Journal of Chemical Crystallography最新文献

{"title":"Synthesis, Crystal Structure and Fluorescent Property of Cis-bis[N,N-diethyl-N'-(p-nitrobenzoyl)thiourea-kS,O] Platinum(II) Complex","authors":"Xing-hong Duan,&nbsp;Bi-quan Su,&nbsp;Liang Xian,&nbsp;Li Sheng,&nbsp;Rong Tan","doi":"10.1007/s10870-022-00976-8","DOIUrl":"10.1007/s10870-022-00976-8","url":null,"abstract":"<div><p>The reaction of the <i>N</i>,<i>N</i>-diethyl-<i>N'</i>-(<i>p</i>-nitrobenzoyl)thiourea with K₂[PtCl₄] results in the complex of configurational <i>cis</i>-[Pt(L-<i>kS</i>,<i>O</i>)₂], and structurally characterized by elemental analyses, FT-IR, ¹H NMR, ¹³H NMR, UV–Vis spectroscopy, and <i>cis</i>-[Pt(L-<i>kS</i>,<i>O</i>)₂] complex have been also characterized by a single-crystal X-ray diffraction study. The <i>cis</i>-[Pt(L-<i>kS</i>,<i>O</i>)₂] crystallizes in the monoclinic crystal system, space group <i>P</i>2₁/<i>c</i>, with <i>Z</i> = 4, and unit cell parameters, <i>a</i> = 15.09299(15) Å, <i>b</i> = 15.26600(14) Å, <i>c</i> = 14.39268(14) Å, <i>α</i> = 90°, <i>β</i> = 107.6347(11)° and <i>γ</i> = 90°. The single-crystal diffraction analysis of the complex shows that the molecular configuration of <i>cis</i>-[Pt(L-<i>kS</i>,<i>O</i>)₂] is a slightly distorted square-planar geometry, and both deprotonated ligands (L) contribute one O atom and one S atom coordinate with a central Pt(II) ion. The intermolecular interactions in the <i>cis</i>-[Pt(L-<i>kS</i>,<i>O</i>)₂] complex were analyzed using the Hirshfeld surface method, including 2D fingerprint plots. In addition, the fluorescence properties of the compounds at room temperature were also studied. The results show that both ligands and complexes have good fluorescence properties, and the fluorescence intensity of the coordination compound enhances.</p><h3>Graphical Abstract</h3><p>In this paper, single-crystal X-ray analysis shows <i>cis</i>-[Pt(L-<i>kS</i>,<i>O</i>)₂] belongs to monoclinic crystal system, space group <i>P</i>2₁/<i>c</i>. The connectivity of the ligand to the metal as 2:1 and the platinum atom is coordinated with two <i>N</i>,<i>N</i>-diethyl-<i>N'</i>-(<i>p</i>-nitrobenzoyl)thiourea ligands in a distorted square-planar geometry.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 3","pages":"357 - 369"},"PeriodicalIF":0.8,"publicationDate":"2022-12-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00976-8.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4890637","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal Structure Analysis of 4-Oxo, 4-hydroxy- and 4-alkyl-7-bromopyrazolo[5,1-c][1,2,4]triazines","authors":"Sergey M. Ivanov,&nbsp;Denis S. Koltun","doi":"10.1007/s10870-022-00973-x","DOIUrl":"10.1007/s10870-022-00973-x","url":null,"abstract":"<div><p>The crystal structures of 8-R¹-7-bromo-3-<i>tert</i>-butyl-1-R²-pyrazolo[5,1-<i>c</i>][1,2,4]triazin-4(1<i>H</i>)-ones <b>1a–c, 2a,c</b> (R¹ = CN, CO₂Et, NO₂, R² = H, 1:1 and 3:1 solvates with DMSO; R¹ = CN, CO₂Et, R² = CH₂Boc), 8-R¹-7-bromo-3-<i>tert</i>-butyl-1-R²-1,4-dihydropyrazolo[5,1-<i>c</i>][1,2,4]triazin-4-ols <b>3a,b</b> (R¹ = CN, R² = <i>n</i>-Bu; R¹ = Br, R² = CH₂Boc), 1,4-dihydro- and aromatic 7-R³-3-<i>tert</i>-butyl-4-R⁴-8-methylpyrazolo[5,1-<i>c</i>][1,2,4]triazines <b>5a,b, 6</b> (R³ = H, R⁴ = <i>n</i>-Pr; R³ = Br, R⁴ = <i>n</i>-Bu) were investigated by X-ray diffraction analysis. The structural preferences and different packing modes based on the intermolecular interactions were analyzed by the Hirshfeld surface and energy framework analysis.</p><h3>Graphical Abstract</h3><p>The crystal structures of ten 3-<i>tert</i>-butyl-4-oxo, 4-hydroxy- and 4-alkyl-7-bromopyrazolo[5,1-c][1,2,4]triazines including non-solvated, 1:1 and 3:1 solvates with DMSO were investigated by single crystal X-ray diffraction, Hirshfeld surface and energy framework analyses.</p><figure><div><div><div><picture><source><img></source></picture></div></div></div></figure></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 3","pages":"345 - 356"},"PeriodicalIF":0.8,"publicationDate":"2022-12-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00973-x.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4968370","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Two New Proton Transfer Salts of Benzo[d]thiazol-2-amine with Different Aromatic Acids","authors":"Nurgün Büyükkıdan,&nbsp;Halil İlki̇men,&nbsp;Seher Kaya,&nbsp;Musa Sarı,&nbsp;Aysel Gülbandılar","doi":"10.1007/s10870-022-00974-w","DOIUrl":"10.1007/s10870-022-00974-w","url":null,"abstract":"<div><p>Two new proton transfer salts (HABT)⁺(SA)⁻ (<b>1</b>) and (HABT)⁺₂(ADSA)²⁻·2H₂O (<b>2</b>) were synthesized from the reaction of benzo[d]thiazol-2-amine (2-aminobenzothiazole) (ABT) with 2-hydroxybenzoic acid (salicylic acid) (HSA) and 2-aminobenzene-1,4-disulfonic acid (H₂ADSA), respectively. The molecular structures of these salts were carried out by elemental analysis, X-ray diffraction crystallography, FTIR and UV–Vis techniques Single-crystal X-ray analysis of the compounds revealed proton transfer from acidic moieties to basic moieties to form salts with intermolecular hydrogen bond motifs R₂²(8) for <b>1</b> and R₃³(10) for <b>2</b>. The intramolecular hydrogen bond creates the cyclic S(6) motif in both structures (<b>1</b> and <b>2</b>). For salt <b>1</b>, crystallization took place in the P2(1)/c space group of the monoclinic system, and for salt <b>2</b> in the P-1 space group of the triclinic system. The antibacterial and antifungal properties of the compounds are assayed against various Gram positive bacteria {<i>Bacillus subtilis</i>, <i>Listeria monocytogenes</i> (ATCC 7644), <i>Enterococcus faecalis</i> (ATCC 29212), <i>Staphylococcus aureus</i> (NRRL B-767)}, Gram negative bacteria {<i>Escherichia coli</i> (ATCC 25922), <i>Pseudomonas aeruginosa</i> (ATCC 27853)} and fungus {<i>Candida albicans</i> (F89)}. Minimum inhibitory concentrations (MIC) of synthesized salts were compared with antibacterial (levofloxacin cefepime, vancomycin) and antifungal (Fluconazole) reference compounds.</p><h3>Graphical Abstract</h3>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 2","pages":"336 - 344"},"PeriodicalIF":0.8,"publicationDate":"2022-12-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4671681","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis, Structural Characterization, Hirshfeld Analysis and AIM Analysis of 2,4,8,10-tetra-tert-butyl-6-phenyldibenzo[d,g][1,3,6,2]-dioxa-selenaphosphocine and its Oxide and Selenide Derivatives","authors":"Pawan Kumar,&nbsp;Dipanjan Mondal,&nbsp;Harish S. Kunchur,&nbsp;Joel T. Mague,&nbsp;Maravanji S. Balakrishna","doi":"10.1007/s10870-022-00972-y","DOIUrl":"10.1007/s10870-022-00972-y","url":null,"abstract":"&lt;div&gt;&lt;p&gt;The reaction of 2,2′-selenobis(4,6-di-&lt;i&gt;tert&lt;/i&gt;-butyl phenol) with equimolar amount of dichlorophenylphosphine afforded the 8-membered cyclic phosphonite, PhP{-OC&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;2&lt;/sub&gt;(&lt;sup&gt;&lt;i&gt;t&lt;/i&gt;&lt;/sup&gt;Bu)&lt;sub&gt;2&lt;/sub&gt;(&lt;i&gt;µ&lt;/i&gt;-Se)(&lt;sup&gt;&lt;i&gt;t&lt;/i&gt;&lt;/sup&gt;Bu)&lt;sub&gt;2&lt;/sub&gt;C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;2&lt;/sub&gt;O&lt;b&gt;-&lt;/b&gt;} (&lt;b&gt;1&lt;/b&gt;). The reaction of &lt;b&gt;1&lt;/b&gt; with 30% aq H&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;2&lt;/sub&gt; resulted in the oxidation of both phosphorus and selenium to give PhP(O){-OC&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;2&lt;/sub&gt;(&lt;sup&gt;&lt;i&gt;t&lt;/i&gt;&lt;/sup&gt;Bu)&lt;sub&gt;2&lt;/sub&gt;(&lt;i&gt;µ&lt;/i&gt;-Se(O))(&lt;sup&gt;&lt;i&gt;t&lt;/i&gt;&lt;/sup&gt;Bu)&lt;sub&gt;2&lt;/sub&gt;C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;2&lt;/sub&gt;O&lt;b&gt;-&lt;/b&gt;} (&lt;b&gt;2&lt;/b&gt;) in quantitative yield. Similar reaction of &lt;b&gt;1&lt;/b&gt; with one equivalent of trimethylamine-&lt;i&gt;N&lt;/i&gt;-oxide yielded the phosphine oxide derivative, PhP(O){-OC&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;2&lt;/sub&gt;(&lt;sup&gt;&lt;i&gt;t&lt;/i&gt;&lt;/sup&gt;Bu)&lt;sub&gt;2&lt;/sub&gt;(&lt;i&gt;µ&lt;/i&gt;-Se)(&lt;sup&gt;&lt;i&gt;t&lt;/i&gt;&lt;/sup&gt;Bu)&lt;sub&gt;2&lt;/sub&gt;C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;2&lt;/sub&gt;O&lt;b&gt;-&lt;/b&gt;} (&lt;b&gt;3&lt;/b&gt;). The reaction of &lt;b&gt;1&lt;/b&gt; with gray selenium in 1:1 molar ratio afforded PhP(Se){-OC&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;2&lt;/sub&gt;(&lt;sup&gt;&lt;i&gt;t&lt;/i&gt;&lt;/sup&gt;Bu)&lt;sub&gt;2&lt;/sub&gt;(&lt;i&gt;µ&lt;/i&gt;-Se)(&lt;sup&gt;&lt;i&gt;t&lt;/i&gt;&lt;/sup&gt;Bu)&lt;sub&gt;2&lt;/sub&gt;C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;2&lt;/sub&gt;O&lt;b&gt;-&lt;/b&gt;} (&lt;b&gt;4&lt;/b&gt;) in good yield. All the derivatives have been structurally characterized. Both the compounds &lt;b&gt;2&lt;/b&gt; and &lt;b&gt;3&lt;/b&gt; crystallized with the asymmetric unit containing a whole molecule, whereas the compound &lt;b&gt;4&lt;/b&gt; crystallized with a CH&lt;sub&gt;2&lt;/sub&gt;Cl&lt;sub&gt;2&lt;/sub&gt; molecule. All of these molecules showed intermolecular C−H⋅⋅⋅O and C−H⋅⋅⋅Se hydrogen bonding interactions which play major role in the crystal packing to form a three-dimensional array. Hirshfeld surface analysis, d&lt;sub&gt;norm&lt;/sub&gt; and two-dimensional fingerprint plots were investigated to validate the contributions of the different intermolecular contacts within the supramolecular structure. A Hirshfeld surface analysis indicated that the most significant contributions to the crystal packing of &lt;b&gt;2&lt;/b&gt; are from H⋅⋅⋅H (72%), C⋅⋅⋅H/H⋅⋅⋅C (15%), O⋅⋅⋅H/H⋅⋅⋅O (10.1%) and Se⋅⋅⋅H/H⋅⋅⋅Se (2.8%) contacts, and those for &lt;b&gt;3&lt;/b&gt; are from H⋅⋅⋅H (74.1%), C⋅⋅⋅H/H⋅⋅⋅C (14.2%), O⋅⋅⋅H/H⋅⋅⋅O (5.7%) and Se⋅⋅⋅H/H⋅⋅⋅Se (5.7%) contacts, while those for &lt;b&gt;4&lt;/b&gt; are from H⋅⋅⋅H (75.9%), C⋅⋅⋅H/H⋅⋅⋅C (10.5%), O⋅⋅⋅H/H⋅⋅⋅O (1%) and Se⋅⋅⋅H/H⋅⋅⋅Se (12.5%) contacts. Non-covalent interactions between C–H and O were observed in the molecular structures of &lt;b&gt;2&lt;/b&gt;–&lt;b&gt;4&lt;/b&gt;. These weak interactions were also assessed by DFT calculations in terms of their non-covalent interaction plots and QTAIM analysis.&lt;/p&gt;&lt;h3&gt;Graphical Abstract&lt;/h3&gt;&lt;p&gt;This paper describes the synthesis and crystal structures of three\u0000selenaphosphocine derivatives. The reaction of 2,2′-selenobis(4,6-di-&lt;i&gt;tert&lt;/i&gt;-butyl phenol) with equimolar amount of dichlorophenylphosphine produce the 8-membered cyclic phosphonite &lt;b&gt;1&lt;/b&gt;. The reaction of &lt;b&gt;1&lt;/b&gt; with 30% aq H&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;2&lt;/sub&gt; and elemental selenium afford three different macrocyclic compounds.&lt;/p&gt;\u0000 &lt;figure&gt;&lt;div&gt;&lt;div&gt;&lt;d","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 2","pages":"321 - 335"},"PeriodicalIF":0.8,"publicationDate":"2022-12-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4372630","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Obituary","authors":"Ray Butcher","doi":"10.1007/s10870-022-00971-z","DOIUrl":"10.1007/s10870-022-00971-z","url":null,"abstract":"","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"52 4","pages":"407 - 408"},"PeriodicalIF":0.8,"publicationDate":"2022-11-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4627369","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis and Crystal Structure of an Adjoined Metallacrown: An Archetypal 12-Metallacrown-4 Connected to a Collapsed 11-Metallacrown-4","authors":"Jordan C. Scalia,&nbsp;Matthias Zeller,&nbsp;Curtis M. Zaleski","doi":"10.1007/s10870-022-00968-8","DOIUrl":"10.1007/s10870-022-00968-8","url":null,"abstract":"<div><p>The adjoined 3<i>d</i>–4<i>f</i> metallacrown (MC) molecule Dy^III₂Mn^III₆(H₂shi)(Hshi)(shi)₇(py)₉·2py·0.7H₂O, <b>1</b>, where H₃shi is salicylhydroxamic acid and py is pyridine, has been synthesized and characterized by FT–IR spectroscopy and single-crystal X-ray diffraction. The core of the molecule consists of two metallacrown (MC) rings, an archetypal 12-MC-4 and a collapsed 11-MC-4, that are linked through a common ring Dy^III center. For the 12-MC-4 portion of <b>1</b>, the heterobimetallic composition of the MC ring with one Dy^III and three Mn^III ions is uncommon for metallacrowns as most 12-MC-4 rings are homometallic. In addition, the 12-MC-4 binds a Dy^III cation in the central cavity of the MC. The coordination environment about the central Dy^III ion has a triangular dodecahedron shape, which again is atypical. For 12-MC-4 molecules with a central lanthanide ion, the central lanthanide ion typically adopts a square antiprism geometry. The ring Dy^III cation of the 12-MC-4, which has a biaugmented trigonal prism shape, is shared with the collapsed 11-MC-4 and serves to join both metallacrowns. The collapsed 11-MC-4 ring is also composed of three Mn^III and one Dy^III ions. For one of the ring metal–metal linkages, only an oxygen atom is present, and an eleven membered ring is generated. In addition, the Dy^III center and one of the Mn^III centers bind to ring oxygen atoms on the opposite side of the MC ring; thus, the potential cavity of the MC is collapsed, and the MC does not bind a central metal ion as is customary.</p><h3>Graphical Abstract</h3>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 2","pages":"307 - 320"},"PeriodicalIF":0.8,"publicationDate":"2022-11-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4512180","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Supramolecular Complexes Built of Octahedral [Ta6Cl12(CN)6]3−/4− Clusters and Terpyridine-Metal Complexes","authors":"Jian-Jun Zhang,&nbsp;H. Andrew Zhou,&nbsp;Abdessadek Lachgar","doi":"10.1007/s10870-022-00969-7","DOIUrl":"10.1007/s10870-022-00969-7","url":null,"abstract":"<div><p>The preparation and characterization of two supramolecular complexes from octahedral [Ta₆Cl₁₂(CN)₆]^4−/3− units and 2, 2′: 6′, 2″-terpyridine (<i>Terpy</i>) metal complexes as building blocks are reported. Single crystal analyses revealed [Mn(<i>Terpy</i>)]₂[Ta₆Cl₁₂(CN)₆]·MeOH (<b>1</b>) features a neutral two-dimensional (2D) framework composed of layers based on [Ta₆Cl₁₂(CN)₆]⁴⁻ and [Mn(<i>Terpy</i>)]²⁺. Each layer is built of 6-connected [Ta₆Cl₁₂]²⁺ and 3-connected Mn(II) nodes bridged by cyanide ligands. The layers are held together by MeOH molecules. The layered structure is maintained after the removal of solvent molecule (MeOH) upon heating, leading to the formation of [Mn(<i>Terpy</i>]₂[Ta₆Cl₁₂(CN)₆] (<b>1′</b>). In the case of using Gd³⁺, the resultant product was revealed by single-crystal analyses to be an ionic compound [Gd(<i>Terpy</i>)(H₂O)₄(DMF)₂][Ta₆Cl₁₂(CN)₆]⋅DMF ⋅3H₂O (<b>2</b>). <b>2</b> has a three-dimensional (3D) framework built of [Gd(<i>Terpy</i>)(H₂O)₄(DMF)₂]³⁺ and [Ta₆Cl₁₂(CN)₆]³⁻ ions connected to each other via extensive hydrogen bonds and π-π interactions between the cations, anions, and solvent molecules. Thermal stabilities of <b>1</b>‒<b>2</b> are reported.</p><h3>Graphical Abstract</h3><p>The X-ray structures and thermal stabilities of a coordination polymer [Mn(<i>Terpy</i>)]₂[Ta₆Cl₁₂(CN)₆] ⋅MeOH and an ionic compound [Gd(<i>Terpy</i>)(H₂O)₄(DMF)₂][Ta₆Cl₁₂(CN)₆]⋅DMF⋅3H₂O are presented.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 2","pages":"299 - 306"},"PeriodicalIF":0.8,"publicationDate":"2022-11-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4402277","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Two Different Compounds in One Crystal: di-μ-chlorobis[2-(5-methyl-pyridin-2-yl-κN)phenyl-κC(1)]diplatinum(II) and chloro(N,N-dimethylformamide-κO)[2-(5-methyl-pyridin-2-yl-κN)phenyl-κC(1)]platinum(II)","authors":"Isabelle Sasaki,&nbsp;Sonia Mallet-Ladeira","doi":"10.1007/s10870-022-00970-0","DOIUrl":"10.1007/s10870-022-00970-0","url":null,"abstract":"<div><p>The crystal structures of di-μ-chlorobis[2-(5-methyl-pyridin-2-yl-κN)phenyl-κC(1)] diplatinum(II) <b>(1)</b> and chloro(N,N-dimethylformamide-κO)[2-(5-methyl-pyridin-2-yl-κN)phenyl-κC(1)]platinum(II) <b>(2)</b> have been determined by means of the X-ray diffraction. Both complexes cocrystallize in the monoclinic space group C2/c with <i>a</i> = 39.5457(18) Å, <i>b</i> = 7.2482(4) Å, <i>c</i> = 21.2269(10) Å and β = 121.460(2)°. The asymmetric unit consists of half a centrosymmetric compound (complex <b>1</b>) and one full independent compound (complex <b>2</b>).</p><h3>Graphical Abstract</h3><p>The X-ray structures of co-crystallized di-μ-chlorobis[2-(5-methyl-pyridin-2-yl-κN)phenyl-κC(1)]diplatinum(II) <b>(1)</b> as starting material and of the derivative chloro(N,N-dimethylformamide-κO)[2-(5-methyl-pyridin-2-yl-κN)phenyl-κC(1)]platinum(II) <b>(2)</b> are reported.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 2","pages":"293 - 298"},"PeriodicalIF":0.8,"publicationDate":"2022-11-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00970-0.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4276019","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis, Structural Characterization and Hirshfeld Analysis of Ag(I), Au(I), Cd(II) and Hg(II) Complexes Containing Hemilabile- Ferrocenylbisphosphine [Fe{C5H4P(C6H4CH2NMe2-o)2}2]","authors":"Dipanjan Mondal,&nbsp;Sowmya Rao,&nbsp;Joel T. Mague,&nbsp;Maravanji S. Balakrishna","doi":"10.1007/s10870-022-00966-w","DOIUrl":"10.1007/s10870-022-00966-w","url":null,"abstract":"&lt;div&gt;&lt;p&gt;The reaction between bis(phosphino)ferrocene, [Fe{C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;P(C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;CH&lt;sub&gt;2&lt;/sub&gt;NMe&lt;sub&gt;2&lt;/sub&gt;-&lt;i&gt;o&lt;/i&gt;)&lt;sub&gt;2&lt;/sub&gt;}&lt;sub&gt;2&lt;/sub&gt;] (&lt;b&gt;1&lt;/b&gt;) and AgOTf resulted in disilver complex [(AgOTf)&lt;sub&gt;2&lt;/sub&gt;{µ-Fe{C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;P(C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;CH&lt;sub&gt;2&lt;/sub&gt;NMe&lt;sub&gt;2&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;}&lt;sub&gt;2&lt;/sub&gt;}] (&lt;b&gt;2&lt;/b&gt;) which on further treatment with 2,2′-bipyrdine yielded a mixed-ligand complex [Ag&lt;sub&gt;2&lt;/sub&gt;(bipy)&lt;sub&gt;2&lt;/sub&gt;{µ-Fe{C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;P(C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;CH&lt;sub&gt;2&lt;/sub&gt;NMe&lt;sub&gt;2&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;}&lt;sub&gt;2&lt;/sub&gt;}](OTf)&lt;sub&gt;2&lt;/sub&gt; (&lt;b&gt;3&lt;/b&gt;). Reaction of &lt;b&gt;1&lt;/b&gt; with AuCl(SMe&lt;sub&gt;2&lt;/sub&gt;) in 1:2 molar ratio afforded a digold complex [(AuCl)&lt;sub&gt;2&lt;/sub&gt;Fe{C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;P(C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;CH&lt;sub&gt;2&lt;/sub&gt;NMe&lt;sub&gt;2&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;}&lt;sub&gt;2&lt;/sub&gt;] (&lt;b&gt;4&lt;/b&gt;). Treatment of &lt;b&gt;4&lt;/b&gt; with anhydrous CdCl&lt;sub&gt;2&lt;/sub&gt; resulted in heterometallic complex [Fe{C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;P(AuCl)(C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;CH&lt;sub&gt;2&lt;/sub&gt;NMe&lt;sub&gt;2&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;(CdCl&lt;sub&gt;2&lt;/sub&gt;)}&lt;sub&gt;2&lt;/sub&gt;] (&lt;b&gt;5&lt;/b&gt;). The reactions of &lt;b&gt;1&lt;/b&gt; with anhydrous CdI&lt;sub&gt;2&lt;/sub&gt; and HgI&lt;sub&gt;2&lt;/sub&gt; in 1:2 molar ratios yielded bimetallic complexes [Fe{C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;P(CdI&lt;sub&gt;2&lt;/sub&gt;)(C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;CH&lt;sub&gt;2&lt;/sub&gt;NMe&lt;sub&gt;2&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;}&lt;sub&gt;2&lt;/sub&gt;] (&lt;b&gt;6&lt;/b&gt;) and [Fe{C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;P(HgI&lt;sub&gt;2&lt;/sub&gt;)(C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;CH&lt;sub&gt;2&lt;/sub&gt;NMe&lt;sub&gt;2&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;}&lt;sub&gt;2&lt;/sub&gt;] (&lt;b&gt;7&lt;/b&gt;), respectively. The molecular structures of &lt;b&gt;3&lt;/b&gt;, &lt;b&gt;4&lt;/b&gt; and &lt;b&gt;7&lt;/b&gt; were confirmed by single crystal X-ray analysis. Complexes &lt;b&gt;3&lt;/b&gt; and &lt;b&gt;7&lt;/b&gt; crystallized in the triclinic space group with P-1, whereas &lt;b&gt;4&lt;/b&gt; crystallized in the monoclinic space group with C2/c. Single crystals suitable for X-ray crystallography were obtained using diffusion method where a solution of [Fe{C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;P(C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;CH&lt;sub&gt;2&lt;/sub&gt;NMe&lt;sub&gt;2&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;}&lt;sub&gt;2&lt;/sub&gt;] (&lt;b&gt;1&lt;/b&gt;) in dichloromethane was layered on a solution of CdI&lt;sub&gt;2&lt;/sub&gt; and HgI&lt;sub&gt;2&lt;/sub&gt; in methanol and stored at room temperature for 24 h, resulted in yellow plates of &lt;b&gt;6&lt;/b&gt; and &lt;b&gt;7&lt;/b&gt;, respectively. All complexes crystallized with the asymmetric unit containing half a molecule and with the Fe atom on an inversion centre. A Hirshfeld surface analysis indicated that the most significant contributions to the crystal packing of &lt;b&gt;3&lt;/b&gt; are from H‧‧‧H (50.2%), C‧‧‧H/H‧‧‧C (8.3%), Cl‧‧‧H/H‧‧‧Cl (12.1%), O‧‧‧H/H‧‧‧O (11.3%), F‧‧‧H/H‧‧‧F (9.0%) contacts, while those for &lt;b&gt;4&lt;/b&gt; are from H‧‧‧H (73.7%), C‧‧‧H/H‧‧‧C (8.9%), Cl‧‧‧H/H‧‧‧Cl (14.5%), Au‧‧‧H/H‧‧‧Au (1.8%) and N‧‧‧H/H‧‧‧N (0.8%) contacts, and those for &lt;b&gt;7&lt;/b&gt; are from H‧‧‧H (65.5%), C‧‧‧H/H‧‧‧C (6.6%), I‧‧‧H/H‧‧‧I (24.1%) and I‧‧‧C/C‧‧‧I (2.9%) contacts.&lt;/p&gt;&lt;h3&gt;Graphical Abstract&lt;/h3&gt;&lt;p&gt;\u0000 Crystal structures of silver(I), gold(I) and mercury(II) complexes containing [Fe{C&lt;sub&gt;5&lt;/sub&gt;H&lt;s","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 2","pages":"273 - 292"},"PeriodicalIF":0.8,"publicationDate":"2022-10-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00966-w.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"5102165","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Crystal structure and solid-state luminescence properties of [Tb(H2O)9]Cl(C10H6O4S4)2 (C10H6O4S42− = 2,6-naphthalenedisulfonate)","authors":"Ming-Qing Liu,&nbsp;Wen-Tong Chen,&nbsp;Lijun Wei,&nbsp;Qiu-Yue Zhong,&nbsp;Chuan-Kang Yin,&nbsp;Xiu-Guang Yi","doi":"10.1007/s10870-022-00963-z","DOIUrl":"10.1007/s10870-022-00963-z","url":null,"abstract":"<div><p>A terbium 2,6-naphthalenedisulfonic acid compound, [Tb(H₂O)₉]Cl(C₁₀H₆O₄S₄)₂ (C₁₀H₆O₄S₄²⁻ = 2,6-naphthalenedisulfonate), is prepared and characterized by single-crystal X-ray diffraction. This compound is characterized by an isolated structure with the terbium ion possessing a mono-capped square antiprism coordination geometry. The [Tb(H₂O)₉]³⁺ cations and (2,6-naphthalenedisulfonic acid)²⁻ anions are linked by hydrogen-bonding interactions to yield a three-dimensional supramolecular network. The solid state luminescence spectrum reveals that this compound shows the strongest emission band in the red region. The luminescence emission peaks can be ascribed to the characteristic emissions of the 4<i>f</i> electron intrashell transitions ⁵<i>D</i>₄ → ⁷<i>F</i>₅, ⁵<i>D</i>₄ → ⁷<i>F</i>₄ and ⁵<i>D</i>₄ → ⁷<i>F</i>₂ of the Tb³⁺ ion. The CIE (Commission Internationale de L’Eclairage) chromaticity coordinates are (0.5647, 0.4338). Solid-state UV/Vis diffuse reflectance spectra reveal that compound <b>1</b> shows a wide optical band gap of 4.92 eV.</p><h3>Graphical abstract</h3><p>A novel terbium 2,6-naphthalenedisulfonic acid compound is prepared and characterized</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 2","pages":"266 - 272"},"PeriodicalIF":0.8,"publicationDate":"2022-10-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"5019779","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}