bridging 4-methylpyridine <em>N</em>-oxide coligands. The layers are parallel to the <em>bc</em> plane and are separated by the methyl groups of the 4-methylpyridine <em>N</em>-oxide coligands. Within the layers, intralayer hydrogen bonding is observed.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 10","pages":"Pages 1029-1033"},"PeriodicalIF":0.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11451497/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142379871","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-01DOI: 10.1107/S2056989024008806
Nomampondo Penelope Magwa , Thompho Jason Rashamuse
The title complex, which consists of a central zinc metal ion surrounded by six 1-methylimidazole ligands, charge balanced by two nitrate anions and which crystallizes in the space group P
has been synthesized and its structure determined.
The synthesis of the title compound, [Zn(C4H6N2)6](NO3)2, is described. This complex consists of a central zinc metal ion surrounded by six 1-methylimidazole ligands, charge balanced by two nitrate anions. The complex crystallizes in the space group P
. In the crystal, the nitrate ions are situated within the cavities created by the [Zn(N-Melm)6]2+ cations, serving as counter-ions. The three oxygen atoms of the nitrate ion engage in weak C—H⋯O interactions. In addition to single-crystal X-ray diffraction analysis, the complex was characterized using elemental analysis, 1H NMR, 13C NMR, and FTIR spectroscopy.
本文描述了标题化合物[Zn(C4H6N2)6](NO3)2 的合成过程。该复合物由一个中心锌金属离子和六个 1-甲基咪唑配体组成，并由两个硝酸根阴离子平衡电荷。在晶体中，硝酸根离子位于[Zn(N-Melm)6]2+阳离子形成的空腔内，起着反离子的作用。硝酸根离子的三个氧原子参与微弱的 C-H⋯O 相互作用。除了单晶 X 射线衍射分析外，还利用元素分析、1H NMR、13C NMR 和傅立叶变换红外光谱对该复合物进行了表征。
{"title":"Synthesis, characterization, and crystal structure of hexakis(1-methyl-1H-imidazole-κN3)zinc(II) dinitrate","authors":"Nomampondo Penelope Magwa , Thompho Jason Rashamuse","doi":"10.1107/S2056989024008806","DOIUrl":"10.1107/S2056989024008806","url":null,"abstract":"<div><div>The title complex, which consists of a central zinc metal ion surrounded by six 1-methylimidazole ligands, charge balanced by two nitrate anions and which crystallizes in the space group <em>P</em><blockquote><div><figure><img></figure></div></blockquote> has been synthesized and its structure determined.</div></div><div><div>The synthesis of the title compound, [Zn(C<sub>4</sub>H<sub>6</sub>N<sub>2</sub>)<sub>6</sub>](NO<sub>3</sub>)<sub>2</sub>, is described. This complex consists of a central zinc metal ion surrounded by six 1-methylimidazole ligands, charge balanced by two nitrate anions. The complex crystallizes in the space group <em>P</em><blockquote><div><figure><img></figure></div></blockquote>. In the crystal, the nitrate ions are situated within the cavities created by the [Zn(<em>N</em>-Melm)<sub>6</sub>]<sup>2+</sup> cations, serving as counter-ions. The three oxygen atoms of the nitrate ion engage in weak C—H⋯O interactions. In addition to single-crystal X-ray diffraction analysis, the complex was characterized using elemental analysis, <sup>1</sup>H NMR, <sup>13</sup>C NMR, and FTIR spectroscopy.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 10","pages":"Pages 1054-1058"},"PeriodicalIF":0.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11451501/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142379872","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-01DOI: 10.1107/S2056989024007606
Gayane S. Tonoyan , Gerald Giester , Vahram V. Ghazaryan , Ruben Yu. Chilingaryan , Arthur A. Margaryan , Artak H. Mkrtchyan , Aram M. Petrosyan
The crystal structure of (GlyH)6(Pb3I12) is reported. Dimeric cations of type (A+⋯A+) for the amino acid glycine are observed for the first time.
The crystal structure of hexaglycinium tetra-μ-iodido-octaiodidotriplumbate, (C2H6NO2)6[Pb3I12] or (GlyH)6[Pb3I12], is reported. The compound crystallizes in the triclinic space group P
. The [Pb3I12]6− anion is discrete and located around a special position: the central Pb ion located on the inversion center is holodirected, while the other two are hemidirected. The supramolecular nature is mainly based on C—H⋯I, N—H⋯I, O—H⋯I and N—H⋯O hydrogen bonds. Dimeric cations of type (A+⋯A+) for the amino acid glycine are observed for the first time.
{"title":"Crystal structure of hexaglycinium dodecaiodotriplumbate","authors":"Gayane S. Tonoyan , Gerald Giester , Vahram V. Ghazaryan , Ruben Yu. Chilingaryan , Arthur A. Margaryan , Artak H. Mkrtchyan , Aram M. Petrosyan","doi":"10.1107/S2056989024007606","DOIUrl":"10.1107/S2056989024007606","url":null,"abstract":"<div><p>The crystal structure of (GlyH)<sub>6</sub>(Pb<sub>3</sub>I<sub>12</sub>) is reported. Dimeric cations of type (<em>A</em><sup>+</sup>⋯<em>A</em><sup>+</sup>) for the amino acid glycine are observed for the first time.</p></div><div><p>The crystal structure of hexaglycinium tetra-μ-iodido-octaiodidotriplumbate, (C<sub>2</sub>H<sub>6</sub>NO<sub>2</sub>)<sub>6</sub>[Pb<sub>3</sub>I<sub>12</sub>] or (GlyH)<sub>6</sub>[Pb<sub>3</sub>I<sub>12</sub>], is reported. The compound crystallizes in the triclinic space group <em>P</em></p><blockquote><p><figure><img></figure></p></blockquote>. The [Pb<sub>3</sub>I<sub>12</sub>]<sup>6−</sup> anion is discrete and located around a special position: the central Pb ion located on the inversion center is holodirected, while the other two are hemidirected. The supramolecular nature is mainly based on C—H⋯I, N—H⋯I, O—H⋯I and N—H⋯O hydrogen bonds. Dimeric cations of type (<em>A</em><sup>+</sup>⋯<em>A</em><sup>+</sup>) for the amino acid glycine are observed for the first time.</div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 9","pages":"Pages 916-920"},"PeriodicalIF":0.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142150203","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-01DOI: 10.1107/S2056989024008508
A. R. Karthiga , S. Divyabharathi , R. Reshwen Shalo , K. Rajeswari , T. Vidhyasagar , S. Selvanayagam
In the title compound, C23H24N2O2S, the two molecules in the asymmetric unit have a structural overlap with an r.m.s. deviation of 0.82 Å.
The two molecules in the asymmetric unit of the title compound, C23H24N2O2S, have a structural overlap with an r.m.s. deviation of 0.82 Å. The piperidine rings adopt a distorted boat conformation. Intra- and intermolecular C—H⋯O hydrogen bonds are responsible for the cohesion of the crystal packing. The intermolecular interactions were quantified and analysed using Hirshfeld surface analysis. The molecular structure optimized by density functional theory (DFT) at the B3LYP/6–311++G(d,p)level is compared with the experimentally determined molecular structure in the solid state.
{"title":"Crystal structure, Hirshfeld surface analysis, DFT optimized molecular structure and the molecular docking studies of 1-[2-(cyanosulfanyl)acetyl]-3-methyl-2,6-bis(4-methylphenyl)piperidin-4-one","authors":"A. R. Karthiga , S. Divyabharathi , R. Reshwen Shalo , K. Rajeswari , T. Vidhyasagar , S. Selvanayagam","doi":"10.1107/S2056989024008508","DOIUrl":"10.1107/S2056989024008508","url":null,"abstract":"<div><div>In the title compound, C<sub>23</sub>H<sub>24</sub>N<sub>2</sub>O<sub>2</sub>S, the two molecules in the asymmetric unit have a structural overlap with an r.m.s. deviation of 0.82 Å.</div></div><div><div>The two molecules in the asymmetric unit of the title compound, C<sub>23</sub>H<sub>24</sub>N<sub>2</sub>O<sub>2</sub>S, have a structural overlap with an r.m.s. deviation of 0.82 Å. The piperidine rings adopt a distorted boat conformation. Intra- and intermolecular C—H⋯O hydrogen bonds are responsible for the cohesion of the crystal packing. The intermolecular interactions were quantified and analysed using Hirshfeld surface analysis. The molecular structure optimized by density functional theory (DFT) at the B3LYP/6–311++G(d,p)level is compared with the experimentally determined molecular structure in the solid state.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 10","pages":"Pages 1014-1019"},"PeriodicalIF":0.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11451485/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142379774","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-01DOI: 10.1107/S2056989024008922
Sachin Thackeray , James Mahoney , Ashleigh Arrington , Miles Wilklow-Marnell , William W. Brennessel
<div><div>Phosphinito and phosphinomethyl ligands incorporating an anthraquinone moiety were reacted with bis(cycloocta-1,5-diene)diiridium(I) dichloride to afford novel diiridium species. Intended as pincer-type tridentate ligands, bidentate binding modes were determined by X-ray crystallography. The anionic μ-trichlorido phosphinito complex formed is charged-balanced by one [Ir(toluene)(cycloocta-1,5-diene)]<sup>+</sup> per asymmetric unit, the structure of which has not previously been reported despite a long history of use as an Ir<sup>I</sup> source in organometallic chemistry.</div></div><div><div>When reacted in dry, degassed toluene, [Ir(COD)Cl]<sub>2</sub> (COD = cycloocta-1,5-diene) and 2 equivalents of 2-(di-<em>tert</em>-butylphosphinito)anthraquinone (<sup>tBu</sup>POAQH) were found to form a unique tri-iridium compound consisting of one monoanionic dinuclear tri-μ-chlorido complex bearing one bidentate <sup>tBu</sup>POAQ ligand per iridium, which was charge-balanced by an outer sphere [Ir(toluene)(COD)]<sup>+</sup> ion, the structure of which has not previously been reported. This product, which is a toluene solvate, namely, (η<sup>2</sup>:η<sup>2</sup>-cycloocta-1,5-diene)(η<sup>6</sup>-toluene)iridium(I) tri-μ-chlorido-bis({3-[(di-<em>tert</em>-butylphosphanyl)oxy]-9,10-dioxoanthracen-2-yl}hydridoiridium(III)) toluene monosolvate, [Ir(C<sub>7</sub>H<sub>8</sub>)(C<sub>8</sub>H<sub>12</sub>)][Ir<sub>2</sub>H<sub>2</sub>(C<sub>22</sub>H<sub>24</sub>O<sub>3</sub>P)<sub>2</sub>Cl<sub>3</sub>]·C<sub>7</sub>H<sub>8</sub> or [Ir(toluene)(COD)][Ir(κ-<em>P</em>,<em>C</em>-<sup>tBu</sup>POAQ)(H)]<sub>2</sub>(μ-Cl)<sub>3</sub>]·toluene, formed as small orange platelets at room temperature, crystallizing in the triclinic space group <em>P</em><blockquote><div><figure><img></figure></div></blockquote>. The cation and anion are linked <em>via</em> weak C—H⋯O interactions. The stronger intermolecular attractions are likely the offset parallel π–π interactions, which occur between the toluene ligands of pairs of inverted cations and between pairs of inverted anthraquinone moieties, the latter of which are capped by toluene solvate molecules, making for π-stacks of four molecules each. The related ligand, 2-(di-<em>tert</em>-butylphosphinomethyl)-anthraquinone (<sup>tBu</sup>PCAQH), did not form crystals suitable for X-ray diffraction under analogous reaction conditions. However, when the reaction was conducted in chloroform, yellow needles readily formed following addition of 1 atm of carbon monoxide. Diffraction studies revealed a neutral, dinuclear, di-μ-chlorido complex, di-μ-chlorido-bis(carbonyl{3-[(di-<em>tert</em>-butylphosphanyl)oxy]-9,10-dioxoanthracen-2-yl}hydridoiridium(I)), [Ir<sub>2</sub>H<sub>2</sub>(C<sub>23</sub>H<sub>26</sub>O<sub>2</sub>P)<sub>2</sub>Cl<sub>2</sub>(CO)<sub>2</sub>] or [Ir(κ-<em>P</em>,<em>C</em>-<sup>tBu</sup>PCAQ)(H)(CO)(μ-Cl)]<sub>2</sub>, Ir<sub>2</sub>C<sub>48</sub>H<sub>54</sub>
{"title":"Crystal structures of the (η2:η2-cycloocta-1,5-diene)(η6-toluene)iridium(I) cation and μ-chlorido-iridium(III) complexes of 2-(phosphinito)- and 2-(phosphinomethyl)anthraquinone ligands","authors":"Sachin Thackeray , James Mahoney , Ashleigh Arrington , Miles Wilklow-Marnell , William W. Brennessel","doi":"10.1107/S2056989024008922","DOIUrl":"10.1107/S2056989024008922","url":null,"abstract":"<div><div>Phosphinito and phosphinomethyl ligands incorporating an anthraquinone moiety were reacted with bis(cycloocta-1,5-diene)diiridium(I) dichloride to afford novel diiridium species. Intended as pincer-type tridentate ligands, bidentate binding modes were determined by X-ray crystallography. The anionic μ-trichlorido phosphinito complex formed is charged-balanced by one [Ir(toluene)(cycloocta-1,5-diene)]<sup>+</sup> per asymmetric unit, the structure of which has not previously been reported despite a long history of use as an Ir<sup>I</sup> source in organometallic chemistry.</div></div><div><div>When reacted in dry, degassed toluene, [Ir(COD)Cl]<sub>2</sub> (COD = cycloocta-1,5-diene) and 2 equivalents of 2-(di-<em>tert</em>-butylphosphinito)anthraquinone (<sup>tBu</sup>POAQH) were found to form a unique tri-iridium compound consisting of one monoanionic dinuclear tri-μ-chlorido complex bearing one bidentate <sup>tBu</sup>POAQ ligand per iridium, which was charge-balanced by an outer sphere [Ir(toluene)(COD)]<sup>+</sup> ion, the structure of which has not previously been reported. This product, which is a toluene solvate, namely, (η<sup>2</sup>:η<sup>2</sup>-cycloocta-1,5-diene)(η<sup>6</sup>-toluene)iridium(I) tri-μ-chlorido-bis({3-[(di-<em>tert</em>-butylphosphanyl)oxy]-9,10-dioxoanthracen-2-yl}hydridoiridium(III)) toluene monosolvate, [Ir(C<sub>7</sub>H<sub>8</sub>)(C<sub>8</sub>H<sub>12</sub>)][Ir<sub>2</sub>H<sub>2</sub>(C<sub>22</sub>H<sub>24</sub>O<sub>3</sub>P)<sub>2</sub>Cl<sub>3</sub>]·C<sub>7</sub>H<sub>8</sub> or [Ir(toluene)(COD)][Ir(κ-<em>P</em>,<em>C</em>-<sup>tBu</sup>POAQ)(H)]<sub>2</sub>(μ-Cl)<sub>3</sub>]·toluene, formed as small orange platelets at room temperature, crystallizing in the triclinic space group <em>P</em><blockquote><div><figure><img></figure></div></blockquote>. The cation and anion are linked <em>via</em> weak C—H⋯O interactions. The stronger intermolecular attractions are likely the offset parallel π–π interactions, which occur between the toluene ligands of pairs of inverted cations and between pairs of inverted anthraquinone moieties, the latter of which are capped by toluene solvate molecules, making for π-stacks of four molecules each. The related ligand, 2-(di-<em>tert</em>-butylphosphinomethyl)-anthraquinone (<sup>tBu</sup>PCAQH), did not form crystals suitable for X-ray diffraction under analogous reaction conditions. However, when the reaction was conducted in chloroform, yellow needles readily formed following addition of 1 atm of carbon monoxide. Diffraction studies revealed a neutral, dinuclear, di-μ-chlorido complex, di-μ-chlorido-bis(carbonyl{3-[(di-<em>tert</em>-butylphosphanyl)oxy]-9,10-dioxoanthracen-2-yl}hydridoiridium(I)), [Ir<sub>2</sub>H<sub>2</sub>(C<sub>23</sub>H<sub>26</sub>O<sub>2</sub>P)<sub>2</sub>Cl<sub>2</sub>(CO)<sub>2</sub>] or [Ir(κ-<em>P</em>,<em>C</em>-<sup>tBu</sup>PCAQ)(H)(CO)(μ-Cl)]<sub>2</sub>, Ir<sub>2</sub>C<sub>48</sub>H<sub>54</sub>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 10","pages":"Pages 1101-1109"},"PeriodicalIF":0.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11451491/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142379776","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-01DOI: 10.1107/S2056989024008685
Ran Yan , Zhaohua Dai , Daniel G. Shlian , Trinit’y D. Mitchell , Aaron Loo , Kaltrina Mulosmani , Rita K. Upmacis
Crystals of tris[(6-bromopyridin-2-yl)methyl]amine (TPABr3) were obtained from a solution in acetonitrile upon evaporation. The crystals are triclinic with space group P
.
Coordination compounds of polydentate nitrogen ligands with metals are used extensively in research areas such as catalysis, and as models of complex active sites of enzymes in bioinorganic chemistry. Tris(2-pyridylmethyl)amine (TPA) is a tripodal tetradentate ligand that is known to form coordination compounds with metals, including copper, iron and zinc. The related compound, tris[(6-bromopyridin-2-yl)methyl]amine (TPABr3), C18H15Br3N4, which possesses a bromine atom on the 6-position of each of the three pyridyl moieties, is also known but has not been heavily investigated. The molecular structure of TPABr3 as determined by X-ray diffraction is reported here. The TPABr3 molecule belongs to the triclinic, P
space group and displays interesting intermolecular Br⋯Br interactions that provide a stabilizing influence within the molecule.
多齿硝基配体与金属的配位化合物被广泛应用于催化等研究领域，以及作为生物无机化学中酶的复合活性位点模型。三(2-吡啶基甲基)胺（TPA）是一种三元四齿配体，可与金属（包括铜、铁和锌）形成配位化合物。三溴吡啶-2-甲胺（TPABr3）（C18H15Br3N4）是一种相关化合物，在三个吡啶基的 6 位上各有一个溴原子。本文报告了通过 X 射线衍射测定的 TPABr3 的分子结构。TPABr3 分子属于三linic P 空间群，分子间存在有趣的 Br⋯Br 相互作用，对分子内部产生稳定影响。
{"title":"Molecular structure of tris[(6-bromopyridin-2-yl)methyl]amine","authors":"Ran Yan , Zhaohua Dai , Daniel G. Shlian , Trinit’y D. Mitchell , Aaron Loo , Kaltrina Mulosmani , Rita K. Upmacis","doi":"10.1107/S2056989024008685","DOIUrl":"10.1107/S2056989024008685","url":null,"abstract":"<div><div>Crystals of tris[(6-bromopyridin-2-yl)methyl]amine (TPABr<sub>3</sub>) were obtained from a solution in acetonitrile upon evaporation. The crystals are triclinic with space group <em>P</em><blockquote><div><figure><img></figure></div></blockquote>.</div></div><div><div>Coordination compounds of polydentate nitrogen ligands with metals are used extensively in research areas such as catalysis, and as models of complex active sites of enzymes in bioinorganic chemistry. Tris(2-pyridylmethyl)amine (TPA) is a tripodal tetradentate ligand that is known to form coordination compounds with metals, including copper, iron and zinc. The related compound, tris[(6-bromopyridin-2-yl)methyl]amine (TPABr<sub>3</sub>), C<sub>18</sub>H<sub>15</sub>Br<sub>3</sub>N<sub>4</sub>, which possesses a bromine atom on the 6-position of each of the three pyridyl moieties, is also known but has not been heavily investigated. The molecular structure of TPABr<sub>3</sub> as determined by X-ray diffraction is reported here. The TPABr<sub>3</sub> molecule belongs to the triclinic, <em>P</em><blockquote><div><figure><img></figure></div></blockquote> space group and displays interesting intermolecular Br⋯Br interactions that provide a stabilizing influence within the molecule.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 10","pages":"Pages 1006-1009"},"PeriodicalIF":0.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11451500/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142379778","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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