Journal of Chemical Crystallography最新文献

{"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, Sowmya Rao, Joel T. Mague, Maravanji S. Balakrishna","doi":"10.1007/s10870-022-00966-w","DOIUrl":"10.1007/s10870-022-00966-w","url":null,"abstract":"<div><p>The reaction between bis(phosphino)ferrocene, [Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>-<i>o</i>)<sub>2</sub>}<sub>2</sub>] (<b>1</b>) and AgOTf resulted in disilver complex [(AgOTf)<sub>2</sub>{µ-Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>}] (<b>2</b>) which on further treatment with 2,2′-bipyrdine yielded a mixed-ligand complex [Ag<sub>2</sub>(bipy)<sub>2</sub>{µ-Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>}](OTf)<sub>2</sub> (<b>3</b>). Reaction of <b>1</b> with AuCl(SMe<sub>2</sub>) in 1:2 molar ratio afforded a digold complex [(AuCl)<sub>2</sub>Fe{C<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>4</b>). Treatment of <b>4</b> with anhydrous CdCl<sub>2</sub> resulted in heterometallic complex [Fe{C<sub>5</sub>H<sub>4</sub>P(AuCl)(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>(CdCl<sub>2</sub>)}<sub>2</sub>] (<b>5</b>). The reactions of <b>1</b> with anhydrous CdI<sub>2</sub> and HgI<sub>2</sub> in 1:2 molar ratios yielded bimetallic complexes [Fe{C<sub>5</sub>H<sub>4</sub>P(CdI<sub>2</sub>)(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>6</b>) and [Fe{C<sub>5</sub>H<sub>4</sub>P(HgI<sub>2</sub>)(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>7</b>), respectively. The molecular structures of <b>3</b>, <b>4</b> and <b>7</b> were confirmed by single crystal X-ray analysis. Complexes <b>3</b> and <b>7</b> crystallized in the triclinic space group with P-1, whereas <b>4</b> 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<sub>5</sub>H<sub>4</sub>P(C<sub>6</sub>H<sub>4</sub>CH<sub>2</sub>NMe<sub>2</sub>)<sub>2</sub>}<sub>2</sub>] (<b>1</b>) in dichloromethane was layered on a solution of CdI<sub>2</sub> and HgI<sub>2</sub> in methanol and stored at room temperature for 24 h, resulted in yellow plates of <b>6</b> and <b>7</b>, 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 <b>3</b> 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 <b>4</b> 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 <b>7</b> 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.</p><h3>Graphical Abstract</h3><p>\u0000 Crystal structures of silver(I), gold(I) and mercury(II) complexes containing [Fe{C<sub>5</sub>H<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}

{"title":"Polynuclear Cyanide-Bridged Heterobimetallic Complexes Based-on Pentacyanometallates: Synthesis, Crystal Structure and Magnetic Property","authors":"Yu Xin,&nbsp;Zhijie Xu,&nbsp;Shuo Meng,&nbsp;Tong Cao,&nbsp;Mingjian Zhang,&nbsp;Xiaoyi Duan,&nbsp;Zhen Zhou,&nbsp;Daopeng Zhang","doi":"10.1007/s10870-022-00967-9","DOIUrl":"10.1007/s10870-022-00967-9","url":null,"abstract":"<div><p>Three new cyanide-bridged heterobimetallic complexes {[Cu(L)]₂[Cr(CN)₅(NO)]}ClO₄·2H₂O (1), {{[Cu(cyclam)][Fe(CN)₅(NO)]}·H₂O}_n (2), {{[Cu(cyclam)]₃[Cr(CN)₅(NO)]₂}·CH₃OH·4H₂O}_n (3) (L=2,12-dimethyl-3,7,11,17-tetraazabicyclo [11.3.1] heptadeca-1 (17), 13, 15-triene, cyclam=1,4,8,11-tetraazacyclodecane) have been successfully assembled from the pentacyanometalates and two copper(II) compounds and characterized by elemental analysis, IR spectroscopy and X-ray structure determination. X-ray structural analysis revealed that the Complex 1 is a cationic trinuclear CrCu₂ entity with the positive charge balanced by ClO₄⁻ ion, while complexes 2 and 3 were structurally characterized showing a 1D chain. The magnetic properties of the reported cyanide-bridged complexes have been experimentally studied and theoretically simulated, disclosing the ferromagnetic interaction between the Cr(I) ion and the Cu(II) ion through the cyanide bridge.</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":"256 - 265"},"PeriodicalIF":0.8,"publicationDate":"2022-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"5105462","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, Characterizations, Crystal Structure, DFT, and Hirshfeld Surface Analysis of 4-Cyclohexyl-1-(thiophene-2-carbonyl)thiosemicarbazide","authors":"Shivendra Kumar Pandey,&nbsp;Seema Gupta,&nbsp;Shubham Jaiswal,&nbsp;M. K. Gond,&nbsp;M. K. Bharty,&nbsp;R. J. Butcher","doi":"10.1007/s10870-022-00965-x","DOIUrl":"10.1007/s10870-022-00965-x","url":null,"abstract":"<div><p>The crystal structure of the thiosemicarbazide derivative 4-cyclohexyl-1-(thiophene-2-carbonyl)thiosemicarbazide (ChtcTSC), C₁₂H₁₇N₃OS₂, is reported here. The title compound ChtcTSC has been characterized by various physicochemical techniques viz UV–Vis., Infrared, and NMR. It crystallizes in the monoclinic system having space group P2₁/c. The dihedral angle between the thiophene and cyclohexyl rings is 60.7(4)^°. The crystal packing is established by intermolecular N–H⋯O packing interactions involving a three-center donor hydrogen bond between the keto oxygen atom of the thiophene group and H atoms belonging to the hydrazine group which links the molecules into chains along the (011) plane of the unit cell. Hydrogen bonds between the hydrazine hydrogen atom and one of the thiophene groups and C–H⋯Cg π -ring interactions provide added stability to the crystal packing. The fingerprint plots associated with Hirshfeld surface analysis indicate that there are different types of weak interactions viz<i>.</i> O⋯H–C, O⋯H–N, and S⋯H–C. The geometry optimization has been performed using the DFT method, and geometrical parameters thus obtained for ChtcTSC correlate with the single-crystal X-ray data. The TD-DFT study showed a small HOMO and LUMO energy gap of 2.869 eV. The electronic transition from the ground state to the excited state due to a transfer of electrons from HOMO to LUMO levels is mainly associated with the n → π* transition.</p><h3>Graphical Abstract</h3><p>The crystal structure of 4-cyclohexyl-1-(thiophene-2-carbonyl)thiosemicarbazide (ChtcTSC) is reported here where the title compound ChtcTSC has been characterized by various physiochemical techniques including UV–Vis., Infrared, NMR, DFT and Hirshfeld surface analysis.</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":"244 - 255"},"PeriodicalIF":0.8,"publicationDate":"2022-10-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4558329","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":"Self-assembly of Hybrid Solids {Hpz}2[H7CrMo6O24]·6H2O and [Co(2-Hampz)2Cl4] (pz = pyrazole, 2-ampz = 2-aminopyrazine) from Aqueous Solution","authors":"Memsy Chiriamkandath Kuriakose,&nbsp;Jisha Joseph,&nbsp;Glinta Mandumpal Joyson,&nbsp;Jency Thomas","doi":"10.1007/s10870-022-00964-y","DOIUrl":"10.1007/s10870-022-00964-y","url":null,"abstract":"<div><p>Two new hybrid solids viz<i>.</i> {H<i>pz</i>}₂[H₇CrMo₆O₂₄]·6H₂O (<b>1</b>) and [Co(2-H<i>ampz</i>)₂Cl₄] (<b>2</b>) have been crystallized via solvent evaporation technique using pyrazole (<i>pz</i>) and 2-aminopyrazine (2-<i>ampz</i>) respectively. The solids were characterized using single crystal X-ray diffraction, fourier transform infrared spectroscopy, elemental analysis, scanning electron microscopy and thermal analysis. The solid <b>1</b> crystallized in orthorhombic system with space group <i>Pbca</i>, <i>a</i> = 23.1796(8), <i>b</i> = 11.1281(4), <i>c</i> = 25.1499(9) Å, Z = 8. The solid <b>2</b> crystallized in triclinic system with space group <i>P-</i>1, <i>a</i> = 7.1986(5), <i>b</i> = 7.3917(5), <i>c</i> = 7.8896(6) Å, <i>α</i> = 115.758(3), <i>β</i> = 110.450(3), <i>γ</i> = 96.904(3)°, Z = 1. While, solid <b>1</b> is a new Anderson–Evans cluster based solid, <b>2</b> is a new pseudopolymorph of cobalt complex [Co(2-<i>ampz</i>)₄Cl₂]. Crystal structure analysis suggested that supramolecular interactions facilitate the crystal packing in solids <b>1</b> and <b>2</b>. In addition, the role of synthetic parameters in dictating the nature of self-assembly of solids <b>1</b> and <b>2</b> in aqueous medium has also been analyzed.</p><h3>Graphical Abstract</h3><p>An Anderson–Evans cluster based solid, {H<i>pz</i>}₂[H₇CrMo₆O₂₄]·6H₂O (<b>1</b>) and a new pseudopolymorph of cobalt complex [Co(2-<i>ampz</i>)₄Cl₂] viz<i>.</i> [Co(2-H<i>ampz</i>)₂Cl₄] (<b>2</b>) have been synthesized using pyrazole (<i>pz</i>) and 2-aminopyrazine (2-<i>ampz</i>) respectively.</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":"236 - 243"},"PeriodicalIF":0.8,"publicationDate":"2022-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4058051","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 Analysis of NH4[Zn(cma)(H2O)2]·H2O Using IAM and HAR Approaches","authors":"Jana Chrappová,&nbsp;Yogeswara Rao Pateda,&nbsp;Erik Rakovský","doi":"10.1007/s10870-022-00961-1","DOIUrl":"10.1007/s10870-022-00961-1","url":null,"abstract":"<div><p>The crystal structure of NH₄[Zn(<i>cma</i>)(H₂O)₂]·H₂O (<i>cma</i>^3– = N-carboxymethylaspartate(3–)) is determined by single crystal X-ray structure analysis. The orthorombic crystals (<i>P</i>2₁2₁2₁, <i>a</i> = 7.7901(4) Å, <i>b</i> = 11.2368(4) Å, <i>c</i> = 13.2048(5) Å, <i>α</i> = <i>β</i> = <i>γ</i> = 90°, <i>Z</i> = 4) were obtained from the reaction mixture in the form of racemic conglomerate. The single crystal X-ray structure analysis revealed the maximum deviation of bond angles around the Zn atom from an ideal octahedral geometry 14.09° with <i>∑</i> = 67.23° and <i>Θ</i> = 236.69°. Intermolecular interactions are based mainly on a moderate N–H⋯O and O–H⋯O hydrogen bonds. The structure shares similar structural features with other structures containing aspartates and their derivatives as a ligands. The results of using different HAR methods based on semi-empirical (B3LYP) and non-empirical (PBE0) global hybrid GGA DFT functionals were compared.</p><h3>Graphical Abstract</h3><p>The crystal structure of NH₄[Zn(<i>cma</i>)(H₂O)₂]·H₂O (<i>cma</i>^3– = N-carboxymethylaspartate(3–)) is determined by single crystal X-ray structure analysis. The orthorombic crystals (<i>P</i>2₁2₁2₁, <i>a</i> = 7.7901(4) Å, <i>b</i> = 11.2368(4) Å, <i>c</i> = 13.2048(5) Å, <i>α</i> = <i>β</i> = <i>γ</i> = 90°, <i>Z</i> = 4) were obtained from the reaction mixture in the form of racemic conglomerate.</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":"228 - 235"},"PeriodicalIF":0.8,"publicationDate":"2022-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4743826","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, Crystal Structure Determination and Electrochemistry of Homoleptic Pd(0) Complexes Supported by Normal and Abnormal N-Heterocyclic Carbene Ligands","authors":"Nurul Amin SK,&nbsp;Bibaswan Sen,&nbsp;Sk Jahir Abbas,&nbsp;Sk Imran Ali","doi":"10.1007/s10870-022-00962-0","DOIUrl":"10.1007/s10870-022-00962-0","url":null,"abstract":"<div><p>Abnormal carbene complex of Pd(L1)₂, where L1 = 1,3-Bis(2,6-diisopropylphenyl)-2,4-diphenylimidazole and normal carbene complex of Pd(L2)₂, where L2 = 1,3-dimesityl-4,9-dioxonaphtho-2,3-diimidazole were prepared from a Pd(0) precursor Pd(COD)(CH₂TMS)₂. Both the complexes crystalize in the triclinic space group <i>P</i>-1 and cell parameters of Pd(L1)₂ and Pd(L2)₂ are <i>a</i> = 12.0477 Å, <i>b</i> = 17.5269 Å, <i>c</i> = 18.9786 Å, <i>α</i> = 114.4855°, <i>β</i> = 92.5295°, <i>γ</i> = 107.9472° and <i>a</i> = 11.5007 Å, <i>b</i> = 15.2316 Å, <i>c</i> = 17.9007 Å, <i>α</i> = 67.061°, <i>β</i> = 72.143°, <i>γ</i> = 72.183° respectively. In both case N-heterocyclic ligands are distorted towards palladium direction. Further, crystal structures reveal that the palladium atom is covalently bonded to the two aNHC and nNHC ligands respectively. The electrochemical properties of these complexes were determined by cyclic voltammetry analysis in THF solution under argon atmosphere. The enunciated reversibility of the complexes can be explained by sequential one electron oxidations of the palladium centre from Pd(0) to Pd(I) and then Pd(II).</p><h3>Graphical Abstract</h3><p>Abnormal carbene complex of Pd(L1)₂, where L1 = 1,3-Bis(2,6-diisopropylphenyl)-2,4-diphenylimidazole and normal carbene complex of Pd(L2)₂, where L2 = 1,3-dimesityl-4,9-dioxonaphtho-2,3-diimidazole were prepared from a Pd(0) precursor of Pd(COD)(CH₂TMS)₂. The crystal structures were determined by single crystal X-ray diffraction data and electrochemical properties were also determined by cyclic voltammetric analysis.</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":"217 - 227"},"PeriodicalIF":0.8,"publicationDate":"2022-09-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00962-0.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4368742","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":"Dinuclear Azide-Bridged Copper(II) Polymer With Azido···π(pyridiyl) Interaction: Synthesis, Crystal Structure and Hirshfeld Surface Analysis","authors":"Layachi Merabet,&nbsp;Zouaoui Setifi,&nbsp;Hela Ferjani,&nbsp;David K. Geiger,&nbsp;Christopher Glidewell,&nbsp;Sibel Demir Kanmazalp,&nbsp;Fatima Setifi,&nbsp;Lakhemici Kaboub","doi":"10.1007/s10870-022-00960-2","DOIUrl":"10.1007/s10870-022-00960-2","url":null,"abstract":"<div><p>A new coordination polymer of coper (II), [tetra-azido)tris(2-pyridyl)amine)dicopper(II)] (<b>1</b>) has been synthesized by the reaction between copper(II) nitrate hexahydrate, sodium azide and tris(2-pyridyl)amine under solvothermal conditions in aqueous methanol. The structure has been characterized by single-crystal X-ray diffraction. An analysis of Hirschfeld surfaces was examined. Single-crystal results reveals that the structure contains two independent copper(II) centers, both having approximately square pyramidal coordination: in one, two of the basal sites are occupied by bidentate tris-(2-pyridyl)amine and two azido ligands, with a third azido ligand at the apical site, while the other center is coordinated only by azido ligands. All azido ligands bind two copper centers, forming a coordination polymer chain with two types of Cu2N2 rings and one type of Cu4N4 ring, and in which all azido ligands form a bridge between two metal centers in mode µ-1,1. The Hirshfeld analysis revealed an azido··· (pyridyl) interaction in the coordination polymer chain, as well as weak C-H···N interactions, one of which links the chains into sheets.</p><h3>Index Abstract</h3><p>A new dinuclear copper (II) polymer [tetra-azido(tris(2-pyridyl)amine)dicopper(II)] (1) has been synthesized under solvothermal conditions and been characterized by single-crystal X-ray diffraction and Hirshfeld surface analysis.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div><div><p>The molecular structure of (1)</p></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 2","pages":"209 - 216"},"PeriodicalIF":0.8,"publicationDate":"2022-09-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4642143","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, Structure, and Reactivity of Triosmium Clusters Bearing a Metalated Dialkyl-substituted Pyrazine Ligand","authors":"Md. Mahbub Alam,&nbsp;Fahima Islam,&nbsp;Subas Rajbangshi,&nbsp;Kazi A. Azam,&nbsp;Shishir Ghosh,&nbsp;Vladimir N. Nesterov,&nbsp;Michael G. Richmond,&nbsp;Shariff E. Kabir","doi":"10.1007/s10870-022-00958-w","DOIUrl":"10.1007/s10870-022-00958-w","url":null,"abstract":"<div><p>Reactions of two dialkyl-substituted pyrazine ligands with a triosmium cluster are described. Both 2-ethyl-3-methylpyrazine (C₄H₂N₂MeEt) and 2,5-dimethylpyrazine (C₄H₂N₂Me₂) react with the labile triosmium cluster [Os₃(CO)₁₀(NCMe)₂] at 80 °C to afford [HOs₃(CO)₁₀(µ-C₄HN₂MeEt)] (<b>1</b>) and [HOs₃(CO)₁₀(µ-C₄HN₂Me₂)] (<b>2</b>), respectively. Clusters <b>1</b> and <b>2</b> are formed <i>via</i> C–H bond activation at the α-carbon of the corresponding pyrazine ligand. Cluster <b>2</b> reacts with PPh₃ at room temperature in the presence of Me₃NO‧2H₂O to yield the mono- and diphosphine-substituted clusters [HOs₃(CO)₉(PPh₃)(µ-C₄HN₂Me₂)] (<b>3</b>) and [HOs₃(CO)₈(PPh₃)₂(µ-C₄HN₂Me₂)] (<b>4</b>), respectively, both of which exist in more than one isomeric form in solution. All new clusters have been characterized using spectroscopic methods together with single-crystal X-ray diffraction studies for <b>1</b>, <b>2</b>, and <b>4</b>. The bonding in these clusters have been investigated by electronic structure calculations.</p><h3>Graphical Abstract</h3><p>Two new triosmium clusters bearing a metalated pyrazine\u0000ligand have been synthesized and structurally characterized.\u0000The reactivity of one of these newly synthesized clusters towards PPh₃ has also been investigated.</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":"197 - 208"},"PeriodicalIF":0.8,"publicationDate":"2022-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4231258","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":"Crystal Structure Characterization, Interaction Energy Analysis and DFT Studies of 3-(4-Chlorophenyl)-N-phenylquinoxalin-2-amine","authors":"P. Akhileshwari,&nbsp;K. R. Kiran,&nbsp;M. A. Sridhar,&nbsp;M. P. Sadashiva","doi":"10.1007/s10870-022-00959-9","DOIUrl":"10.1007/s10870-022-00959-9","url":null,"abstract":"<p>The title compound is synthesized, and characterized by spectroscopic and XRD methods. The compound crystallizes in the orthorhombic crystal system with the space group <i>P</i>2₁2₁2₁. The structure exhibits C–H⋯N intermolecular interaction and π⋯π interactions. Hirshfeld surface analysis was performed to determine the individual contributions of intermolecular contacts to the crystal packing. The structural and electronic properties of the molecule were investigated by density functional theory method with B3LYP hybrid functional. Intramolecular interactions involved in the crystal structure was analyzed through topological atom-in-molecules analysis and noncovalent interactions method. Molecular electrostatic potential surface shows the chemical reactive regions around the nitrogen and hydrogen atoms.</p><p>The article presents the characterization of synthesized compound by single crystal X-ray diffraction\u0000method. Atom-in-molecules analysis and noncovalent interactions Intramolecular\u0000interactions involved in the crystal structure were analyzed by DFT method.</p>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 2","pages":"185 - 196"},"PeriodicalIF":0.8,"publicationDate":"2022-08-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00959-9.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4636628","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}