Journal of Chemical Crystallography最新文献

A novel Cd(II) Coordination Polymer, [Cd(L)₂(SO₄)₂(H₂O)₂][Cd(H₂O)₆]·4H₂O (CP 1) (L = (1,1'-((2,3,5,6-tetramethyl-1,4-phenylene)bis(methylene))bis(4-carboxypyridin-1-ium)chloride)), is prepared and characterized by single-crystal X-ray diffraction, elemental analysis, powder X-ray diffraction, infrared spectrum, thermogravimetric analysis, solid-state fluorescence properties and CIE analysis. The single-crystal X-ray diffraction studies reveal that the ligand HLClO₄·H₂O crystallizes in the monoclinic P2₁/n space group, while CP 1 crystallized in the triclinic P-1 space group with two distinct Cd(II) centers. Abundant hydrogen bonds produce the 3D supramolecular structure of CP 1. The experimental results show that the CP 1 has good thermal stability and has potential applications in blue luminescent materials.

Graphical Abstract

The single crystal of a novel Cd (II) coordination polymer based on pyridinium zwitterionic ligand were synthesized in this work.

Methyl 3-O-α-d-glucopyranosyl 2-acetamido-2-deoxy-α-d-galactopyranoside as a monohydrate, C₁₅H₂₇NO₁₁·H₂O, crystallizes in space group P2₁2₁2₁, with four molecules in the unit cell. It constitutes the methyl glycoside of the carbohydrate part of the teichoic acid type polysaccharide from Micrococcus sp. A1, in which the disaccharides are joined through phosphodiester linkages. The conformation of the disaccharide is described by the glycosidic torsion angles ϕ =  − 31° and ψ =  + 1°, and the hydroxymethyl groups of the constituent monosaccharides are present in the gg and gt conformations for the sugar residues having the gluco- and galacto-configuration, respectively. For the N-acetyl group at C2 of the galactosamine residue the torsion angle τ_H = 147°, i.e., the amide proton has an antiperiplanar relationship to H2 of the sugar ring. The structure shows extensive hydrogen bonding along the a-direction, including the water molecule, and forms sheets with hydrophilic interactions within the sheets as a result of hydrogen bonding between disaccharides as well as hydrophobic interactions between the sheets, in particular, amongst methyl groups of the N-acetyl group of the α-d-GalpNAc residue in the disaccharides.

Graphical Abstract

The structure of the title disaccharide as a monohydrate, C₁₅H₂₇NO₁₁·H₂O, which shows extensive hydrogen bonding as well as hydrophobic interactions, was determined from minute crystals using synchrotron radiation and verified by solid state DFT calculations using plane waves.

The new compound 4-hydroxy-1-[(4-nitrophenyl)sulfonyl]pyrrolidine-2-carboxyllic acid was obtained by the reaction of 4-hydroxyproline with 4-nitrobenzenesulfonyl chloride. The compound was characterized using single crystal X-ray diffraction studies. Spectroscopic methods including NMR, FTIR, ES-MS, and UV were employed for further structural analysis of the synthesized compound. The title compound was found to have crystallized in an orthorhombic crystal system with space group P2₁2₁2₁. The S1-N1 bond length of 1.628 (2) Å was a strong indication of the formation of the title compound. The absence of characteristic downfield ¹H NMR peak of pyrrolidine ring and the presence of S–N stretching vibration at 857.82 cm⁻¹ on the FTIR are strong indications for the formation of the sulfonamide. The experimental study was complemented with computations at the B3LYP/6-311G +  + (d,p) level of theory to gain more understanding of interactions in the compound at the molecular level. Noncovalent interaction, Hirsfeld surface analysis and interaction energy calculations were employed in the analysis of the supramolecular architecture of the compound. Predicted ADMET parameters, awarded suitable bioavailability credentials, while the molecular docking study indicated that the compound enchants promising inhibition prospects against dihydropteroate synthase, DNA topoisomerase, and SARS-CoV-2 spike.

Graphical Abstract

Herein we present the solid state structure, noncovalent interaction and spectroscopic analysis of a prospective bioactive compound 4-hydroxy-1-[(4-nitrophenyl)sulphonyl]pyrrolidine-2-carboxyllic acid.

Strychnine is well known as a highly toxic alkaloid derived from the plant Strychnos nux-vomica. It has been applied for chiral separations as a resolving agent for co-crystallizations, as a standard for chromatographic separations, as a rodenticide, as a natural therapy and stimulant, and as a poisonous plot device in works of fiction. Dissolving strychnine into the common organic solvent dichloromethane results in the spontaneous crystallization of the title compound N-(chloromethyl)strychninium chloride. Crystals of the compound were isolated in the orthorhombic space group P2₁2₁2₁ with a = 7.6819(2) Å, b = 7.9621(2) Å, c = 30.7170(9) Å, α = 90°, β = 90°, γ = 90°. The crystal structure has bilayers of N-(chloromethyl)strychninium cations with corresponding bilayers of chloride ions interacting to the cations through C–H hydrogen bonds.

Graphical Abstract

The novel third-order nonlinear optical organic material 4-fluoro-N-[4-(diethylamino)benzylidene]aniline (FDEABA) is synthesized and single crystals of FDEABA are grown using the slow evaporation method. The placement of the protons is confirmed by nuclear magnetic resonance spectral analysis. Employing Fourier transform infrared spectral analysis, vibrational frequencies of various functional groups of the FDEABA compound are identified. The three-dimensional crystal structure of the grown crystal is elucidated using single crystal X-ray diffraction studies, which reveal that the compound FDEABA crystallized in the monoclinic non-centrosymmetric space group P2₁. Intermolecular interactions are studied using Hirshfeld surface analysis and compared with similar structures of halogen-substituted benzylideneaniline derivatives. Thermal stability of FDEABA is measured using thermogravimetric and differential thermal analyses and the melting point of the synthesized FDEABA compound is 51 °C. Open aperture Z-scan measurements carried out at 532 nm using 5 ns laser pulses reveal nonlinear optical absorption leading to strong optical limiting behaviour, which can be useful in the protection of eyes and sensitive optical detectors from harmful laser radiation.

Graphical Abstract

The reaction of the N,N-diethyl-N'-(p-nitrobenzoyl)thiourea with K₂[PtCl₄] results in the complex of configurational cis-[Pt(L-kS,O)₂], and structurally characterized by elemental analyses, FT-IR, ¹H NMR, ¹³H NMR, UV–Vis spectroscopy, and cis-[Pt(L-kS,O)₂] complex have been also characterized by a single-crystal X-ray diffraction study. The cis-[Pt(L-kS,O)₂] crystallizes in the monoclinic crystal system, space group P2₁/c, with Z = 4, and unit cell parameters, a = 15.09299(15) Å, b = 15.26600(14) Å, c = 14.39268(14) Å, α = 90°, β = 107.6347(11)° and γ = 90°. The single-crystal diffraction analysis of the complex shows that the molecular configuration of cis-[Pt(L-kS,O)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 cis-[Pt(L-kS,O)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.

Graphical Abstract

In this paper, single-crystal X-ray analysis shows cis-[Pt(L-kS,O)₂] belongs to monoclinic crystal system, space group P2₁/c. The connectivity of the ligand to the metal as 2:1 and the platinum atom is coordinated with two N,N-diethyl-N'-(p-nitrobenzoyl)thiourea ligands in a distorted square-planar geometry.

The crystal structures of 8-R¹-7-bromo-3-tert-butyl-1-R²-pyrazolo[5,1-c][1,2,4]triazin-4(1H)-ones 1a–c, 2a,c (R¹ = CN, CO₂Et, NO₂, R² = H, 1:1 and 3:1 solvates with DMSO; R¹ = CN, CO₂Et, R² = CH₂Boc), 8-R¹-7-bromo-3-tert-butyl-1-R²-1,4-dihydropyrazolo[5,1-c][1,2,4]triazin-4-ols 3a,b (R¹ = CN, R² = n-Bu; R¹ = Br, R² = CH₂Boc), 1,4-dihydro- and aromatic 7-R³-3-tert-butyl-4-R⁴-8-methylpyrazolo[5,1-c][1,2,4]triazines 5a,b, 6 (R³ = H, R⁴ = n-Pr; R³ = Br, R⁴ = n-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.

Graphical Abstract

The crystal structures of ten 3-tert-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.

Two new proton transfer salts (HABT)⁺(SA)⁻ (1) and (HABT)⁺₂(ADSA)²⁻·2H₂O (2) 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 1 and R₃³(10) for 2. The intramolecular hydrogen bond creates the cyclic S(6) motif in both structures (1 and 2). For salt 1, crystallization took place in the P2(1)/c space group of the monoclinic system, and for salt 2 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 {Bacillus subtilis, Listeria monocytogenes (ATCC 7644), Enterococcus faecalis (ATCC 29212), Staphylococcus aureus (NRRL B-767)}, Gram negative bacteria {Escherichia coli (ATCC 25922), Pseudomonas aeruginosa (ATCC 27853)} and fungus {Candida albicans (F89)}. Minimum inhibitory concentrations (MIC) of synthesized salts were compared with antibacterial (levofloxacin cefepime, vancomycin) and antifungal (Fluconazole) reference compounds.

Graphical Abstract