Journal of Chemical Crystallography最新文献

{"title":"New Tetraruthenium Cluster from the Thermolysis of [Ru3(CO)10(μ-dppm)]: Crystal Structure of [HRu4(CO)9(μ3-PhPCH2PPh2) (μ3,η2:η1:η1-C6H4)]","authors":"Md. Abdullah Al Mamun,&nbsp;Tazul Islam,&nbsp;Subas Rajbangshi,&nbsp;Shishir Ghosh,&nbsp;Michael G. Richmond,&nbsp;Shariff E. Kabir","doi":"10.1007/s10870-023-00998-w","DOIUrl":"10.1007/s10870-023-00998-w","url":null,"abstract":"<div><p>Thermolysis of [Ru₃(CO)₁₀(μ-dppm)] (<b>1</b>) in refluxing benzene, followed by chromatographic separation by TLC, afforded the new cluster [HRu₄(CO)₉(μ₃-PhPCH₂PPh₂)(μ₃,η²:η¹:η¹-C₆H₄)] (<b>10</b>) in 7% yield in addition to the previously reported clusters [Ru₃(CO)₉{µ₃-PhPCH₂PPh(C₆H₄)}] (<b>2</b>) and [HRu₄(CO)₉(μ₄-PhPCH₂PPh₂)(μ₄,η⁶:η¹:η¹-C₆H₄)] (<b>8</b>) in 70% and 4% yields, respectively. The molecular structure of <b>10</b> has been determined by single-crystal X-ray diffraction analysis. Compound <b>10</b> possesses a Ru₄ metal core where two of the six triangular faces are capped by μ₃,η²:η¹:η¹-C₆H₄ (benzyne) and µ₃-PhPCH₂PPh₂ ligands. Compound <b>10</b> transforms to the known cluster [HRu₄(CO)₉(μ₃-PhPCH₂PPh₂)(μ₄,η⁶:η¹:η¹-C₆H₄)] (<b>8</b>) slowly at 80 °C. The bonding in the new cluster <b>10</b> has been investigated by electronic structure calculations.</p><h3>Graphical Abstract</h3><p>A new tetraruthenium cluster has been isolated and structurally characterized from the thermolysis of [Ru₃(CO)₁₀(μ-dppm)] at 80 °C.</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":"54 1","pages":"54 - 63"},"PeriodicalIF":0.4,"publicationDate":"2023-12-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138523664","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 and Molecular Structures of Three Co-crystals from 1,3-Dimethyl-3,7-dihydro-1H-purine-2,6-dione and Carboxylic Acids","authors":"Zhaozhi Li,&nbsp;Xianhong Wen,&nbsp;Shouwen Jin,&nbsp;Xingjun Gao,&nbsp;Weiqiang Xu,&nbsp;Yaoqi Zhen,&nbsp;Chenzhe Shi,&nbsp;Daqi Wang","doi":"10.1007/s10870-023-01000-3","DOIUrl":"10.1007/s10870-023-01000-3","url":null,"abstract":"<div><p>The preparation, X-ray crystal structure, Fourier Transform infrared (FTIR) spectroscopy, and elemental analysis of the three complexes (1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione): (2,6-dichlorobenzoic acid)₂: H₂O [(tp)· (Hbza)₂ · H₂O, Hdcba = 2,6-dichlorobenzoic acid] (<b>1</b>) (1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione): (2-pyrazinecarboxylic acid) [(tp) · (Hpyca), Hpyca = 2-pyrazinecarboxylic acid] (<b>2</b>) and (1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione): (3-nitrophthalic acid) [(tp) · (Hntpa)] (<b>3</b>) based on 1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione, 2,6-dichlorobenzoic acid 2-pyrazinecarboxylic acid, and 3-nitrophthalic acid are reported. XRD and FTIR analysis indicated that they are all co-crystal. <b>1</b> crystallizes in the monoclinic, space group <i>P</i>2₁/<i>n</i>, with a = 7.1019(7) Å, b = 12.9494(12) Å, c = 26.253(3) Å, β = 93.536(3)°, V = 2409.8(4) ų, Z = 4. <b>2</b> crystallizes in the monoclinic, space group <i>P</i>2₁/<i>c</i>, with a = 6.9863(7) Å, b = 25.437(3) Å, c = 7.3987(7) Å, β = 95.152(2)°, V = 1309.5(2) ų, Z = 4. <b>3</b> crystallizes in the monoclinic, space group <i>P</i>2₁/<i>n</i>, with a = 14.2133(15) Å, b = 8.2333(9) Å, c = 15.3860(17) Å, <i>β</i> = 117.236(5)º, V = 1600.9(3) ų, Z = 4. The imidazole-carboxylic acid synthon of the CO₂H···N type is observed in all the co-crystal. The imidazole H–N also donated the N–H···O hydrogen bonds in all cases. Apart from the classical hydrogen bonds, the auxiliary expanding interactions as CH···O, CH₃···O, CH···Cl, O···O, Cl···O, Cl···Cl, Cl···π, O···π, and π···π also play important roles in the structure extension. For the coexistence of the various weak interactions these structures adopted the most common R₂²(7) supramolecular synthon. In conclusion, we have shown that 2D–3D connections can be constructed by the collective non-covalent interactions.</p><h3>Graphical Abstract</h3><p>\u0000In the three prepared supramolecular assemblies there are plenty of weak nonbonding interactions such as directional hydrogen bonds of O–H···N, N-H···O, O–H···O, intra- and interchain CH···O, CH₃···O, CH···Cl, O···O, Cl···O, Cl···Cl, Cl···π, O···π, and π···π interactions, on account of these collective weak interactions, these compounds displayed the 2D–3D framework structures.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 1","pages":"41 - 53"},"PeriodicalIF":0.4,"publicationDate":"2023-12-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138523681","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 of 2-((E)-((Z)-3-(((4-hydroxyphenyl)amino)methylene)-4-oxocyclohexa-1,5-dien-1-yl)diazenyl)benzoic Acid and Synthesis, Spectroscopy, and DFT Study of Its Dibutyltin(IV) Complex","authors":"Pratima Debnath,&nbsp;Chinmoy Majumder,&nbsp;Arnab Bhattacharya,&nbsp;Paresh Debnath,&nbsp;Subhadip Roy,&nbsp;Alexander S. Novikov,&nbsp;Manojit Roy,&nbsp;Tarun Kumar Misra","doi":"10.1007/s10870-023-00996-y","DOIUrl":"10.1007/s10870-023-00996-y","url":null,"abstract":"<div><p>The structure of the 2-((<i>E</i>)-((<i>Z</i>)-3-(((4-hydroxyphenyl)amino)methylene)-4-oxocyclohexa-1,5-dien-1-yl)diazenyl)benzoic acid (H₃L) was confirmed by single crystal X-ray diffraction and Hirshfeld surface analysis was used further to quantify the intermolecular interactions. It crystallized in monoclinic space group <i>P</i>2₁/c. The observed bond distances evidence that the structure exists predominately in azo-enamine tautomeric form in the solid state. A novel dibutyltin(IV) complex, [(Bu₂SnHL)₂] (<b>1</b>) was synthesized from H₃L. The complex was then characterized by studying different techniques including elemental analysis, FT-IR, and NMR (¹H, ¹³C, and ¹¹⁹Sn) spectroscopy. In solution state, the molar mass of the compound was confirmed by Mass spectrometry. Spectroscopy study guides to predict the structure of the complex which is supposed to be a cyclic dimer [(Bu₂SnHL)₂] and Sn(IV) adopts a six-coordinated geometry. However, in solution Sn(IV) adopts four coordinated distorted tetrahedral geometry which was supported by ¹¹⁹Sn NMR spectroscopy (δ_Sn(119), 126.34 ppm) and EI-MS results of the complex ion ([C₂₈H₃₂N₃O₄Sn]⁺,m/z 593.1). Further, the structures in solid and solution state were supported by developing their optimized structures and IR data from the DFT calculation.</p><h3>Graphical Abstract</h3><p>The crystal structure of the ligand is in azo-enamine tautomeric form and in accordance with DFT study, its dibutyltin(IV) complex is a cyclic dimer, (Bu₂SnHL)₂, which becomes monomer in solution.</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":"54 1","pages":"28 - 40"},"PeriodicalIF":0.4,"publicationDate":"2023-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138523679","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":"Exploring Cyclic Hydrogen Bonds and Polymorphic Potential in 1,2-Diols Through Hirshfeld Analyses and Fingerprint Plots","authors":"Mónica Farfán-Paredes,&nbsp;Ma. Eugenia Ochoa,&nbsp;Rosa Santillan,&nbsp;Norberto Farfán","doi":"10.1007/s10870-023-00997-x","DOIUrl":"10.1007/s10870-023-00997-x","url":null,"abstract":"<div><p>The molecular environment in the crystal of [1,1′-bi(cyclopentane)-1,1′-diol] <b>D-1</b> and [1,1′-bi(cyclohexane)-1,1′-diol] <b>D-2</b> were comparatively investigated using X-ray diffraction, Hirshfeld surface analysis and two-dimensional plotting of the normalized interatomic distance. Different ways of crystallization of <b>D-1</b> led to polymorphism. Studying the differences between the chemical environments of polymorphic molecules is the key for understanding the structure in the solid state. Hirshfeld analyses along with fingerprint plots revealed the differences between the two polymorphs of <b>D-1</b> with <i>anti-</i> and <i>syn-</i>conformation, and the similarities between <b>D-1</b> and <b>D-2</b> that show the same six hydrogen bonds motif. A co-crystal <b>DB</b> between <b>D-2</b> and a hexahydroisobenzofuran derivative was also analyzed. Fingerprint plots show a distinctive pair of spikes in the structures with cyclic hydrogen bonds as well as information about the contribution of O–H⋯O/O⋯H–O interactions, that is different for each system despite having the same number of –OH groups. Knowledge of the conformation and the intermolecular interactions is crucial to understand its role in this kind of systems and for their potential use in pharmaceutical industry, supramolecular engineering, catalysis, and design of new materials.</p><h3>Graphical Abstract</h3><p>Hirshfeld analyses along with fingerprint plots revealed the differences between two polymorphs with <i>anti-</i> and <i>syn-</i>conformation, and the similarities between compounds that show the same six hydrogen bonds motif.</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":"54 1","pages":"18 - 27"},"PeriodicalIF":0.4,"publicationDate":"2023-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134901245","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, Hirshfeld Surface Analysis, and DFT Calculations of Ni(II) Complex with 3,3′-(-(pentane-3,3-diylbis(1H-pyrrole-5,2-diyl))bis(diazene-2,1-diyl))Dipyridine","authors":"Jialin Sun,&nbsp;Ying Sun,&nbsp;Zhenming Yin","doi":"10.1007/s10870-023-00994-0","DOIUrl":"10.1007/s10870-023-00994-0","url":null,"abstract":"<div><p>A Ni(II) complex of 3,3′-(-(pentane-3,3-diylbis(1H-pyrrole-5,2-diyl))bis(diazene-2,1-diyl)) dipyridine, <b>NiL</b>, has been synthesized and characterized. In the crystal, the Ni(II) ion is in square-planar geometry by coordinating to two pyrrole nitrogen atoms and two azo nitrogen atoms. Anagostic C–H···Ni interactions, as well as C–H···N hydrogen bond were found play important role in the self-assembly of the complex molecules. The intermolecular interactions were evaluated by Hirshfeld surface analysis. Frontier molecular orbitals (HOMO and LUMO), their energy gap and associated reactive parameters were calculated to understand the properties of the complex. UV–Vis spectrum of the complex were also performed.</p><h3>Graphical Abstract</h3><p>Anagostic C–H···Ni interactions were found play important role in the crystal of the Ni(II) complex with 3,3'-(-(pentane-3,3-diylbis(1H-pyrrole-5,2-diyl))bis(diazene-2,1-diyl)) dipyridine.\u0000</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"54 1","pages":"1 - 8"},"PeriodicalIF":0.4,"publicationDate":"2023-09-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135535698","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":"Assembly of a 2D Cd(II) Coordination Polymer from a New Multidentate Ligand 2-((1H-Tetrazol-5-yl)methyl)-1H-imidazole-4,5-dicarboxylic acid","authors":"Qiang Cai,&nbsp;Xuehai You,&nbsp;Jun Su,&nbsp;Weibin Tang","doi":"10.1007/s10870-023-00995-z","DOIUrl":"10.1007/s10870-023-00995-z","url":null,"abstract":"<div><p>A new substituted imidazole-dicarboxylate compound, namely 2-((1<i>H</i>-tetrazol-5-yl)methyl)-1<i>H</i>-imidazole-4,5-dicarboxylic acid (H₄tamIDC), has been successfully designed and prepared. Then, H₄tamIDC is used as a multidentate ligand to react with Cd(II) ion under solvothermal conditions, giving rise to the construction of a two-dimensional (2D) Cd(II) coordination polymer formulated as {[Cd(H₂tamIDC)(H₂O)]·CH₃CN}_n (<b>1</b>). Single-crystal X-ray diffraction study indicates that the H₂tamIDC²⁻ ligand in complex <b>1</b> adopts an interesting coordination fashion named <i>µ</i>₃-<i>kO</i>:<i>kO′</i>:<i>kN</i>:<i>kN</i>′:<i>kN″</i> to connect the Cd(II) ions into a 2D coordination framework containing dinuclear cadmium clusters. Such a 2D network can be simplified as a (4,4) topological net if each Cd₂ cluster is viewed as a four-connected node. Furthermore, the investigation of luminescence property reveals that complex <b>1</b> displays an intense emission around 475 nm when excited at 371 nm.</p><h3>Graphical Abstract</h3><p>A new 2D Cd(II) coordination polymer containing dinuclear cadmium clusters has been constructed by using a newly designed multidentate ligand 2-((1H-tetrazol-5-yl)methyl)-1H-imidazole-4,5-dicarboxylic acid and displays intense blue photoluminescence with a maximum emission band at 475 nm upon excitation at 371 nm.</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":"54 1","pages":"9 - 17"},"PeriodicalIF":0.4,"publicationDate":"2023-09-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135535433","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 of Tetrakis(dimethyl N-cyanodithioiminocarbonate) Bis[(aqua)-µ2-hydroxy-n-butyldichloridotin(IV)]","authors":"Babacar Mbaye,&nbsp;Mouhamadou Birame Diop,&nbsp;Mouhamadou Sembene Boye,&nbsp;Thierry Maris,&nbsp;Aminata Diassé-Sarr,&nbsp;Libasse Diop","doi":"10.1007/s10870-023-00992-2","DOIUrl":"10.1007/s10870-023-00992-2","url":null,"abstract":"<div><p>The reaction between two equivalents of dimethyl <i>N</i>-cyanodithioiminocarbonate, [(MeS)₂C=N–C≡N] (<b>1</b>), one equivalent of <i>n</i>-butyltin trichloride, Sn(<i>n</i>-Bu)Cl₃ and one equivalent of sodium hydroxide, NaOH led to isolation of a dinuclear complex {[Sn(<i>n</i>-Bu)Cl₂(OH)(H₂O)]₂} (<b>2</b>) which co-crystallized with four [(MeS)₂C=N–C≡N] molecules, {[Sn(<i>n</i>-Bu)Cl₂(OH)(H₂O)]₂[(CH₃S)₂C=N–C≡N]₄} (<b>3</b>). The compound was investigated by single-crystal X-ray diffraction analysis and infrared spectroscopy. Compound <b>3</b> crystallizes in the triclinic space group <i>P</i> <span>(overline{1 })</span> with <i>a</i> = 9.8208(15), <i>b</i> = 11.2664(17), <i>c</i> = 12.0446(18) Å, <i>α</i> = 106.236(5), <i>β</i> = 111.510(5), <i>γ</i> = 97.710(6)°, <i>V</i> = 1147.9(3) ų, <i>Z</i> = 1 and Z′ = 0.5. In the complex, two aqua-<i>n</i>-butyltinhydroxide dichloride moieties, [Sn(<i>n</i>-Bu)Cl₂(OH)(H₂O)], are bridged by the hydroxides. The hydroxide bridges bond lengths describe a static <i>trans</i> effect yielding a dissymmetry in Sn–O bonding. Two inner O2–H2D⋯Cl1 hydrogen bonds strengthen the dinuclear component. The dimethyl <i>N</i>-cyanodithioiminocarbonate molecules are linked to the dinuclear component through the hydroxide bridges and the water molecules by O1–H1⋯N2A and O2–H2C⋯N2B hydrogen bonding patterns of D type, respectively. The [(MeS)₂C=N–C≡N] molecules exhibit a positional disorder. These hydrogen bonding interactions lead to cyclic patterns generating <span>({R}_{1}^{1})</span>(6) and <span>({R}_{2}^{2})</span>(8) rings. Additional C–H⋯Cl and C–H⋯N hydrogen bond patterns also contribute to the crystal structure framework: they give rise to a 3D structure.</p><h3>Graphical Abstract</h3><p>Reacting with <i>n</i>-BuSnCl₃ and NaOH in an aqueous mixed solvent, dimethyl <i>N</i>-cyanodithioiminocarbonate, (MeS)₂C=N–C≡N forms a co-crystalline 4:1 assembly with the bimetallic organotin(IV) complex, [Sn(<i>n</i>-Bu)Cl₂(OH)(H₂O)]₂, whose single crystal XRD analysis exhibits a 3D hydrogen bonded structure.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 4","pages":"547 - 554"},"PeriodicalIF":0.8,"publicationDate":"2023-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47709923","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":"A 3D Compound Based on Semi-rigid Tricarboxylato-Bridged Co(II): Synthesis, Crystal Structure and Magnetism","authors":"Yan-Yan An,&nbsp;Ting-Ting Guo,&nbsp;Jian-Hong Bian,&nbsp;Juan-Zhi Yan","doi":"10.1007/s10870-023-00993-1","DOIUrl":"10.1007/s10870-023-00993-1","url":null,"abstract":"<div><p>With the assistance of N-donor ligand 1,4-bi(1H-imidazol-1-yl)benzene (1,4-bib), Co(II) reacts with 5-((4-carboxyphenoxy)-methyl)isophthalic acid (H₃L) under hydrothermal condition to form a compound [Co₃(L³⁻)₂(1,4-bib)₄]·4H₂O (<b>1</b>). The both contributions of semi-rigid tricarboxylic ligand L³⁻ and rigid 1,4-bib leads to predictably high dimensional structure. Compound <b>1</b> crystallizes in a complicated 3D network, which can be simplified as 3,6,8-<i>conn</i> topology. For the correlation between structure and property, the structural feature is well reflected in the magnetic property: a carboxylato group bridges two Co(II) paramagnetic ions. Within the dinuclear subunit, significant anti-ferromagnetic interactions are observed.</p><h3>Graphical Abstract</h3><p>A novel 3D Co(II) compound <b>1</b> is formed via hydrothermal reaction in this work. Antiferromagnetic interactions between two neighbour cations coordinated by one carboxylato group are observed.</p>\u0000 <div><figure><div><div><picture><source><img></source></picture></div></div></figure></div>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 4","pages":"540 - 546"},"PeriodicalIF":0.8,"publicationDate":"2023-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45284644","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, Spectral Properties, Crystal Structure and DFT Studies of 2,2′-diamino-4,4′-(propane-2,2′-diyl)-Diphenol","authors":"Fatma Aydin,&nbsp;N. Burcu Arslan","doi":"10.1007/s10870-023-00990-4","DOIUrl":"10.1007/s10870-023-00990-4","url":null,"abstract":"<div><p>A bisphenol-A derivative, 2,2′-diamino-4,4′-(propane-2,2-diyl)-diphenol (<b>3</b>), was synthesized by nitration of bisphenol-A and then by its reduction. The title compound was characterized by elemental analysis, typical spectroscopic techniques, namely FT-IR, ¹H-NMR, and ¹³C-NMR. The structure of the compound was also determined by single crystal X-ray diffraction method. The compound crystallized in the orthorhombic system with space group P_bcn and a = 15.51106(18) Å, b = 11.6910 (10) Å, c = 7.6473 (7) Å. It is seen that the hydrogen atoms of the -OH groups are in trans-position to the NH2 groups in the crystal structure of the title compound. Moreover, it was observed in the dimeric lattice that the hydrogens of the –NH₂ groups made intramolecular and those of the –OH groups intermolecular hydrogen bonds. The geometry of the compound was optimized by the DFT method and the results were compared with the X-ray diffraction data. Frontier molecular orbitals of the title compound were calculated by using the B3LYP/6-31G(d) method. MEP analysis and Mulliken charge density, Global reactivity and thermodynamic properties were also performed.</p><h3>Graphical Abstract</h3><p>The single crystals of 2,2׳-diamino-4,4׳-(propane-2,2-diyl)-diphenol was obtained and by refining the structure, the –NH⋅⋅⋅O and –OH⋅⋅⋅N hydrogen bonding interactions in the crystal structure was investigated by experimentally and theoretically.</p>\u0000 <div><figure><div><div><picture><source><img></source></picture></div></div></figure></div>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 4","pages":"529 - 539"},"PeriodicalIF":0.8,"publicationDate":"2023-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45580210","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":"Disulfide Versus Diselenide Complexes of Copper: Air-Free and Air-Exposed Syntheses Result in Variable Ligands and Coordination","authors":"Jaime M. Murphy,&nbsp;Amanda M. Owen,&nbsp;Colin D. McMillen,&nbsp;Julia L. Brumaghim","doi":"10.1007/s10870-023-00991-3","DOIUrl":"10.1007/s10870-023-00991-3","url":null,"abstract":"<div><p>Reactions of <i>bis</i>(1-methylimidazole-2)disulfide (MMI^DS) or <i>bis</i>(1-methylimidazole-2)diselenide (MMI^DSe) with Cu(I) result in a variety of products depending on conditions. Under air-free conditions, dinuclear complexes [Cu₂(µ,<i>κ</i>^<i>S</i><i>-</i>MMI)₂(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^DS)₂][BF₄]₂ and [Cu₂(µ,<i>κ</i>^<i>Se</i>-MMI^Se)₂(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^DSe)₂][BF₄]₂ were obtained and structurally characterized. Both complexes show reduction of the MMI^DS or MMI^DSe and subsequent bridging of the thione or selone between the dinuclear Cu(I) centers. Combining MMI^DSe with Cu(I) in air resulted in crystallization of three different complexes from the same reaction mixture, as confirmed by X-ray crystallography. The various products, [Cu(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^MSe)(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^TSe)(CH₃CN)][BF₄]₂, [Cu(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^Se-CH₂-MMI^Se)₂[BF₄]₂, and the co-crystallized [[Cu(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^DSe)₂][Cu(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^Se-CH₂-MMI^Se)][BF₄]₄, indicate that significant reactivity occurs with the availability of air and CH₂Cl₂ solvent. In addition to oxidation of Cu(I) to Cu(II), the MMI^DSe ligands also react to form monoselenide, triselenide, and Se-CH₂-Se bridged selenide ligands.</p><h3>Graphical Abstract</h3><p>Although Cu(I) reactions with <i>bis</i>(1-methylimidazole-2)disulfide (MMI^DS) or <i>bis</i>(1-methylimidazole-2)diselenide (MMI^DSe) under air-free conditions result in formation of [Cu₂(µ,<i>κ</i>^<i>S</i><i>-</i>MMI)₂(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^DS)₂][BF₄]₂ and [Cu₂(µ,<i>κ</i>^<i>Se</i><i>-</i>MMI^Se)₂(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^DSe)₂][BF₄]₂, respectively, treating MMI^DSe with Cu(I) in air results in crystallization of three different complexes from the same reaction mixture: [Cu(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^MSe)(<i> κ</i>^{<i>N,N’</i>}<i>-</i>MMI^TSe)(CH₃CN)][BF₄]₂, [Cu(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^Se-CH₂-MMI^Se)₂[BF₄]₂, and the co-crystallized [[Cu(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI^DSe)₂][Cu(<i>κ</i>^{<i>N,N’</i>}<i>-</i>MMI<sup","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 4","pages":"515 - 528"},"PeriodicalIF":0.8,"publicationDate":"2023-08-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45489639","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}