Journal of Chemical Crystallography最新文献

{"title":"The X-ray Structure of [Fe(CO)3(η4-6-exo-(4-biphenylamino)cyclohepta-2,4-dien-1-one]","authors":"Ian S. Leiby,&nbsp;Eric W. Reinheimer,&nbsp;Daniel R. Griffith,&nbsp;Chip Nataro","doi":"10.1007/s10870-025-01039-4","DOIUrl":"10.1007/s10870-025-01039-4","url":null,"abstract":"<div><p>The structure of [Fe(CO)₃(η⁴-6-<i>exo</i>-(4-biphenylamino)cyclohepta-2,4-dien-1-one] [monoclinic, <i>a</i> = 20.368 (1), <i>b</i> <b>=</b> 6.2757(4), <i>c</i> = 29.5214(14), <i>β</i> = 101.024(5), space group C2/c] has been determined. There is a moderate hydrogen-bond between the amine proton and the oxygen atom of the ketone in another molecule. There is no significant π-stacking of the phenyl rings, but the nitrogen atom is fairly planar likely due to interaction with the π-system of the 4-biphenyl group and the hydrogen-bonding.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>Addition of two equivalents of 4-biphenylamine to [Fe(CO)₃(η⁵-cyclohepta-2,4-dien-5-yl-1-one)][BF₄] results in <i>exo</i>- attack at the coordinated ring forming the [Fe(CO)₃(η⁴-6-<i>exo</i>-(NH(4-biphenyl)))cyclohepta-2,4-dien-1-one], which was structurally characterized</p></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 2","pages":"92 - 96"},"PeriodicalIF":0.4,"publicationDate":"2025-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-025-01039-4.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949513","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":"A Rare Example of Manganese Aminopyridinate – Synthesis and Structure","authors":"Awal Noor","doi":"10.1007/s10870-024-01038-x","DOIUrl":"10.1007/s10870-024-01038-x","url":null,"abstract":"<div><p>Lithiated N-(2,6-diisopropylphenyl)-[6-(2,4,6-triisopropylphenyl)-pyridine-2-yl]-amine (ApH) undergoes a salt metathesis reaction with MnBr₂ in tetrahydrofuran (THF) at 50 °C in the presence of two equivalents of 4-<i>tert</i>-butylpyridine (^<i>t</i>BuPy) to yield only the second example of mononuclear manganese aminopyridinates, [Mn(Ap)₂(^<i>t</i>BuPy)]. The compound [C₅₉H₇₁MnN₅], crystallized in the monoclinic space group, <i>P</i>2₁/<i>c</i> with unit cell parameters: a = 11.9650(5) b = 17.9530(7) c = 24.3110(10) Å, β = 95.081(3)°, V = 5201.7(4) A³, Z = 4. Hirshfeld analyses show that H⋯H (89.1%) and H⋯C/C⋯H (10.9%) interactions are the two main contributors that lead to intermolecular stabilization in the solid-state structure.</p></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 2","pages":"85 - 91"},"PeriodicalIF":0.4,"publicationDate":"2025-01-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949415","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 Analysis of Four 2-Pyridineformamide Thiosemicarbazone Derivatives Using Non-Spherical Atomic Form Factors","authors":"Bhushan Shakya,&nbsp;Kuldeep Mahiya,&nbsp;Ramina Maharjan Shrestha,&nbsp;Hari Bhakta Oli,&nbsp;Paras Nath Yadav","doi":"10.1007/s10870-024-01037-y","DOIUrl":"10.1007/s10870-024-01037-y","url":null,"abstract":"<div><p>The crystal structures of four 2-pyridineformamide thiosemicarbazone derivatives <i>viz</i>, (<i>Z</i>,<i> Z’</i>)-4-methyl-<i>N</i>’-(morpholine-4-carbonothioyl)picolinohydrazonamide (<b>1</b>), (<i>Z</i>,<i> Z’</i>)-4-methyl-<i>N</i>’-(thiomorpholine-4-carbonothioyl) picolinohydrazonamide (<b>2</b>), (<i>Z</i>,<i> Z’</i>)-6-methyl-<i>N</i>’-(thiomorpholine-4-carbonothioyl)picolinohydrazonamide (<b>3</b>) and (<i>Z</i>,<i> Z’</i>)-<i>N</i>’-(azepane-1-carbonothioyl)-4-methylpicolinohydrazonamide (<b>4</b>) has been determined by single crystal X-ray diffraction analysis. Combined quantum mechanical methods (ORCA) and computation of non-spherical scattering form factors (NoSpherA2) were used for the refinement with anisotropic hydrogen atoms. The results of using independent atom model (IAM) and Hirshfield atom refinement (HAR) method based R2SCAN/ def2-TZVP functional were compared. All compounds show an improvement in the model after HAR refinement compared to independent atom model (IAM). There is a significant decrease in the residual factors with the use of anisotropic hydrogen refinement. HAR refinement provides a clearer understanding of electron delocalization, lone pairs, and the accumulation and depletion of electron density. The information obtained came from standard resolution single crystal X-ray diffraction data, indicating that high-quality structural analysis can now be performed without the need for neutron or synchrotron facilities.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>Structural studies of four 2-pyridineformamide thiosemicarbazone derivatives using non-spherical atomic form factors</p></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 2","pages":"75 - 84"},"PeriodicalIF":0.4,"publicationDate":"2025-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143949480","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":"Structures of 1,4,2-dithiazolidine 1,1-dioxide and 1,2,4-thiadiazolidin-3-one 1,1-dioxide heterocycles formed from N-benzyl-1-chloromethanesulfonamide and either phenyl isothiocyanate or 3,5-dimethylphenyl isocyanate","authors":"Noah Forrest,&nbsp;Edward J. Valente,&nbsp;Warren J. L. Wood","doi":"10.1007/s10870-024-01034-1","DOIUrl":"10.1007/s10870-024-01034-1","url":null,"abstract":"<div><p>Reaction of <i>N</i>-benzyl-1-chloromethanesulfonamide with phenyl isothiocyanate formed <i>N</i>-benzyl-3-phenylimino-1,4,2-dithiazolidine 1,1-dioxide. Crystals of this compound occurred in the monoclinic system, space group <i>P</i> 2(1), <i>a</i> = 26.7099(16) Å, <i>b</i> = 13.2518(5) Å, <i>c</i> = 8.2769(4) Å, <i>β</i> = 97.099(5)^o, Z = 8, with four molecules in the asymmetric unit. The structure confirms a prior assignment that the C = S bond of the isothiocyanate was the reactive moiety. Using the same reaction conditions, 3,5-dimethylphenyl isocyanate was reacted <i>N</i>-benzyl-1-chloromethanesulfonamide to produce a product in 81% yield, which was determined to be 2-benzyl-4-(3’,5’-dimethylphenyl)-1,2,4-thiadiazolidin-3-one 1,1-dioxide. Crystals of this compound are monoclinic, space group <i>P</i> 2(1)/<i>n</i>, <i>a</i> = 5.2243(11) Å, <i>b</i> = 15.844(5) Å, <i>c</i> = 18.628(3) Å, <i>β</i> = 96.72(2)^o, and Z = 4. This product demonstrated that the C = N bond of the aryl isocyanate reacted to form the 1,2,4-thiadiazolidin-3-one 1,1-dioxide ring system.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>Heterocyclic rings formed from <i>N</i>-benzyl-1-chloromethanesulfonamide and phenyl isothiocyanate via the C = S bond (structure on the left) or 3,5-dimethylphenyl isocyanate via the C = N bond (structure on the right)</p></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 1","pages":"67 - 73"},"PeriodicalIF":0.4,"publicationDate":"2024-12-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143668150","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":"Polymorphism and Whole-Molecule Disorder of an Antitubercular 8-Nitrobenzothiazinone","authors":"Rüdiger W. Seidel,&nbsp;Richard Goddard,&nbsp;Tom U. Schlegel,&nbsp;Adrian Richter,&nbsp;Ines Rudolph,&nbsp;Peter Imming","doi":"10.1007/s10870-024-01035-0","DOIUrl":"10.1007/s10870-024-01035-0","url":null,"abstract":"<div><p>8-Nitrobenzo-1,3-thiazin-4-ones (BTZs) are a promising class of antitubercular agents with a novel mechanism of action, viz. suicide inhibition of decaprenylphosphoryl-β-D-ribose 2’-epimerase 1 (DprE1), an enzyme crucial for cell wall synthesis in the pathogen <i>Mycobacterium tuberculosis</i>. 8-Nitro-2-(piperidin-1-yl)-6-(trifluoromethyl)-4<i>H</i>-benzo-1,3-thiazin-4-one (<b>1</b>) is a chemically simplified analogue of the anti-tuberculosis phase 2 clinical drug candidate BTZ-043. Structural elucidation of <b>1</b> in the solid-state has been carried out by X-ray crystallography and two polymorphic forms of <b>1</b> have been revealed. <b>1</b>-I crystallizes in the triclinic system (space group <i>P</i>-1, <i>Z</i> = 6) with one molecule exhibiting whole-molecule disorder with a preferred orientation. The crystal structure of <b>1</b>-II belongs to the tetragonal system (space group <i>P</i>4₃, <i>Z</i> = 4) and exhibits positional disorder in several parts of the molecule.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>X-ray crystallography revealed a triclinic (space group <i>P</i>-1, <i>Z</i> = 6) and a tetragonal (space group <i>P</i>4₃, <i>Z</i> = 4) polymorph of the antimycobacterial agent 8-nitro-2-(piperidin-1-yl)-6-(trifluoromethyl)-4<i>H</i>-benzo-1,3-thiazin-4-one</p></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 1","pages":"56 - 65"},"PeriodicalIF":0.4,"publicationDate":"2024-12-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-024-01035-0.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143667836","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":"The Supramolecular Structures and Photo-Physical Properties Modulated by Spacer Lengths in 1,ω-Bis(isoquinoline)Alkane/(Bi4I16)4− Hybrids","authors":"Peng Wang,&nbsp;Wen-Wen Sheng,&nbsp;Ying-Sheng Xu,&nbsp;Zhi-Rong Chen","doi":"10.1007/s10870-024-01033-2","DOIUrl":"10.1007/s10870-024-01033-2","url":null,"abstract":"<div><p>The study about the supramolecular interactions in the organic–inorganic hybrids will be significant for the design of new photo/electrical functional materials. In this work, 1,<i>ω</i>-bis(isoquinoline)alkane cations with different spacer lengths (n = 3, 5, 6) have been incorporated with iodobismuthates to construct three new hybrids, which have been formula as [BIQPP]₂[Bi₄I₁₆] (<b>1</b>), [BIQPT]₂[Bi₄I₁₆] (<b>2</b>) and [BIQHX]₂[Bi₄I₁₆] (<b>3</b>) through X-ray single crystal diffraction method (BIQPP²⁺ = 1,3-bis(isoquinoline)propane, BIQPT²⁺ = 1,5-bis(isoquinoline) pentane, BIQHX²⁺ = 1,6-bis(isoquinoline)hexane). The centrosymmetric [Bi₄I₁₆]⁴⁻ anions are constructed from four edge-sharing BiI₆ octahedra. Interestingly, with the elongation of spacer length on isoquinoline from 3, 5 to 6, the iodobismuthate anions exhibit 0-D [Bi₄I₁₆]⁴⁻ tetramers (n = 3, 6 for <b>1</b> and <b>3</b>) and pseudo 3-D [Bi₄I₁₆]_n⁴ⁿ⁻ network (n = 5, for <b>2</b>) based on I···I interactions. Supramolecular interactions including π–π stacking interactions and C–H···I hydrogen bonds contribute to their structural extensions. Consequently, the enhanced red emission intensity and the lower thermochromic temperature can be observed in <b>2</b>. The clarification on the spacer effect on the supramolecular interactions and functional properties of this work will be beneficial for the design of new functional materials.</p><h3>Graphical Abstract</h3><p> Different iodobismuthate anions and photo-physical properties including red emission intensity and thermochromism can be achieved by elongating the spacer lengths in 1,ω-Bis(isoquinoline)alkane cations</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 1","pages":"47 - 55"},"PeriodicalIF":0.4,"publicationDate":"2024-11-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143668408","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":"The X-ray Structures of [Fe(CO)3(η4-6-exo-(PAr3)cyclohepta-2,4-dien-1-one][BF4] (Ar = m-C6H4CH3 or p-C6H4F)","authors":"Makenna R. Miller,&nbsp;Ryann A. Carlotz,&nbsp;Jeremiah E. Stevens,&nbsp;Daniel R. Griffith,&nbsp;Chip Nataro","doi":"10.1007/s10870-024-01036-z","DOIUrl":"10.1007/s10870-024-01036-z","url":null,"abstract":"<div><p>The structures of [Fe(CO)₃(η⁴-6-<i>exo</i>-(tri-<i>m</i>-tolylphosphine)cyclohepta-2,4-dien-1-one][BF₄] [tetragonal, <i>a</i> = 35.6005(7), <i>b</i> <b>=</b> 35.6005(7), <i>c</i> = 10.5456(3), space group I4₁/a] and [Fe(CO)₃(η⁴-6-<i>exo</i>-(tri-<i>p</i>-fluorophenylphosphine)cyclohepta-2,4-dien-1-one][BF₄] [triclinic, <i>a</i> = 9.8852(3), <i>b</i> <b>=</b> 10.0996(4), <i>c</i> = 16.0526(4), <i>α</i> = 99.813(3), <i>β</i> = 94.164(2), <i>g</i> = 102.911(3) space group P-1] have been determined. Both structures contain a disordered CH₂Cl₂ molecule. The tetrafluoroborate ion in [Fe(CO)₃(η⁴-6-<i>exo</i>-(tri-<i>m</i>-tolylphosphine)cyclohepta-2,4-dien-1-one][BF₄] is also disordered. There are no close contacts indicative of hydrogen bonding within either structure, but there is <i>π</i>-<i>π</i> stacking observed for [Fe(CO)₃(η⁴-6-<i>exo</i>-(tri-<i>m</i>-tolylphosphine)cyclohepta-2,4-dien-1-one][BF₄].</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>Addition of PAr₃ (Ar = <i>m</i>-C₆H₄CH₃ or <i>p</i>-C₆H₄F) to [Fe(CO)₃(η⁵-cyclohepta-2,4-dien-5-yl-1-one)][BF₄] results in attack at the coordinated ring in a position <i>exo</i>- to the iron atom forming the corresponding [Fe(CO)₃(η⁴-6-<i>exo</i>-(PAr₃)cyclohepta-2,4-dien-1-one][BF₄] compounds, which were structurally characterized</p></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 1","pages":"41 - 46"},"PeriodicalIF":0.4,"publicationDate":"2024-11-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-024-01036-z.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143667869","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":"The X-ray Structures of [Fe(CO)3(η4-6-exo-(PPh2R)cyclohepta-2,4-dien-1-one][BF4] (R = Me or tBu)","authors":"Stephanie M. Ingwer,&nbsp;Christopher J. Yoler,&nbsp;Todd Reynolds,&nbsp;Daniel R. Griffith,&nbsp;Chip Nataro","doi":"10.1007/s10870-024-01031-4","DOIUrl":"10.1007/s10870-024-01031-4","url":null,"abstract":"<div><p>The structures of [Fe(CO)₃(η⁴-6-<i>exo</i>-(methyldiphenylphosphine)cyclohepta-2,4-dien-1-one][BF₄] [orthorhombic, <i>a</i> = 12.3269(4), <i>b</i><b> = </b>13.5243(5), <i>c</i> = 13.7127(4), space group Pna2₁] and [Fe(CO)₃(η⁴-6-<i>exo</i>-(<i>tert</i>-butyldiphenylphosphine)cyclohepta-2,4-dien-1-one][BF₄] [monoclinic, <i>a</i> = 9.7947(3), <i>b</i><b> = </b>12.8766(3), <i>c</i> = 20.2168(5), <i>β</i> = 91.089(3), space group P2₁/c] have been determined. The disordered tetrafluoroborate ion in [Fe(CO)₃(η⁴-6-<i>exo</i>-(methyldiphenylphosphine)cyclohepta-2,4-dien-1-one][BF₄] sits between two of the cations and displays interactions with hydrogen atoms in the <i>ortho</i>- position of the phenyl rings, the methyl group and the 6-position of the seven-membered ring. There is also close contact between the ketone oxygen atom and two protons in another cation, a proton of the methyl group and the proton in the 5-position of the seven-membered ring. The tetrafluoroborate anion in [Fe(CO)₃(η⁴-6-<i>exo</i>-(<i>tert</i>-butyldiphenylphosphine)cyclohepta-2,4-dien-1-one][BF₄] is not disordered and shows close contacts with protons in three cation units. In one cation the interaction is with two protons from separate methyl groups of the <i>tert</i>-butyl substituent. The remaining interactions are with a proton in the <i>ortho</i>- position of a phenyl ring in one cation and the proton in the 2-position of the seven-membered ring. There is also an interaction between the ketone oxygen and a proton from the <i>tert</i>-butyl group in another cationic unit.</p><h3>Graphical abstract</h3><p>Addition of PPh₂R (R = Me or ^<i>t</i>Bu) to [Fe(CO)₃(η⁵-cyclohepta-2,4-dien-5-yl-1-one)][BF₄] results in <i>exo</i>- attack at the coordinated ring forming the [Fe(CO)₃(η⁴-6-<i>exo</i>-(PPh₂R)cyclohepta-2,4-dien-1-one][BF₄] compounds, both of which were structurally characterized.</p>\u0000<div><figure><div><div><picture><img></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 1","pages":"35 - 40"},"PeriodicalIF":0.4,"publicationDate":"2024-10-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143668329","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":"High-Yielding Syntheses, Crystal Structures and Hirshfeld Surface Analysis of Bis-1,1′-(2-nitropropenes) Extended with Benzene-1,4-diyl and Biphenyl-4,4′-diyl Spacers","authors":"Kostiantyn V. Domasevitch,&nbsp;Ganna A. Senchyk,&nbsp;Harald Krautscheid","doi":"10.1007/s10870-024-01032-3","DOIUrl":"10.1007/s10870-024-01032-3","url":null,"abstract":"<div><p>Crystal structures of two 2-nitropropene derivatives, namely 1,4-bis((<i>E</i>)-2-nitroprop-1-enyl)benzene and 4,4′-bis((<i>E</i>)-2-nitroprop-1-enyl)biphenyl, support relevance of lone pair-π-hole interactions of nitro groups to the crystal packing of extended polyaromatic molecules. For the former structure, these bonds complement slipped π–π interactions of the benzene rings within a basic supramolecular motif representing infinite stacks. In the biphenyl derivative, only one out of two nitro groups afford NO₂⋯NO₂ bonds (N⋯O = 3.191(2) Å) as a local pattern. The decreased significance of lone pair-π-hole interactions is in line with growing contribution of weak dispersion forces, which favor close alignment of the molecules and larger interaction areas to generate multiple C–H⋯π bonds. Different types of C–H⋯O, C–H⋯π, π–π, NO₂–π, NO₂⋯NO₂, tetrel CH₃⋯O and CH₃⋯π bonds, which actualize in the present structures were further assessed by Hirshfeld surface analysis and intermolecular interaction energies were calculated using the CE B3LYP/6 31G(d,p) energy model. In addition, the facile and high-yielding preparations by condensation of dialdehydes and nitroethane, provide a straightforward access to the present 2-nitropropenes, as valuable synthetic intermediates.</p><h3>Graphical Abstract</h3><p>The X-ray structures of 1,4-bis((<i>E</i>)-2-nitroprop-1-enyl)benzene and 4,4′-bis((<i>E</i>)-2-nitroprop-1-enyl)biphenyl reveal coexistence and interplay of lone pair-π-hole NO₂⋯NO₂ bonds, weak hydrogen and tetrel bonds and aromatic interactions.</p>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 1","pages":"22 - 34"},"PeriodicalIF":0.4,"publicationDate":"2024-10-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143668252","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":"The Versatility of the Dicyanamide Anion (Dca) as a Bridging Ligand: Synthesis, Structure and Theory of a Unique Ladder Chain Consisting of 2 µ1,5-dca Bridged Dinuclear Cu2(dca)2 Units with Additional µ1,3-dca Bridges Along the Chain","authors":"Yaakoub Saadallah,&nbsp;Zouaoui Setifi,&nbsp;Hela Ferjani,&nbsp;Christopher Glidewell,&nbsp;Christian Jelsch,&nbsp;Fatima Setifi,&nbsp;Diego M. Gil,&nbsp;Jorge Echeverria,&nbsp;Jan Reedijk","doi":"10.1007/s10870-024-01028-z","DOIUrl":"10.1007/s10870-024-01028-z","url":null,"abstract":"<div><p>The synthesis and structural details of a mixed-ligand Cu(II) coordination compound, specifically <i>catena</i>-poly[bis(dicyanamido)(1,10-phenanthroline-5,6-dione)copper(II)] <b>1</b>, are reported. The title compound was synthesized utilizing a solvothermal method by employing dicyanamide, 1,10-phenanthroline-5,6-dione (phendione) and copper(II) sulfate pentahydrate (CuSO₄•5H₂O) as the starting materials. The title compound was characterized by standard analytical and spectroscopic methods. The 3D structure was determined by single-crystal X-ray diffraction. Examination of the supramolecular interaction patterns indicates that the stability of the ladder structure is achieved by the bridging dca anions and the presence of weak hydrogen-bonding contacts, specifically C-H···O and C-H···N bonds, as well as C-O/N···π interactions. These interactions together contribute to the formation of a ladder-type infinite chain structure. The generated structure has been theoretically investigated with Hirshfeld surface analysis, QTAIM and NCI analysis to reveal the interaction energies and bonds present inside and between molecules. The non-covalent interactions present in the crystal structure were further investigated theoretically, with particular attention to the cooperative C ≡ N···π(py) and N···π(hole) interactions involving the dicyanamide ligand and nitrile moieties in the compound. The solid-state stability of compound <b>1</b> appears to be strongly influenced by the cooperative effect of H-bonding interactions as well as the C ≡ N···π(py) and N···π(hole) contacts, as confirmed by theoretical calculations.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div><p><i>Synthesis, Structure and Theoretical Calculations of a Unique Ladder Chain Containing the Dicyanamido Ligand (dca), Consisting of 2 µ</i>_<i>1,5</i><i>-dca Bridged Dinuclear Cu</i>_<i>2</i><i>(dca)</i>_<i>2</i><i>Units and Having µ</i>_<i>1,3</i><i>-dca Bridges along the Chain.</i></p><p><b>One sentence essence:</b></p><p>\u0000 <i>catena</i>-poly[bis(dicyanamido)(1,10-phenanthroline-5,6-dione)copper(II)] is a unique ribbon ladder, infinite chain structure with two differently bridged dicyanamide anions</p></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"55 1","pages":"10 - 21"},"PeriodicalIF":0.4,"publicationDate":"2024-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-024-01028-z.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142215301","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}