Journal of Chemical Crystallography最新文献

Crystal structures of two 2-nitropropene derivatives, namely 1,4-bis((E)-2-nitroprop-1-enyl)benzene and 4,4′-bis((E)-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.

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The X-ray structures of 1,4-bis((E)-2-nitroprop-1-enyl)benzene and 4,4′-bis((E)-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.

The synthesis and structural details of a mixed-ligand Cu(II) coordination compound, specifically catena-poly[bis(dicyanamido)(1,10-phenanthroline-5,6-dione)copper(II)] 1, 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 1 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.

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Synthesis, Structure and Theoretical Calculations of a Unique Ladder Chain Containing the Dicyanamido Ligand (dca), Consisting of 2 µ_1,5-dca Bridged Dinuclear Cu₂(dca)₂Units and Having µ_1,3-dca Bridges along the Chain.

One sentence essence:

catena-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

A novel Cadmium(II) coordination polymer, namely {[Cd(L)(bpmh)_0.5(DMA)(H₂O)]}_n (CP 1), has been successfully synthesized under solvothermal conditions using H₂L (5-(1-oxoisoindion-2-yl)isophthalic acid) and bpmh ((1E,2E)-1,2-bis(pyridine-4-ylmethylene)hydrazine) ligand. The CP 1 is well described by single-crystal X-ray diffraction, PXRD, FT-IR, TGA and solid-state fluorescence properties. X-ray single crystal diffraction analysis shows that CP 1 crystallizes in the P-1 space group, and possesses 1D ladder chains, which were further connected by hydrogen bonding interactions to form 3D supramolecular architecture. Results of the property studies showed that we successfully synthesized a pure phase fluorescent material with good thermal stability and has potential applications for the development of future fluorescent materials.(II)

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Single-crystal X-ray analysis shows that a novel Cd (II) fluorescence coordination polymer based on nitrogen-containing aromatic ligands was described in this work.

Two chiral ferrocenylamine alcohols of (R)-[Fe(η⁵-C₅H₅){η⁵-C₅H₄CH₂NHCH(ⁱPr)(CH₂OH)}] (1) and (R)-[Fe(η⁵-C₅H₅){η⁵-C₅H₄CH₂NHCH(C₆H₅)(CH₂OH)}] (2) were synthesized by condensation reaction of ferrocenylformaldehyde and chiral aminoalcohols followed by the reduction with sodium borohydride. The crystal structures of the two compounds were determined by single crystal X-ray diffraction. Compound 1 crystallizes in the orthorhombic space group P2₁2₁2 with a = 16.600(8) Å, b = 28.990(14) Å, c = 6.531(3) Å, and Z = 8. Compound 21.13H₂O crystallizes in the monoclinic space group I2 with a = 22.671(4) Å, b = 6.2481(10) Å, c = 22.112(4) Å, β = 96.763(12)°, and Z = 8.

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The ionic compound N-(2-hydroxyethyl)piperazinium chloride (HEPH)Cl, containing a piperazinium cation with a + 1 charge, was crystallized in the orthorhombic space group P2₁2₁2₁. The unit cell parameters were determined to be a = 8.6083(3) Å, b = 8.8523(3) Å, and c = 10.7405(4) Å. The volume of the unit cell was found to be 818.46(5) ų, with a Z value of 4. Refinement yielded R[F² > 2σ(F²)] = 0.018, wR(F²) = 0.028, and a goodness-of-fit parameter of S = 1.77. The crystal structure reveals the presence of three hydrogen bonds: O1–H1o1···Cl1, N1–H1n1···N2, and N1–H2n1···Cl1, which contribute to the specific molecular arrangements within the crystal lattice.Electrochemical properties of (HEPH)Cl were examined by cyclic voltammetry (CV). Molecular docking experiments were conducted to assess the interactions of (HEPH)Cl with Mycobacterium tuberculosis DNA gyrase, coronavirus main protease, Plasmodium falciparum protein, and human serum albumin.

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N-(2-hydroxyethyl)piperazinium chloride cation uniquely adopts a chair conformation carrying a +1 charge, stabilized by crucial hydrogen bonding interactions that enhance molecular recognition and binding affinity observed in docking study.

Crystals of mono- and dibromo as well as two isomeric tribromocymantrenes [Mn(C₅H_5-nBr_n)(CO)₂(PPh₃)] (n = 1–3) were obtained and examined by X-ray diffraction. The degree of substitution has only minor influence on bond lengths and angles. However, the relative orientations of bromo substituents and PPh₃ ligand as well as relative orientation of the cyclopentadienyl ring and the MnC₂P tripod are sensitive to the number and position of bromines. All compounds show weak Br…O interactions, mostly combined with hydrogen bonds, while Br…Br interactions are unimportant. These interactions lead to sometimes complicated chain structures.

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In the crystal structures of the bromocymantrenes [Mn(C₅H_5-nBr_n)(CO)₂(PPh₃₎] (n = 1–3) a combination of H bonds and Br…O/Br…Br interactions leads to one-dimensional molecular chains or double-chains, which are not further connected in the other dimensions.

4-(2-amino-2-oxoethyl) phenyl 4-methylbenzenesulfonate (APMBS), a novel compound, has been synthesized and characterized by spectro-analytical techniques. X-ray diffraction data reveals it crystallizes in the triclinic crystal system with space group (Poverline{1}). The structure is stabilized through strong N–H⋯O, weak C–H⋯O and C–H⋯π hydrogen bond interactions yielding a supramolecular structure. The N1A–H1AA⋯O4A, C4–H4⋯O3, and C14–H14⋯Cg1 (Ring: C8–C13) interactions link the molecules into dimers, while the interaction C9-H9–O2 results in the formation of a molecular chain along the a-axis. The optimized structural geometry, by and large, as calculated using DFT and HF techniques is in conformity with the corresponding X-ray data. The DFT computation further aid in the follow up investigations including frontier molecular orbitals (FMOs), density of states (DOS), atomic charges, and molecular electrostatic potential surface (MEP). For a comprehensive description of various molecular intersections, Hirsheld surface and fingerprint plots analysis has been reported, besides the combined atoms-in-molecules (QTAIM) and reduced density gradient (RDG) analysis. Docking studies have been performed against the target protein Tubulin-Colchicine: Stathmin-Like Domain Complex.

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A new coordination polymer, namely, {[Zn(DTPP)(H₂O)₂]·H₂O}_n (H₂DTPP = 3-(3,5-di(2H-tetrazol-5-yl)phenoxy)pyridine, compound 1), was successfully assembled by using a new semirigid tripodal nitrogen-containing heterotopic ligand and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectroscopy, TG, and luminescence. X-ray single-crystal diffraction analysis revealed that compound 1 crystallizes in an orthorhombic crystal system with space groups of Ibca. It is a 2D coordination network with (4·8²) topology, and the 2D networks are further connected by hydrogen bonds between coordinated water molecules and tetrazole N atoms to form a 3D supramolecular framework. Moreover, compound 1 exhibits intense blue emission centered at 345 nm upon excitation at 276 nm and has the ability to sense Fe³⁺ via photoluminescence quenching.

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A new coordination polymer synthesized from a new semirigid tripodal nitrogen-containing heterotopic ligand, {[Zn(DTPP)(H₂O)₂]·H₂O}_n, was characterized.

New polymorphs of (2-(chloro(pyrrol-2-ylidene)methyl)pyrrole)-difluoro-borane (1) and (2-(chloro(4-ethyl-3,5-dimethyl-2H-pyrrol-2-ylidene)methyl)pyrrole)-4-ethyl-3,5-dimethyl-1H-pyrrolato)-difluoro-borane (2) were identified using single crystal X-ray diffraction. The new polymorph of 1 crystallises in the triclinic, P-1 space group with an asymmetric unit comprising two crystallographically-independent molecules (Z′ = 2). The differences between this structure and that of the known polymorph of 1 are attributed to the formation of two distinct dimer motifs in each polymorph and the packing between these dimer units. The new polymorph structure of 2, exhibits a similar asymmetric unit to the known form, comprising 3 molecules (Zʹ = 3). The two structures differ in the orientation of the molecules within the trimeric asymmetric unit and the manner in which these trimers pack along the crystallographic [010] direction.

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The triclinic polymorph of 8-chloro BODIPY exhibits an asymmetric unit with two crystallographically-independent molecules.

In this study, we have synthesized a novel organic–inorganic hybrid crystal 4-nitrobenzyl-4-aminopyridinium tetrachlorocuprate(II) [4NO₂Bz-4NH₂Py]₂[CuCl₄](1). The single-crystal X-ray diffraction analysis revealed that the crystal belongs to the triclinic space group P–1, and consists of four [4NO₂Bz-4NH₂Py]⁺ cations and two [CuCl₄]²⁻ anions. O⋯π, C–H⋯π, π⋯π, N–H⋯Cl, C–H⋯Cl, C–H⋯O, and C–H⋯N weak interactions in the crystals play an important role in facilitating the stacking and stabilization of the crystals. The different types of contribution have been quantified by the calculation of Hirshfeld surface percentage and depicted by fingerprint plots. The bulk phase purity, homogeneity, and morphology of the desired compound were checked using powder XRD, and SEM–EDX analysis. Vibrational, optical, and thermal properties were investigated by FT-IR, UV–Vis spectrum, and TG–DTA measurements of [4NO₂Bz-4NH₂Py]₂[CuCl₄](1), respectively. The low energy gap (2.41 eV) suggested that the crystal was a suitable semiconductor material for optical applications. In addition, the compound presented good bactericidal activity against E. coli and S. aureus.

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A novel organic–inorganic hybrid material, 4-nitrobenzyl-4-aminopyridinium tetrachlorocuprate(II), has been synthesised and characterized with a study of its crystal structure, vibrational spectra, weak interaction, Hirshfield surface, thermal stability and antibacterial activity.