Isostructural behaviour in ammonium and potassium salt forms of sulfonated azo dyes
The structures of five ammonium salt forms of monosulfonated azo dyes, derivatives of 4-(2-phenyldiazen-1-yl)benzenesulfonate, with the general formula [NH4][O3S(C6H4)NN(C6H3)RR ′ ] · XH2O [R = OH, NH2 or N(C2H4OH)2; R ′ = H or OH] are presented. All form simple layered structures with alternating hydrophobic (organic) and hydrophilic (cation, solvent and polar groups) layers. To assess for isostructural behaviour of the ammonium cation with M+ ions, the packing of these structures is compared with literature examples. To aid this comparison, the corresponding structures of four potassium salt forms of the monosulfona...
Source: Acta Crystallographica Section C - February 15, 2024 Category: Chemistry Authors: Kennedy, A.R. Kirkhouse, J.B.A. McCarney, K.M. Puissegur, O. Tags: single-crystal X-ray diffraction dye salt selection sulfonated azo pseudo-alkali metal crystal structure isostructural research papers Source Type: research
Crystal structure and Hirshfeld surface analysis of a salt of antineoplastic kinase inhibitor vandetanib
A salt of vandetanib, namely, 4-({4-[(4-bromo-2-fluorophenyl)amino]-6-methoxyquinazolin-7-yl}methoxy)-1-methylpiperazin-1-ium 2-(butylamino)-4-phenoxy-6-sulfamoylbenzoate acetonitrile monosolvate, C22H25BrFN4O2+ · C17H19N2O5S − · C2H3N, composed of kinase inhibitor vandetanib and sulfamyl diuretic bumetanide in a 1:1 molar ratio, is reported. There is proton transfer between the piperidine ring of vandetanib and the carboxyl group of bumetanide to form the salt. In the vandetanib cation, the arene and pyrimidine rings are not coplanar, their planes subtending a dihedral angle of 60.47 (14) ° . The roles of the int...
Source: Acta Crystallographica Section C - February 7, 2024 Category: Chemistry Authors: Yang, H. Liang, M. Tian, F. Tags: Hirshfeld surface analysis salt vandetanib bumetanide crystal structure intermolecular interaction antineoplastic kinase inhibitor sulfamyl diuretic research papers Source Type: research
High-pressure study of a 3d – 4f heterometallic CuEu – organic skeleton
We prepared a 3d – 4f heterobimetallic CuEu – organic framework NBU-8 with a density of 1921 kg m − 3 belonging to the family of dense packing materials (dense metal – organic frameworks or MOFs). This MOF material was prepared from 4-(pyrimidin-5-yl)benzoic acid (HPBA) with a bifunctional ligand site as a tripodal ligand and Cu2+ and Eu3+ as the metal centres; the molecular formula is Cu3Eu2(PBA)6(NO3)6 · H2O. This material is a very promising dimethylformamide (DMF) molecular chemical sensor. Systematic high-pressure studies of NBU-8 were carried out by powder X-ray diffraction, high-pressure X-ray diffr...
Source: Acta Crystallographica Section C - January 31, 2024 Category: Chemistry Authors: Yang, K. Yang, Y. Yao, Z. Cheng, S. Cui, X. Wang, X. Han, Y. Yi, F. Mo, G. Tags: metal – organic framework MOF high pressure X-ray diffraction Rietveld refinement bulk modulus DMF sensor molecular dynamics research papers Source Type: research
(+)-Cedrol hemihydrate: a natural product derived from drying eastern red cedar (Juniperus virginiana) wood
Cedrol-like compounds are of pharmacological interest due to their diverse range of medicinal effects and are used globally in traditional medicines and cosmetics. Many cedrol tautomers are known from molecular studies but few have been studied in crystalline form by X-ray diffraction. Acicular white crystals collected from the wood of eastern red cedar (Juniperus virginiana) are determined to be (+)-cedrol hemihydrate, namely, (1S,2R,5S,7R,8R)-2,6,6,8-tetramethyltricyclo[5.3.1.01,5]undecan-8-ol hemihydrate, C15H26O · 0.5H2O, a novel packing of two unique cedrol molecules (Z ′ = 2) with a single water molecule [space gr...
Source: Acta Crystallographica Section C - January 28, 2024 Category: Chemistry Authors: Chakoumakos, B.C. Wang, X. Tags: cedrol eastern red cedar pharmacological interest traditional medicine chirality tricyclic sesquiterpene crystal structure spiral chain hydrogen bonding research papers Source Type: research
Using synchrotron high-resolution powder X-ray diffraction for the structure determination of a new cocrystal formed by two active principle ingredients
The crystal structure of a new 1:1 cocrystal of carbamazepine and S-naproxen (C15H12N2O · C14H14O3) was solved from powder X-ray diffraction (PXRD). The PXRD pattern was measured at the high-resolution beamline CRISTAL at synchrotron SOLEIL (France). The structure was solved using Monte Carlo simulated annealing, then refined with Rietveld refinement. The positions of the H atoms were obtained from density functional theory (DFT) ground-state calculations. The symmetry is orthorhombic with the space group P212121 (No. 19) and the following lattice parameters: a = 33.5486 (9), b = 26.4223 (6), c = 5.3651 (10) ...
Source: Acta Crystallographica Section C - January 28, 2024 Category: Chemistry Authors: Guerain, M. Correia, N. Roca-Paix ã o, L. Chevreau, H. Affouard, F. Tags: powder diffraction API carbamazepine naproxen cocrystal PXRD crystal structure liquid-assisted grinding research papers Source Type: research
Hydrogen-bonding interactions in 5-fluorocytosine – urea (2/1), 5-fluorocytosine – 5-fluorocytosinium 3,5-dinitrosalicylate – water (2/1/1) and 2-amino-4-chloro-6-methylpyrimidine – 6-chloronicotinic acid (1/1)
Three new compounds, namely, 5-fluorocytosine – urea (2/1), 2C4H4FN3O · CH4N2O, (I), 5-fluorocytosine – 5-fluorocytosinium 3,5-dinitrosalicylate – water (2/1/1), 2C4H4FN3O · C4H5FN3O+ · C7H2N2O7 − · H2O, (II), and 2-amino-4-chloro-6-methylpyrimidine – 6-chloronicotinic acid (1/1), C6H4ClNO2 · C5H6ClN3, (III), have been synthesized and characterized by single-crystal X-ray diffraction. In compound (I), 5-fluorocytosine (5FC) molecules A and B form two different homosynthons [R22(8) ring motif], one formed via N — H...O hydrogen bonds and the second via N — H...N hydrogen bonds. In addition to this interac...
Source: Acta Crystallographica Section C - January 23, 2024 Category: Chemistry Authors: Sangavi, M. Kumaraguru, N. Butcher, R.J. McMillen, C.D. Tags: homosynthon ring motif hydrogen bonds supramolecular network dimeric synthon primary motif base pair stacking interactions crystal structure research papers Source Type: research
α -d-2 ′ -Deoxyadenosine, an irradiation product of canonical DNA and a component of anomeric nucleic acids: crystal structure, packing and Hirshfeld surface analysis
α -d-2 ′ -Deoxyribonucleosides are products of the γ -irradiation of DNA under oxygen-free conditions and are constituents of anomeric DNA. They are not found as natural building blocks of canonical DNA. Reports on their conformational properties are limited. Herein, the single-crystal X-ray structure of α -d-2 ′ -deoxyadenosine ( α -dA), C10H13N5O3, and its conformational parameters were determined. In the crystalline state, α -dA forms two conformers in the asymmetric unit which are connected by hydrogen bonds. The sugar moiety of each conformer is arranged in a `clamp'-like fashion with respect to the other con...
Source: Acta Crystallographica Section C - January 22, 2024 Category: Chemistry Authors: Leonard, P. Zhang, A. Budow-Busse, S. Daniliuc, C. Seela, F. Tags: α -2 ′ -deoxyadenosine anomer crystal structure crystal packing nucleoside Hirshfeld surface analysis research papers Source Type: research
X-ray crystallographic structure of a novel enantiopure chiral isothiourea with potential applications in enantioselective synthesis
The synthesis of a chiral isothiourea, namely, (4aR,8aR)-3-phenyl-4a,5,6,7,8,8a-hexahydrobenzo[4,5]imidazo[2,1-b]thiazol-9-ium bromide, C15H17N2S+ · Br − , with potential organocatalytic and anti-inflammatory activity is reported. The preparation of the heterocycle of interest was carried out in two high-yielding steps. The hydrobromide salt of the isothiourea of interest provided suitable crystals for X-ray diffraction analysis, the results of which are reported. Salient observations from this analysis are the near perpendicular arrangement of the phenyl ring and the mean plane of the heterocycle. This conformational c...
Source: Acta Crystallographica Section C - January 1, 2024 Category: Chemistry Authors: Savin, J.A. Á vila-Ort í z, C.G. Leyva-Ram í rez, M.A. Juaristi, E. Tags: resolution chiral diamine chiral isothiourea crystal structure asymmetric organocatalysis halogen bond enantiopure research papers Source Type: research
Synthesis and crystal structure of Ba2Y0.87(1)Mn1.71(1)Te5
We report the structural characterization of a new quaternary telluride, Ba2Y0.87(1)Mn1.71(1)Te5, which was synthesized by the direct reaction of the elements inside a vacuum-sealed fused-silica tube. The quaternary phase is the first member of the Ba – M – Mn – Te system (M = Sc and Y). The composition and structure of the phase were elucidated using SEM – EDX (scanning electron microscopy – energy dispersive X-ray spectrometry) and single-crystal X-ray diffraction (SCXRD) studies. The title phase is nonstoichiometric and crystallizes in the monoclinic system (space group C2/m) having the refined unit-cell pa...
Source: Acta Crystallographica Section C - January 1, 2024 Category: Chemistry Authors: Yadav, S. Prakash, J. Tags: chalcogenide solid-state synthesis crystal structure quaternary telluride research papers Source Type: research
Crystal structures of three uranyl – acetate – bipyridine complexes crystallized from hydraulic fracking fluid
Hydraulic fracking exposes shale plays to acidic hydraulic fracking fluid (HFF), releasing toxic uranium (U) along with the desired oil and gas. With no existing methods to ensure U remains sequestered in the shale, this study sought to add organic ligands to HFF to explore potential U retention in shale plays. To test this possibility, incubations were set up in which uranyl acetate and one organic bipyridine ligand (either 2,2 ′ -, 2,3 ′ -, 2,4 ′ -, or 4,4 ′ -bipyridine) were added to pristine HFF as the crystallization medium. After several months and complete evaporation of all volatiles, bulk yellow crystallin...
Source: Acta Crystallographica Section C - December 6, 2023 Category: Chemistry Authors: Whittington, A.A. Keimowitz, A.R. Tanski, J.M. Tags: crystal structure uranyl acetate bipyridine complex uranium retention hydraulic fracking research papers Source Type: research
An efficient one-pot synthesis of pyrazole complexes formed in situ: synthesis, crystal structure, Hirshfeld surface analysis and in vitro biological properties
The molecular crystals of monomeric and dimeric pyrazole complexes were prepared via one-pot syntheses. These are dichloridobis(3,5-dimethyl-1H-pyrazole- κ N1)cobalt/zinc(0.2/0.8), [Co0.20Zn0.80Cl2(C5H8N2)2] or [Co0.2Zn0.8Cl2(3,5-dmp)2] (1), and bis( μ -3,5-dimethyl-1H-pyrazole)- κ 2N1:N2; κ 2N2:N1-bis[bromido/chlorido(0.7/0.3)bis(3,5-dimethyl-1H-pyrazole- κ N1)cobalt/zinc(0.1/0.9)], [Co0.20Zn1.80Br1.40Cl0.60(C5H7N2)2(C5H8N2)2] or [Co0.1Zn0.9Br0.7Cl0.3( μ -3,5-dmp)(3,5-dmp)]2 (2). The isolated complexes contain 3,5-dimethylpyrazole (3,5-dmp) ligands formed in situ from the decomposition of 1-hydroxymethyl-3,5-dimethy...
Source: Acta Crystallographica Section C - November 30, 2023 Category: Chemistry Authors: Adach, A. Tyszka-Czochara, M. Daszkiewicz, M. Tags: one-pot synthesis pyrazole IR spectroscopy cytotoxicity crystal structure cobalt zinc research papers Source Type: research
Molecular simulation of imperfect structure I CO2 hydrate growth in brine
In order to investigate the viability of carbon dioxide (CO2) storage in seawater, molecular dynamics techniques were employed to study the dynamic evolution of CO2 hydrate in saline water. The simulation was conducted under specific conditions: a temperature of 275 K, a pressure of 10 MPa and a simulated marine environment achieved using a 3.4 wt% sodium chloride (NaCl) solution. The total simulation time was 1000 ns. The results of the simulation indicate that the pre-existence of CO2 hydrate crystals as seeds leads to rapid growth of CO2 hydrate. However, analysis of the F3 and F4 order parameters reveal...
Source: Acta Crystallographica Section C - November 29, 2023 Category: Chemistry Authors: Fu, Z. Jing, X. Zhou, L. Luo, Q. Zhang, P. Tags: CO2 hydrate molecular dynamics simulation order parameters climate change IPCC carbon capture research papers Source Type: research
Structures and biological activity of three 2-(pyridin-2-yl)-1H-benzimidazole derivatives
Two new 2-(pyridin-2-yl)-1H-benzimidazole derivatives, namely, 2-(4-phenoxypyridin-2-yl)-1H-benzimidazole, C18H13N3O, and 2-[4-(4-fluorophenoxy)pyridin-2-yl]-1H-benzimidazole, C18H12FN3O, were synthesized and characterized by NMR spectroscopy. Crystal structure, biological activity and ADME analyses were performed for these two new compounds and a third compound, namely, 5,6-dimethyl-2-[4-(4-phenylpiperazin-1-yl)pyridin-2-yl]-1H-benzimidazole methanol monosolvate, C24H25N5 · CH3OH, the synthesis of which had been described previously. All three compounds have a similar chain hydrogen-bonding pattern. One of them (the fluo...
Source: Acta Crystallographica Section C - November 8, 2023 Category: Chemistry Authors: Sukiennik, J. Olczak, A. Gobis, K. Korona-G ł owniak, I. Su ś niak, K. Fruzi ń ski, A. Szczesio, M. Tags: crystal structure benzimidazole ADME antibacterial activity research papers Source Type: research
1-(Pyridin-4-yl)-4-thiopyridine (PTP) in the crystalline state – pure PTP and a cocrystal and salt
The first in situ preparation and single-crystal structure identification of pure 1-(pyridin-4-yl)-4-thiopyridine (PTP), C10H8N2S, a simple and basic derivative of mercaptopyridine, from a crystallization mixture is described. The same PTP was found in two multicomponent crystal forms with 3,5-dinitrobenzoic acid as a classic two-component cocrystal, namely, 1-(pyridin-4-yl)-4-thiopyridine – 3,5-dinitrobenzoic acid (1/1), C7H4N2O6 · C10H8N2S, and with 2-hydroxy-3,5-dinitrobenzoic acid as a salt formed via proton transfer from the hydroxy group of the acid to the pyridyl N atom of PTP, namely, 4-(4-sulfanylidene-1,4-dihy...
Source: Acta Crystallographica Section C - November 7, 2023 Category: Chemistry Authors: Wzgarda-Raj, K. Wla ź lak, M. Ksi ą ź kiewicz, O. Palusiak, M. Tags: 4-thiopyridine 4-mercaptopyridine crystal structure proton affinity cocrystal salt crystal engineering research papers Source Type: research
Studies of κ 2- and κ 3-tripyridylamine complexes of ruthenium and π -stacking by pyridyls
The reaction of tris(pyridin-2-yl)amine with [CyRuCl2]2 (Cy = p-isopropyltoluene or cymene) in refluxing diglyme led to the formation of cis-[RuCl2{ κ 2-(2-py)3N}2] · CHCl3 (1a) after recrystallization from chloroform/pentane, or cis-dichloridobis[tris(pyridin-2-yl)amine- κ 2N,N ′ ]ruthenium(II) dichloromethane disolvate, [RuCl2(C15H12N4)2] · 2CH2Cl2 or cis-[RuCl2{ κ 2-(2-py)3N}2] · 2CH2Cl2 (1b). Treatment of 1a with one equivalent of silver(I) hexafluoridoantimonate in dichloromethane gave [RuCl{ κ 2-(2-py)3N}{ κ 3-(2-py)3N}][SbF6] · CH2Cl2 (2a). Crystallization of 2a from chloroform provided chlorido[tris(pyri...
Source: Acta Crystallographica Section C - November 6, 2023 Category: Chemistry Authors: Faller, J. Chase, K.J. Parr, J. Mercado, B. Tags: tripyridylamine crystal structure ruthenium solvent encapsulation methylene chloride tetramer polypyridyl research papers Source Type: research
