Acta Crystallographica. Section C, Structural Chemistry

The coordination of hydrotris[3-(2'-furyl)pyrazol-1-yl]borate (Tp2-Fu , C21 H16 BN6 O3 ) to lanthanide(III) ions is achieved for the first time with the complex [Ln(Tp2-Fu )2 ](BPh4 )·xCH2 Cl2 (1-Ln has Ln = Ce and x = 2; 1-Dy has Ln = Dy and x = 1). This was accomplished via both hydrous (Ln = Ce) and anhydrous methods (Ln = Dy). When isolating the dysprosium analogue, the filtrate produced a second crop of crystals which were revealed to be the 1,2-borotropic-shifted product [Dy(κ4 -Tp2-Fu )(κ5 -Tp2-Fu *)](BPh4 ) (2) {Tp2-Fu * = hydrobis[3-(2'-furyl)pyrazol-1-yl][5-(2'-furyl)pyrazol-1-yl]borate}...

Typically reactions of N-heterocyclic carbenes with transition metals are straightforward and require a carbene salt, a base strong enough to deprotonate such a salt and a metal. Yet when carbene precursors are in the form of triazolium salts, reaction may not proceed as easily as expected. In our work, we intended to obtain a triazolylidene complex of iron(II) chloride, but due to the presence of small amounts of water in the tetrahydrofuran solvent used, bis(acetonitrile)tetrakis(1-benzyl-1H-1,2,4-triazole-κN4 )iron(II) μ-oxido-bis[trichloridoferrate(III)] acetonitrile disolvate, [Fe(C9 H9 N3 )4 (CH3 CN)2 ][Fe2 Cl6 O]·2CH3 CN - an interesting anion with a linear geometry of the O atom - was formed instead of the iron carbene complex...

X-ray and electron diffraction methods independently identify the S-enantiomer of Berkecoumarin [systematic name: (S)-8-hydroxy-3-(2-hydroxypropyl)-6-methoxy-2H-chromen-2-one]. Isolated from Berkeley Pit Lake Penicillium sp., Berkecoumarin is a natural product with a light-atom composition (C13 H14 O5 ) that challenges in-house absolute structure determination by anomalous scattering. This study further demonstrates the utility of dynamical refinement of electron-diffraction data for absolute structure determination...

A newly synthesized N,N'-dipropyl-substituted isoindigo derivative, namely, 1-propyl-3-(1-propyl-1,2-dihydro-2-oxo-3H-indol-3-ylidene)-1,3-dihydro-2H-indol-2-one, C22 H22 N2 O2 , was found to have three polymorphic forms (denoted Forms I, II and III) under various crystallization conditions. Crystal structure analysis indicated that Form III had a significantly different molecular conformation from the other two polymorphs. Their different packing arrangements were correlated with differences in the intermolecular interactions...

Acridines are a class of bioactive agents which exhibit high biological stability and the ability to intercalate with DNA; they have a wide range of applications. Pyridine derivatives have a wide range of biological activities. To enhance the properties of acridine and 2-amino-3-methylpyridine as the active pharmaceutical ingredient (API), 4-nitrobenzoic acid was chosen as a coformer. In the present study, a mixture of acridine and 4-nitrobenzoic acid forms the salt acridinium 4-nitrobenzoate, C13 H10 N+ ·C7 H4 NO4 - (I), whereas a mixture of 2-amino-3-methylpyridine and 4-nitrobenzoic acid forms the salt 2-amino-3-methylpyridinium 4-nitrobenzoate, C6 H9 N2 + ·C7 H4 NO4 - (II)...

A novel ZnII coordination polymer, namely, poly[{μ2 -bis[4-(2-methyl-1H-imidazol-1-yl)phenyl]methanone-κ2 N3 :N3' }(μ2 -5-bromobenzene-1,3-dicarboxylato-κ2 O1 :O3 )zinc(II)], [Zn(C8 H3 BrO4 )(C21 H18 N4 O)]n or [Zn(Br-BDC)(MIPMO)]n , (I), has been synthesized by the solvothermal method using 5-bromoisophthalic acid (Br-H2 BDC), bis[4-(2-methyl-1H-imidazol-1-yl)phenyl]methanone (MIPMO) and Zn(NO3 )2 ·6H2 O. Structure analysis showed that compound (I) displays twofold parallel interwoven sql nets...

Six new pyrimidin-2-yl-substituted triaryltriazoles, namely, 4-(4-R-phenyl)-3-(pyridin-2-yl)-5-(pyrimidin-2-yl)-1,2,4-triazoles [L1 : R = methoxy (OCH3 ); L2 : R = methyl (CH3 ); L3 : R = nil (H); L4 : R = bromo (Br); L5 : R = chloro (Cl); L6 : R = fluoro (F)] have been successfully synthesized with yields in the range 68.3-81.7%. Compounds L1-6 have been characterized by UV-Vis, FT-IR, 1 H NMR and ESI-MS spectroscopy, and elemental analysis. In addition, the structures of L2-6 and the ethanol monosolvate of L2 (L2 ·C2 H5 OH) have been determined by single-crystal X-ray diffraction...

A confiscated package of street drugs was characterized by the usual mass spectral (MS) and FT-IR analyses. The confiscated powder material was highly crystalline and was found to consist of two very different species, accidentally of sizes convenient for X-ray diffraction. Thus, one each was selected and redundant complete sets of data were collected at 100 K using Cu Kα radiation. The selected crystals contained: (a) 1,2-diphenyl-2-(pyrrolidin-1-yl)ethanone hydrochloride hemihydrate or 1-(2-oxo-1,2-diphenylethyl)pyrrolidin-1-ium chloride hemihydrate, C18 H20 NO+ ·Cl- ·0...

Beauveriolides, including the main beauveriolide I {systematic name: (3R,6S,9S,13S)-9-benzyl-13-[(2S)-hexan-2-yl]-6-methyl-3-(2-methylpropyl)-1-oxa-4,7,10-triazacyclotridecane-2,5,8,11-tetrone, C27 H41 N3 O5 }, are a series of cyclodepsipeptides that have shown promising results in the treatment of Alzheimer's disease and in the prevention of foam cell formation in atherosclerosis. Their crystal structure studies have been difficult due to their tiny crystal size and fibre-like morphology, until now. Recent developments in 3D electron diffraction methodology have made it possible to accurately study the crystal structures of submicron crystals by overcoming the problems of beam sensitivity and dynamical scattering...

The compound [5,10,15,20-tetrakis(4-fluoro-2,6-dimethylphenyl)porphyrinato]platinum(II), [Pt(C52 H40 F4 N4 )] or Pt(II)TFP, has been synthesized and structurally characterized by single-crystal X-ray crystallography. The Pt porphyrin exhibits a long-lived phosphorescent excited state (τ0  = 66 µs), which has been characterized by transient absorption and emission spectroscopy. The phosphorescence is extremely sensitive to oxygen, as reflected by a quenching rate constant of 5.0 × 108  M-1  s-1 , and as measured by Stern-Volmer quenching analysis...

Silver nitrate reacts with 6-methylmercaptopurine riboside (6-MMPR) in aqueous solution containing methanol and dimethyl sulfoxide at room temperature to give a colourless crystalline complex, namely, bis(6-methylmercaptopurine riboside-κN7 )(nitrato-κ2 O,O')silver(I) 2.32-hydrate, [Ag(NO3 )(C11 H14 N4 O4 S)2 ]·2.32H2 O. The crystal structure, determined from synchrotron diffraction data, shows a central AgI ion on a crystallographic twofold rotation axis, coordinated in an almost linear fashion by two 6-MMPR ligands via atom N7 (purine numbering), with the nitrate counter-ion loosely coordinated as a bidentate ligand, forming a discrete molecular complex as an approximate dihydrate...

The structures of five ammonium salt forms of monosulfonated azo dyes, derivatives of 4-(2-phenyldiazen-1-yl)benzenesulfonate, with the general formula [NH4 ][O3 S(C6 H4 )NN(C6 H3 )RR']·XH2 O [R = OH, NH2 or N(C2 H4 OH)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...

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, C22 H25 BrFN4 O2 + ·C17 H19 N2 O5 S- ·C2 H3 N, 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...

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, C15 H26 O·0...

The crystal structure of a new 1:1 cocrystal of carbamazepine and S-naproxen (C15 H12 N2 O·C14 H14 O3 ) 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 P21 21 21 (No...

Three new compounds, namely, 5-fluorocytosine-urea (2/1), 2C4 H4 FN3 O·CH4 N2 O, (I), 5-fluorocytosine-5-fluorocytosinium 3,5-dinitrosalicylate-water (2/1/1), 2C4 H4 FN3 O·C4 H5 FN3 O+ ·C7 H2 N2 O7 - ·H2 O, (II), and 2-amino-4-chloro-6-methylpyrimidine-6-chloronicotinic acid (1/1), C6 H4 ClNO2 ·C5 H6 ClN3 , (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 [R2 2 (8) ring motif], one formed via N-H...

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), C10 H13 N5 O3 , 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...

This report presents a comprehensive investigation into the synthesis and characterization of Schiff base compounds derived from benzenesulfonamide. The synthesis process, involved the reaction between N-cycloamino-2-sulfanilamide and various substituted o-salicylaldehydes, resulted in a set of compounds that were subjected to rigorous characterization using advanced spectral techniques, including 1 H NMR, 13 C NMR and FT-IR spectroscopy, and single-crystal X-ray diffraction. Furthermore, an in-depth assessment of the synthesized compounds was conducted through Absorption, Distribution, Metabolism, Excretion and Toxicity (ADMET) analysis, in conjunction with docking studies, to elucidate their pharmacokinetic profiles and potential...

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 Cu3 Eu2 (PBA)6 (NO3 )6 ·H2 O. This material is a very promising dimethylformamide (DMF) molecular chemical sensor...

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, C15 H17 N2 S+ ·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...