Borotropic shifting of the [hydrotris(2 ′ -furyl)pyrazol-1-yl]borate ligand in high-coordinate lanthanide complexes
The coordination of hydrotris[3-(2 ′ -furyl)pyrazol-1-yl]borate (Tp2-Fu, C21H16BN6O3) to lanthanide(III) ions is achieved for the first time with the complex [Ln(Tp2-Fu)2](BPh4) · xCH2Cl2 (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( κ 4-Tp2-Fu)( κ 5-Tp2-Fu*)](BPh4) (2) {Tp2-Fu* = hydrobis[3-(2 ′ -furyl)pyrazol-1-yl][5-(2 ′ -furyl)pyrazol-1-yl]borate...
Source: Acta Crystallographica Section C - April 16, 2024 Category: Chemistry Authors: Thomas, J.R. Sulway, S.A. Tags: crystal structure lanthanide high-coordinate borotropic shifting icosahedral dysprosium cerium scorpionate research papers Source Type: research
Synthesis and crystal structure of an iron triazole complex resulting from the unexpected ligand cleavage of a triazolium carbene precursor
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- κ N4)iron(II) μ -oxido-bis[trichloridoferrate(III)] acetonitrile disolvate, [Fe(C9H9N3)4(CH3CN)2][Fe2Cl6O] · 2CH...
Source: Acta Crystallographica Section C - April 12, 2024 Category: Chemistry Authors: Pacholski, R. Durka, K. Buchalski, P. Tags: crystal structure triazole imine hexachloridooxidodiferrate anion iron complex N-heterocyclic carbene organometallic chemistry research papers Source Type: research
Absolute structure determination of Berkecoumarin by X-ray and electron diffraction
This study further demonstrates the utility of dynamical refinement of electron-diffraction data for absolute structure determination. (Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - April 10, 2024 Category: Chemistry Authors: Decato, D. Palatinus, L. Stierle, A. Stierle, D. Tags: crystal structure absolute structure determination electron diffraction microED dynamical refinement Berkecoumarin chromenone natural product research papers Source Type: research
Synthesis, crystal structure and in-silico evaluation of arylsulfonamide Schiff bases for potential activity against colon cancer
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 1H NMR, 13C 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...
Source: Acta Crystallographica Section C - March 28, 2024 Category: Chemistry Authors: Kolade, S.O. Aina, O.S. Gordon, A.T. Hosten, E.C. Olasupo, I.A. Ogunlaja, A.S. Asekun, O.T. Familoni, O.B. Tags: Schiff base arylsulfonamide colon cancer crystal structure molecular docking ADMET research papers Source Type: research
Three polymorphs of a new N,N ′ -dipropylated isoindigo derivative
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, C22H22N2O2, 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. Thermal measurements revealed that Forms I and II are enantiotropically related, and Form II exh...
Source: Acta Crystallographica Section C - March 21, 2024 Category: Chemistry Authors: Jozuka, W. Kim, S. Matsumoto, S. Tags: crystal structure isoindigo indolone dyestuff polymorphs thermal measurements research papers Source Type: research
Crystal structure, intermolecular interactions, charge – density distribution and ADME properties of the acridinium 4-nitrobenzoate and 2-amino-3-methylpyridinium 4-nitrobenzoate salts: a combined experimental and theoretical study
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, C13H10N+ · C7H4NO4 − (I), whereas a mixture of 2-amino-3-methylpyridine and 4-nitrobenzoic acid forms the salt 2-amino-3-methylp...
Source: Acta Crystallographica Section C - March 19, 2024 Category: Chemistry Authors: Balasubramanian, H. Mariappan, P.R. Poomani, K. Tags: intermolecular interaction charge-density distribution crystal structure ADME properties acridinium nitrobenzoate salt theoretical study research papers Source Type: research
Syntheses, crystal structures and intermolecular interactions of six novel pyrimidin-2-yl-substituted triaryltriazoles
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, 1H NMR and ESI – MS spectroscopy, and elemental analysis. In addition, the structures of L2 – 6 and the ethanol monosolvate of L2 (L2 · C2H5OH) have been determined by single-crystal X-ray diffraction. A combi...
Source: Acta Crystallographica Section C - March 12, 2024 Category: Chemistry Authors: Song, H. Peng, R. Zuo, Y. Wang, T. Zhu, D. Tags: synthesis crystal structure pyrimidine triaryltriazole spectral characterization hydrogen bonding Hirshfeld surface analysis research papers Source Type: research
A twofold interpenetrated two-dimensional zinc(II) coordination polymer for the highly sensitive detection of nitrofurantoin in aqueous medium
A novel ZnII coordination polymer, namely, poly[{ μ 2-bis[4-(2-methyl-1H-imidazol-1-yl)phenyl]methanone- κ 2N3:N3 ′ }( μ 2-5-bromobenzene-1,3-dicarboxylato- κ 2O1:O3)zinc(II)], [Zn(C8H3BrO4)(C21H18N4O)]n or [Zn(Br-BDC)(MIPMO)]n, (I), has been synthesized by the solvothermal method using 5-bromoisophthalic acid (Br-H2BDC), bis[4-(2-methyl-1H-imidazol-1-yl)phenyl]methanone (MIPMO) and Zn(NO3)2 · 6H2O. Structure analysis showed that compound (I) displays twofold parallel interwoven sql nets. Fluorescence experiments confirmed that the compound can sensitively and selectively detect nitrofurantoin (NFT) in aqueous mediu...
Source: Acta Crystallographica Section C - March 12, 2024 Category: Chemistry Authors: Wang, Y. Cheng, W.W. Mou, Y. Wen, S. Wang, D. Xue, Y.S. Tags: coordination polymer methanone crystal structure 5-bromoisophthalic acid fluorescence recognition antibiotic nitrofurantoin detection research papers Source Type: research
Crystal structure and analytical profile of 1,2-diphenyl-2-pyrrolidin-1-ylethanone hydrochloride or ` α -D2PV': a synthetic cathinone seized by law enforcement, along with its diluent sugar, myo-inositol
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 K α 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, C18H20NO+ · Cl − · 0.5H2O, (I), a synthetic cathinone cal...
Source: Acta Crystallographica Section C - March 5, 2024 Category: Chemistry Authors: Wood, M.R. Bernal, I. Lalancette, R.A. Tags: crystal structure cathinones bath salts racemic drugs sugars inositol asymmetric units molecular overlays novel psychoactive substances π – interactions hydrogen bonding research papers Source Type: research
Structure and absolute configuration of natural fungal product beauveriolide I, isolated from Cordyceps javanica, determined by 3D electron diffraction
In this study, the absolute structure of beauveriolide I was determined by 3D electron diffraction. The cyclodepsipeptide crystallizes in the space group I2 with lattice parameters a = 40.2744 (4), b = 5.0976 (5), c = 27.698 (4) Å and β = 105.729 (6) ° . After dynamical refinement, its absolute structure was determined by comparing the R factors and calculating the z-scores of the two possible enantiomorphs of beauveriolide I. (Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - February 27, 2024 Category: Chemistry Authors: Gurung, K. Š imek, P. Jegorov, A. Palatinus, L. Tags: crystal structure natural product 3D electron diffraction absolute structure Alzheimer's disease research papers Source Type: research
Oxygen quenching of structurally characterized [5,10,15,20-tetrakis(4-fluoro-2,6-dimethylphenyl)porphyrinato]platinum(II)
The compound [5,10,15,20-tetrakis(4-fluoro-2,6-dimethylphenyl)porphyrinato]platinum(II), [Pt(C52H40F4N4)] 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 ( τ 0 = 66 µ s), 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. (Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - February 26, 2024 Category: Chemistry Authors: Dash, Z.S. Huang, R.Q. Kimber, A.N. Olubajo, O.T. Polk, M. Rancu, O.P. Zhang, L.L. Fu, J. Nagelj, N. Reynolds, K.G. Zheng, S.-L. Dogutan, D.K. Tags: platinum porphyrin oxygen sensing time-resolved absorption spectroscopy crystal structure time-resolved emission spectroscopy research papers Source Type: research
Synthesis and crystal structure of a silver(I) 6-methylmercaptopurine riboside complex
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- κ N7)(nitrato- κ 2O,O ′ )silver(I) 2.32-hydrate, [Ag(NO3)(C11H14N4O4S)2] · 2.32H2O. 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,...
Source: Acta Crystallographica Section C - February 22, 2024 Category: Chemistry Authors: Al-Mahamad, L.L.G. Clegg, W. Tags: synchrotron crystal structure silver complex thiopurine riboside secondary coordination research papers Source Type: research
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
