The crystal structure of a mercury(II) halide complex containing bis(tert-butylamido)cyclodiphosphazane ligand with an unusual chelation mode is reported. The molecular structure features weak N—H⋯O interactions that propagate and link the molecules into a three-dimensional structure.
The mercury(II) halide complex [1,3-di-tert-butyl-2,4-bis(tert-butylamino)-1,3,2λ5,4λ5-diazadiphosphetidine-2,4-diselone-κ2Se,Se′]diiodidomercury(II)N,N-dimethylformamide monosolvate, [HgI2(C16H38N4P2Se2)]·C3H7NO or (1)HgI2, 2, containing cis-[(tBuNH)(Se)P(μ-NtBu)2P(Se)(NHtBu)] (1) was synthesized and structurally characterized. The crystal structure of 2 confirms the chelation of chalcogen donors to HgI2 with a natural bite angle of 112.95 (2)°. The coordination geometry around mercury is distorted tetrahedral as indicated by the τ4 geometry index parameter (τ4 = 0.90). In the mercury complex, the exocyclic tert-butylamido substituents are arranged in an (endo, endo) fashion, whereas in the free ligand (1), the exocyclic substituents are arranged in an (exo, endo) pattern. Compound 2 displays non-classical N—H⋯O hydrogen-bonding interactions with the solvent N,N-dimethylformamide. These interactions may introduce geometrical distortion and deviation from an ideal geometry. An isostructural HgBr2 analogue containing cis-[(tBuNH)(S)P(μ-NtBu)2P(S)(NHtBu)] was also synthesized and structurally characterized, CIF data for the compound being presented as supporting information.
合成了含顺式-[(t BuNH)(Se)P(μ-N -t Bu)2P(Se)(NH t Bu)]（1)的汞（II）卤化物配合物[1,3-二叔丁基-2,4-二叔丁基-氨基）-1,3,2λ5,4λ5-二氮杂二磷酸-2,4-二甲基甲酰胺-κ2 Se，Se']二碘汞（II）N，N-二甲基甲酰胺单溶剂化物[HgI2(C16H38N4P2Se2)]·C3H7NO或(1)hgi2,2](1)。2的晶体结构证实了硫供体与HgI2的螯合作用，其自然咬合角为112.95(2)°。由τ4几何指数参数（τ4 = 0.90）可知，汞周围的配位几何是扭曲的四面体。在汞配合物中，外环叔丁基胺取代基以（内、内）方式排列，而在自由配体(1)中，外环取代基以（外、内）方式排列。化合物2与溶剂N，N-二甲基甲酰胺表现出非经典的N- h⋯O氢键相互作用。这些相互作用可能导致几何畸变和偏离理想几何。合成了一种含有顺式-[(t BuNH)(S)P(μ-N t Bu)2P(S)(NH t Bu)]的同构HgBr2类似物，并对其进行了结构表征，以CIF数据作为支持信息。
{"title":"Mercury(II) halide complex of cis-[(tBuNH)(Se)P(μ-NtBu)2P(Se)(NHtBu)]","authors":"Troy Selby-Karney , Kalpana Sampath , Kuppuswamy Arumugam , Chandru P. Chandrasekaran","doi":"10.1107/S205698902400937X","DOIUrl":"10.1107/S205698902400937X","url":null,"abstract":"<div><div>The crystal structure of a mercury(II) halide complex containing bis(<em>tert-</em>butylamido)cyclodiphosphazane ligand with an unusual chelation mode is reported. The molecular structure features weak N—H⋯O interactions that propagate and link the molecules into a three-dimensional structure.</div></div><div><div>The mercury(II) halide complex [1,3-di-<em>tert</em>-butyl-2,4-bis(<em>tert</em>-butylamino)-1,3,2λ<sup>5</sup>,4λ<sup>5</sup>-diazadiphosphetidine-2,4-diselone-κ<sup>2</sup><em>Se</em>,<em>Se</em>′]diiodidomercury(II)<em>N</em>,<em>N</em>-dimethylformamide monosolvate, [HgI<sub>2</sub>(C<sub>16</sub>H<sub>38</sub>N<sub>4</sub>P<sub>2</sub>Se<sub>2</sub>)]·C<sub>3</sub>H<sub>7</sub>NO or (<strong>1</strong>)HgI<sub>2</sub>, <strong>2</strong>, containing <em>cis</em>-[(<sup><em>t</em></sup>BuNH)(Se)P(μ-N<sup><em>t</em></sup>Bu)<sub>2</sub>P(Se)(NH<sup><em>t</em></sup>Bu)] (<strong>1</strong>) was synthesized and structurally characterized. The crystal structure of <strong>2</strong> confirms the chelation of chalcogen donors to HgI<sub>2</sub> with a natural bite angle of 112.95 (2)°. The coordination geometry around mercury is distorted tetrahedral as indicated by the τ<sub>4</sub> geometry index parameter (τ<sub>4</sub> = 0.90). In the mercury complex, the exocyclic <em>tert</em>-butylamido substituents are arranged in an (<em>endo, endo</em>) fashion, whereas in the free ligand (<strong>1</strong>), the exocyclic substituents are arranged in an (<em>exo, endo</em>) pattern. Compound <strong>2</strong> displays non-classical N—H⋯O hydrogen-bonding interactions with the solvent <em>N</em>,<em>N</em>-dimethylformamide. These interactions may introduce geometrical distortion and deviation from an ideal geometry. An isostructural HgBr<sub>2</sub> analogue containing <em>cis</em>-[(<sup><em>t</em></sup>BuNH)(S)P(μ-N<sup><em>t</em></sup>Bu)<sub>2</sub>P(S)(NH<sup><em>t</em></sup>Bu)] was also synthesized and structurally characterized, CIF data for the compound being presented as supporting information.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 11","pages":"Pages 1142-1145"},"PeriodicalIF":0.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11660463/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142875860","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 : 2024-10-01DOI: 10.1107/S2056989024004158
Tebogo M. L. Mokoto , Andreas Lemmerer , Yasien Sayed , Mark G. Smith
The multi-component solvated Lopinavir crystal was prepared using evaporative methods. The crystal structure is unusual in that the unit cell contains 18 molecules. The stoichiometric ratio of this crystal is eight Lopinavir molecules, three ethane-1,2-diol molecules and seven water molecules.
Lopinavir is a potent protease inhibitor that is used as a first-line pharmaceutical drug for the treatment of HIV. The multi-component solvated Lopinavir crystal, systematic name (2S)-N-[(2S,4S,5S)-5-[2-(2,6-dimethylphenoxy)acetamido]-4-hydroxy-1,6-diphenylhexan-2-yl]-3-methyl-2-(2-oxo-1,3-diazinan-1-yl)butanamide–ethane-1,2-diol–water (8/3/7) 8C37H48N4O5·3C2H6O2·7H2O, was prepared using evaporative methods. The crystalline material obtained from this experimental synthesis was characterized and elucidated by single-crystal X-ray diffraction (SC-XRD). The crystal structure is unusual in that the unit cell contains 18 molecules. The stoichiometric ratio of this crystal is eight Lopinavir molecules [8(C37H48N4O5)], three ethane-1,2-diol molecules [3(C2H6O2)] and seven water molecules [7(H2O)]. The crystal packing features both bi- and trifurcated hydrogen bonds between atoms.
{"title":"Structural multiplicity in a solvated hydrate of the antiretroviral protease inhibitor Lopinavir","authors":"Tebogo M. L. Mokoto , Andreas Lemmerer , Yasien Sayed , Mark G. Smith","doi":"10.1107/S2056989024004158","DOIUrl":"10.1107/S2056989024004158","url":null,"abstract":"<div><div>The multi-component solvated Lopinavir crystal was prepared using evaporative methods. The crystal structure is unusual in that the unit cell contains 18 molecules. The stoichiometric ratio of this crystal is eight Lopinavir molecules, three ethane-1,2-diol molecules and seven water molecules.</div></div><div><div>Lopinavir is a potent protease inhibitor that is used as a first-line pharmaceutical drug for the treatment of HIV. The multi-component solvated Lopinavir crystal, systematic name (2<em>S</em>)-<em>N</em>-[(2<em>S</em>,4<em>S</em>,5<em>S</em>)-5-[2-(2,6-dimethylphenoxy)acetamido]-4-hydroxy-1,6-diphenylhexan-2-yl]-3-methyl-2-(2-oxo-1,3-diazinan-1-yl)butanamide–ethane-1,2-diol–water (8/3/7) 8C<sub>37</sub>H<sub>48</sub>N<sub>4</sub>O<sub>5</sub>·3C<sub>2</sub>H<sub>6</sub>O<sub>2</sub>·7H<sub>2</sub>O, was prepared using evaporative methods. The crystalline material obtained from this experimental synthesis was characterized and elucidated by single-crystal X-ray diffraction (SC-XRD). The crystal structure is unusual in that the unit cell contains 18 molecules. The stoichiometric ratio of this crystal is eight Lopinavir molecules [8(C<sub>37</sub>H<sub>48</sub>N<sub>4</sub>O<sub>5</sub>)], three ethane-1,2-diol molecules [3(C<sub>2</sub>H<sub>6</sub>O<sub>2</sub>)] and seven water molecules [7(H<sub>2</sub>O)]. The crystal packing features both bi- and trifurcated hydrogen bonds between atoms.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 11","pages":"Pages 1206-1209"},"PeriodicalIF":0.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11660481/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142875868","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 : 2024-10-01DOI: 10.1107/S2056989024009356
Christian Näther , Henning Lühmann , Wolfgang Bensch
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.
{"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":"10.1107/S2056989024009356","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":0.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11660490/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142875898","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 : 2024-10-01DOI: 10.1107/S2056989024009800
Manuel Stapf , Venugopal Rao Miyyapuram , Wilhelm Seichter , Monika Mazik
In the crystal structure, the molecules are connected by N—H⋯O hydrogen bonds to create two-dimensional supramolecular networks extending parallel to the crystallographic ab plane.
The title compound, C18H21N3O3, was prepared from 1,3,5-benzenetricarbonyl trichloride and cyclopropylamine. Its crystal structure was solved in the monoclinic space group P21/c. In the crystal, the three amide groups of the molecule are inclined at angles of 26.5 (1), 36.9 (1) and 37.8 (1)° with respect to the plane of the benzene ring. The molecules are linked by N—H⋯O hydrogen bonds, forming two-dimensional supramolecular aggregates that extend parallel to the crystallographic ab plane and are further connected by C—H⋯O contacts. As a result of the supramolecular interactions, a propeller-like conformation of the title molecule can be observed.
{"title":"Crystal structure of N,N′,N′′-tricyclopropylbenzene-1,3,5-tricarboxamide","authors":"Manuel Stapf , Venugopal Rao Miyyapuram , Wilhelm Seichter , Monika Mazik","doi":"10.1107/S2056989024009800","DOIUrl":"10.1107/S2056989024009800","url":null,"abstract":"<div><div>In the crystal structure, the molecules are connected by N—H⋯O hydrogen bonds to create two-dimensional supramolecular networks extending parallel to the crystallographic <em>ab</em> plane.</div></div><div><div>The title compound, C<sub>18</sub>H<sub>21</sub>N<sub>3</sub>O<sub>3</sub>, was prepared from 1,3,5-benzenetricarbonyl trichloride and cyclopropylamine. Its crystal structure was solved in the monoclinic space group <em>P</em>2<sub>1</sub>/<em>c</em>. In the crystal, the three amide groups of the molecule are inclined at angles of 26.5 (1), 36.9 (1) and 37.8 (1)° with respect to the plane of the benzene ring. The molecules are linked by N—H⋯O hydrogen bonds, forming two-dimensional supramolecular aggregates that extend parallel to the crystallographic <em>ab</em> plane and are further connected by C—H⋯O contacts. As a result of the supramolecular interactions, a propeller-like conformation of the title molecule can be observed.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 11","pages":"Pages 1194-1197"},"PeriodicalIF":0.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11660470/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142875778","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 : 2024-10-01DOI: 10.1107/S2056989024009976
Pierre Seidel , Franziska Gottwald , Eric Meier , Monika Mazik
The title molecule adopts a conformation in which the three phenyl rings are arranged in a paddlewheel-like fashion around the central arene ring and the carboxyl residue is oriented nearly perpendicular to the plane of this benzene ring. Inversion-symmetric dimers of O—H⋯O-bonded molecules represent the basic supramolecular entities of the crystal structure. These dimeric molecular units are further linked by C—H⋯O=C bonds, forming one-dimensional supramolecular aggregates along [111].
Crystal growth of 2-(3,4,5-triphenylphenyl)acetic acid (1) from acetonitrile yields a monosolvate, C26H20O2·CH3CN, of the space group P1. In the crystal, the title molecule adopts a conformation in which the three phenyl rings are arranged in a paddlewheel-like fashion around the central arene ring and the carboxyl residue is oriented nearly perpendicular to the plane of this benzene ring. Inversion-symmetric dimers of O—H⋯O-bonded molecules of 1 represent the basic supramolecular entities of the crystal structure. These dimeric molecular units are further linked by C—H⋯O=C bonds to form one-dimensional supramolecular aggregates running along the crystallographic [111] direction. Weak Caryl—H⋯N interactions occur between the molecules of 1 and acetonitrile.
{"title":"Crystal structure of an acetonitrile solvate of 2-(3,4,5-triphenylphenyl)acetic acid","authors":"Pierre Seidel , Franziska Gottwald , Eric Meier , Monika Mazik","doi":"10.1107/S2056989024009976","DOIUrl":"10.1107/S2056989024009976","url":null,"abstract":"<div><div>The title molecule adopts a conformation in which the three phenyl rings are arranged in a paddlewheel-like fashion around the central arene ring and the carboxyl residue is oriented nearly perpendicular to the plane of this benzene ring. Inversion-symmetric dimers of O—H⋯O-bonded molecules represent the basic supramolecular entities of the crystal structure. These dimeric molecular units are further linked by C—H⋯O=C bonds, forming one-dimensional supramolecular aggregates along [111].</div></div><div><div>Crystal growth of 2-(3,4,5-triphenylphenyl)acetic acid (<strong>1</strong>) from acetonitrile yields a monosolvate, C<sub>26</sub>H<sub>20</sub>O<sub>2</sub>·CH<sub>3</sub>CN, of the space group <em>P</em>1. In the crystal, the title molecule adopts a conformation in which the three phenyl rings are arranged in a paddlewheel-like fashion around the central arene ring and the carboxyl residue is oriented nearly perpendicular to the plane of this benzene ring. Inversion-symmetric dimers of O—H⋯O-bonded molecules of <strong>1</strong> represent the basic supramolecular entities of the crystal structure. These dimeric molecular units are further linked by C—H⋯O=C bonds to form one-dimensional supramolecular aggregates running along the crystallographic [111] direction. Weak C<sub>aryl</sub>—H⋯N interactions occur between the molecules of <strong>1</strong> and acetonitrile.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 11","pages":"Pages 1198-1201"},"PeriodicalIF":0.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11660473/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142875832","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 : 2024-10-01DOI: 10.1107/S2056989024010302
Hai Le Thi Hong , Hien Nguyen , Duong Trinh Hong , Ninh Nguyen Hoang , Khanh Nguyen Nhat , Luc Van Meervelt
Two new zinc(II) complexes, C21H13Cl2N2O3Zn·C6H16N (ZnOQ) and C20H14Cl4N2O2Zn·2C6H16N (ZnBS), were synthesized and their structures were determined using ESI–MS spectrometry, 1H NMR spectroscopy, and single-crystal X-ray diffraction.
Two new zinc(II) complexes, triethylammonium dichlorido[2-(4-nitrophenyl)-4-phenylquinolin-8-olato]zinc(II), (C6H16N){Zn(C21H13N2O3)Cl2] (ZnOQ), and bis(triethylammonium) {2,2′-[1,4-phenylenebis(nitrilomethylidyne)]diphenolato}bis[dichloridozinc(II)], (C6H16N)2[Zn2(C20H14N2O2)Cl4] (ZnBS), were synthesized and their structures were determined using ESI–MS spectrometry, 1H NMR spectroscopy, and single-crystal X-ray diffraction. The results showed that the ligands 2-(4-nitrophenyl)-4-phenylquinolin-8-ol (HOQ) and N,N′-bis(2-hydroxybenzylidene)benzene-1,4-diamine (H2BS) were deprotonated by triethyl-amine, forming the counter-ion Et3NH+, which interacts via an N—H⋯O hydrogen bond with the ligand. The ZnII atoms have a distorted trigonal–pyramidal (ZnOQ) and distorted tetrahedral (ZnBS) geometries with a coordination number of four, coordinating with the ligands via N and O atoms. The N atoms coordinating with ZnII correspond to the heterocyclic nitrogen for the HOQ ligand, while for the H2BS ligand, it is the nitrogen of the imine (CH=N). The crystal packing of ZnOQ is characterized by C—H⋯π interactions, while that of ZnBS by C—H⋯Cl interactions. The emission spectra showed that ZnBS complex exhibits green fluorescence in the solid state with a small band-gap energy, and the ZnOQ complex does exhibit non-fluorescence.
{"title":"Crystal structures and photophysical properties of mono- and dinuclear ZnII complexes flanked by triethylammonium","authors":"Hai Le Thi Hong , Hien Nguyen , Duong Trinh Hong , Ninh Nguyen Hoang , Khanh Nguyen Nhat , Luc Van Meervelt","doi":"10.1107/S2056989024010302","DOIUrl":"10.1107/S2056989024010302","url":null,"abstract":"<div><div>Two new zinc(II) complexes, C<sub>21</sub>H<sub>13</sub>Cl<sub>2</sub>N<sub>2</sub>O<sub>3</sub>Zn·C<sub>6</sub>H<sub>16</sub>N (<strong>ZnOQ</strong>) and C<sub>20</sub>H<sub>14</sub>Cl<sub>4</sub>N<sub>2</sub>O<sub>2</sub>Zn·2C<sub>6</sub>H<sub>16</sub>N (<strong>ZnBS</strong>), were synthesized and their structures were determined using ESI–MS spectrometry, <sup>1</sup>H NMR spectroscopy, and single-crystal X-ray diffraction.</div></div><div><div>Two new zinc(II) complexes, triethylammonium dichlorido[2-(4-nitrophenyl)-4-phenylquinolin-8-olato]zinc(II), (C<sub>6</sub>H<sub>16</sub>N){Zn(C<sub>21</sub>H<sub>13</sub>N<sub>2</sub>O<sub>3</sub>)Cl<sub>2</sub>] (<strong>ZnOQ</strong>), and bis(triethylammonium) {2,2′-[1,4-phenylenebis(nitrilomethylidyne)]diphenolato}bis[dichloridozinc(II)], (C<sub>6</sub>H<sub>16</sub>N)<sub>2</sub>[Zn<sub>2</sub>(C<sub>20</sub>H<sub>14</sub>N<sub>2</sub>O<sub>2</sub>)Cl<sub>4</sub>] (<strong>ZnBS</strong>), were synthesized and their structures were determined using ESI–MS spectrometry, <sup>1</sup>H NMR spectroscopy, and single-crystal X-ray diffraction. The results showed that the ligands 2-(4-nitrophenyl)-4-phenylquinolin-8-ol (<strong>HOQ</strong>) and <em>N</em>,<em>N</em>′-bis(2-hydroxybenzylidene)benzene-1,4-diamine (<strong>H<sub>2</sub>BS</strong>) were deprotonated by triethyl-amine, forming the counter-ion Et<sub>3</sub>NH<sup>+</sup>, which interacts <em>via</em> an N—H⋯O hydrogen bond with the ligand. The Zn<sup>II</sup> atoms have a distorted trigonal–pyramidal (<strong>ZnOQ</strong>) and distorted tetrahedral (<strong>ZnBS</strong>) geometries with a coordination number of four, coordinating with the ligands <em>via</em> N and O atoms. The N atoms coordinating with Zn<sup>II</sup> correspond to the heterocyclic nitrogen for the <strong>HOQ</strong> ligand, while for the <strong>H<sub>2</sub>BS</strong> ligand, it is the nitrogen of the imine (CH=N). The crystal packing of <strong>ZnOQ</strong> is characterized by C—H⋯π interactions, while that of <strong>ZnBS</strong> by C—H⋯Cl interactions. The emission spectra showed that <strong>ZnBS</strong> complex exhibits green fluorescence in the solid state with a small band-gap energy, and the <strong>ZnOQ</strong> complex does exhibit non-fluorescence.</div></div>","PeriodicalId":7367,"journal":{"name":"Acta Crystallographica Section E: Crystallographic Communications","volume":"80 11","pages":"Pages 1210-1216"},"PeriodicalIF":0.5,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11660477/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142875847","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 : 2024-09-30eCollection 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 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}
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