Thermal-induced transformation of glutamic acid to pyroglutamic acid and self-cocrystallization: a charge – density analysis
Thermal-induced transformation of glutamic acid to pyroglutamic acid is well known. However, confusion remains over the exact temperature at which this happens. Moreover, no diffraction data are available to support the transition. In this article, we make a systematic investigation involving thermal analysis, hot-stage microscopy and single-crystal X-ray diffraction to study a one-pot thermal transition of glutamic acid to pyroglutamic acid and subsequent self-cocrystallization between the product (hydrated pyroglutamic acid) and the unreacted precursor (glutamic acid). The melt upon cooling gave a robust cocrystal, namel...
Source: Acta Crystallographica Section C - January 13, 2022 Category: Chemistry Authors: Akram, S. Mehmood, A. Noureen, S. Ahmed, M. Tags: glutamic acid pyroglutamic acid MoPro cocrystal ELMAM2 crystal structure transferability principle research papers Source Type: research
FeIII in a high-spin state in bis(5-bromosalicylaldehyde 4-ethylthiosemicarbazonato- κ 3O,N1,S)ferrate(III) nitrate monohydrate, the first example of such a cationic FeIII complex unit
The synthesis and crystal structure (100 K) of the title compound, [Fe(C10H11BrN3OS)2]NO3 · H2O, is reported. The asymmetric unit consists of an octahedral [FeIII(HL)2]+ cation, where HL − is H-5-Br-thsa-Et or 5-bromosalicylaldehyde 4-ethylthiosemicarbazonate(1 − ) {systematic name: 4-bromo-2-[(4-ethylthiosemicarbazidoidene)methyl]phenolate}, a nitrate anion and a noncoordinated water molecule. Each HL − ligand binds via the thione S, the imine N and the phenolate O atom, resulting in an FeIIIS2N2O2 chromophore. The ligands are orientated in two perpendicular planes, with the O and S atoms in cis and the N atoms...
Source: Acta Crystallographica Section C - December 30, 2021 Category: Chemistry Authors: Powell, R.E. Lees, M.R. Tizzard, G.J. Koningsbruggen, P.J. van Tags: iron(III) carbazone high spin tautomerism crystal structure magnetic susceptibility research papers Source Type: research
Crystallographic characterization of three cathinone hydrochlorides new on the NPS market: 1-(4-methylphenyl)-2-(pyrrolidin-1-yl)hexan-1-one (4-MPHP), 4-methyl-1-phenyl-2-(pyrrolidin-1-yl)pentan-1-one ( α -PiHP) and 2-(methylamino)-1-(4-methylphenyl)pentan-1-one (4-MPD)
Cathinones belong to a group of compounds of great interest in the new psychoactive substances (NPS) market. Constant changes to the chemical structure made by the producers of these compounds require a quick reaction from analytical laboratories in ascertaining their characteristics. In this article, three cathinone derivatives were characterized by X-ray crystallography. The investigated compounds were confirmed as: 1-[1-(4-methylphenyl)-1-oxohexan-2-yl]pyrrolidin-1-ium chloride (1, C17H26NO+ · Cl − , the hydrochloride of 4-MPHP), 1-(4-methyl-1-oxo-1-phenylpentan-2-yl)pyrrolidin-1-ium chloride (2; C16H24NO+ · Cl − ...
Source: Acta Crystallographica Section C - December 29, 2021 Category: Chemistry Authors: Rojkiewicz, M. Ku ś , P. Ksi ą ż ek, M. Kusz, J. Tags: cathinone new psychoactive substance crystal structure pentanone NPS 4-MPHP α -PiHP 4-MPD research papers Source Type: research
Psilocybin: crystal structure solutions enable phase analysis of prior art and recently patented examples
This article presents new crystal structure solutions for the two anhydrates, Polymorphs A and B, based on Rietveld refinement using laboratory and synchrotron X-ray diffraction data, and density functional theory (DFT) calculations. Utilizing the three solved structures, an investigation was conducted via Rietveld method (RM) based quantitative phase analysis (QPA) to estimate the contribution of the three different forms in powder X-ray diffraction (PXRD) patterns provided by different sources of bulk psilocybin produced between 1963 and 2021. Over the last 57 years, each of these samples quantitatively reflect one or mo...
Source: Acta Crystallographica Section C - December 20, 2021 Category: Chemistry Authors: Sherwood, A.M. Kargbo, R.B. Kaylo, K.W. Cozzi, N.V. Meisenheimer, P. Kaduk, J.A. Tags: psilocybin Rietveld pharmaceutical psychedelic quantitative phase analysis crystal structure research papers Source Type: research
Crystal structures of 3/4-pyridyl-based thiosemicarbazones and related Cu and Ni coordination compounds
In this investigation, the crystal structures of the thio-ligands 3-formylpyridine 4-phenylthiosemicarbazone (C13H12N4S, 1) and 4-benzoylpyridine 4-ethylthiosemicarbazone (C15H16N4S, 2), and of two new coordination compounds, chlorido(3-formylpyridine 4-phenylthiosemicarbazone- κ S)bis(triphenylphosphane- κ P)copper(I) acetonitrile monosolvate, [CuCl(C13H12N4S)(C18H15P)2] · CH3CN, 3, and bis(3-formylpyridine 4-ethylthiosemicarbazonato- κ 2N1,S)nickel(II), [Ni(C9H11N4S)2], 4, are reported. In complex 3, the thio-ligand coordinates in a neutral form to the Cu atom through its S-donor atom, and in complex 4, the anionic t...
Source: Acta Crystallographica Section C - December 20, 2021 Category: Chemistry Authors: Lobana, T.S. Kaushal, M. Bhatia, R. Bala, R. Butcher, R.J. Jasinksi, J.P. Tags: coordination compound thiosemicarbazone copper nickel crystal structure research papers Source Type: research
Syntheses, structures and magnetic properties of two CoII/NiII isostructural coordination polymers based on an asymmetric semirigid tricarboxylate ligand
Two new isostructural complexes, namely, poly[aqua[ μ 3-2-(4-carboxyphenoxy)terephthalato- κ 3O1:O4:O4 ′ ](1,10-phenanthroline- κ 2N,N ′ )cobalt(II)], [Co(C15H8O7)(C12H8N2)(H2O)]n or [Co( μ 3-Hcpota)(phen)(H2O)]n, I, and poly[aqua[ μ 3-2-(4-carboxyphenoxy)terephthalato- κ 3O1:O4:O4 ′ ](1,10-phenanthroline- κ 2N,N ′ )nickel(II)], [Ni(C15H8O7)(C12H8N2)(H2O)]n or [Ni( μ 3-Hcpota)(phen)(H2O)]n, II, have been synthesized by solvothermal reactions. Complexes I and II were fully characterized by IR spectroscopy, elemental analyses, thermogravimetric analyses, and powder and single-crystal X-ray diffraction. They b...
Source: Acta Crystallographica Section C - December 10, 2021 Category: Chemistry Authors: Li, S.-D. Su, F. Zhou, C.-Y. Hu, Q.-L. Li, Y.-Q. Wang, Z.-J. Tags: cobalt(II) nickel(II) two-dimensional coordination polymer semirigid ligand topology magnetism crystal structure research papers Source Type: research
Influence of protonation on the geometry of 2-{[(2,6-dimethylphenoxy)ethyl]amino}-1-phenylethan-1-ol: crystal structures of the free base and of its chloride and 3-hydroxybenzoate salt forms
The aroxyalkylaminoalcohol derivatives are a group of compounds known for their pharmacological action. The crystal structures of four new xylenoxyaminoalcohol derivatives having anticonvulsant activity are reported, namely, 2-{[2-(2,6-dimethylphenoxy)ethyl]amino}-1-phenylethan-1-ol, C18H23NO2, 1, the salt N-[2-(2,6-dimethylphenoxy)ethyl]-1-hydroxy-1-phenylethan-2-aminium 3-hydroxybenzoate, C18H24NO2+ · C7H5O3 − , 2, and two polymorphs of the salt (R)-N-[2-(2,6-dimethylphenoxy)ethyl]-1-hydroxy-1-phenylethan-2-aminium chloride, C18H24NO2+ · Cl − , 3 and 3p. Both polymorphs crystallize in the space group P21212 and eac...
Source: Acta Crystallographica Section C - December 7, 2021 Category: Chemistry Authors: Nitek, W. Kania, A. Marona, H. Waszkielewicz, A.M. Ż es ł awska, E. Tags: hydrogen bonding aminoalkanol aroxyalkyl derivative 3-hydroxybenzoic acid anticonvulsant activity crystal structure research papers Source Type: research
A novel hydrogen-bonding N-oxide – sulfonamide – nitro N — H...O synthon determining the architecture of benzenesulfonamide cocrystals
We present here a more detailed analysis of the N-oxide – sulfonamide – nitro N — H...O ternary complex with quantum theory computations and the Quantum Theory of Atoms in Molecules (QTAIM) approach. Both interactions are present in the crystals, but the O atom of the N-oxide group is found to be a more effective proton acceptor in hydrogen bonds, with an interaction energy about twice that of the nitro-group O atoms. (Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - December 7, 2021 Category: Chemistry Authors: Wzgarda-Raj, K. Rybarczyk-Pirek, A.J. Wojtulewski, S. Palusiak, M. Tags: nitropyridine benzenesulfonamide hydrogen bond halogen bond oxide synthon Hirshfeld surface QTAIM crystal structure research papers Source Type: research
Deep hydration of an Li7 – 3xLa3Zr2MIIIxO12 solid-state electrolyte material: a case study on Al- and Ga-stabilized LLZO
Single crystals of an Li-stuffed, Al- and Ga-stabilized garnet-type solid-state electrolyte material, Li7La3Zr2O12 (LLZO), have been analysed using single-crystal X-ray diffraction to determine the pristine structural state immediately after synthesis via ceramic sintering techniques. Hydrothermal treatment at 150 ° C for 28 d induces a phase transition in the Al-stabilized compound from the commonly observed cubic Ia\overline{3}d structure to the acentric I\overline{4}3d subtype. LiI ions at the interstitial octahedrally (4 + 2-fold) coordinated 48e site are most easily extracted and AlIII ions order onto the...
Source: Acta Crystallographica Section C - December 7, 2021 Category: Chemistry Authors: Redhammer, G.J. Tippelt, G. Rettenwander, D. Tags: solid-state electrolyte LLZO hydrothermal degradation crystal structure structure analysis garnet lattice expansion research papers Source Type: research
Effect of conjugated system extension on structural features and electron-density distribution in charge – transfer difluoroborates
A comparative structural study of two related donor – acceptor pyridine-based BF2 complexes, namely, 3-(dimethylamino)-1,1-difluoro-1H-pyrido[1,2-c][1,3,5,2]oxadiazaborinin-9-ium-1-uide, C8H10BF2N3O (1), and 3-{(1E,3E)-4-[4-(dimethylamino)phenyl]buta-1,3-dien-1-yl}-1,1-difluoro-1H-pyrido[1,2-c][1,3,5,2]oxadiazaborinin-9-ium-1-uide, C18H18BF2N3O (2), containing a dimethylamino group and either the shortest (in 1) or the longest (in 2) charge-transfer path known until now in this family of compounds, is presented. Single-crystal X-ray diffraction analysis supported by computational investigations shed more light on these s...
Source: Acta Crystallographica Section C - November 22, 2021 Category: Chemistry Authors: O ś mia ł owski, B. Dziuk, B. Ejsmont, K. Ch ę ci ń ska, L. Dobrza ń ska, L. Tags: charge transfer fluoroborate computational chemistry borininium crystal structure research papers Source Type: research
Structure determination of riboflavin by synchrotron high-resolution powder X-ray diffraction
The crystal structure of the stable form of vitamin B2 or riboflavin (C17H20N4O6) was solved using high-resolution powder X-ray diffraction (PXRD). The high-resolution PXRD pattern of riboflavin was recorded at room temperature at the European Synchrotron Radiation Facility (Grenoble, France). The starting structural model was generated using a Monte Carlo simulated annealing method. The final structure was obtained through Rietveld refinement. The positions of the H atoms belonging to hydroxy groups were estimated from computational energy minimizations. The symmetry is orthorhombic with the space group P212121 and the fo...
Source: Acta Crystallographica Section C - November 22, 2021 Category: Chemistry Authors: Guerain, M. Affouard, F. Henaff, C. Dejoie, C. Dan è de, F. Siepman, J. Siepman, F. Willart, J.-F. Tags: powder diffraction crystal structure riboflavin Monte Carlo simulated annealing computational energy minimization API synchrotron research papers Source Type: research
Salt formation, hydrogen-bonding patterns and supramolecular architectures of acridine with salicylic and hippuric acid molecules
The intermolecular interactions and salt formation of acridine with 4-aminosalicylic acid, 5-chlorosalicylic acid and hippuric acid were investigated. The salts obtained were acridin-1-ium 4-aminosalicylate (4-amino-2-hydroxybenzoate), C13H10N+ · C7H6NO3 − (I), acridin-1-ium 5-chlorosalicylate (5-chloro-2-hydroxybenzoate), C13H10N+ · C7H4ClO3 − (II), and acridin-1-ium hippurate (2-benzamidoacetate) monohydrate, C13H10N+ · C9H8NO3 − · H2O (III). Acridine is involved in strong intermolecular interactions with the hydroxy group of the three acids, enabling it to form supramolecular assemblies. Hirshfeld surfaces, fi...
Source: Acta Crystallographica Section C - November 19, 2021 Category: Chemistry Authors: Suganya, S. Saravanan, K. Jaganathan, R. Kumaradhas, P. Tags: intermolecular interaction supramolecular assembly Hirshfeld surface charge density salicylic acid hippuric acid crystal structure research papers Source Type: research
A new three-dimensional twofold interpenetrated cadmium(II) metal – organic framework: synthesis, structure and photoluminescence properties. Corrigendum
In the article by Zhang& Wang [Acta Cryst. (2021), C77, 691 – 697], the topology of the title compound is corrected. (Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - November 16, 2021 Category: Chemistry Authors: Zhang, H.-T. Wang, X.-L. Tags: three-dimensional metal – organic framework twofold interpenetrated coordination polymer MOF fluorescence emission decay photoluminescence quantum yield addenda and errata Source Type: research
A three-dimensional manganese(II) coordination polymer with two functional properties: magnetism and photochemical detection
Hydrothermal reaction of Mn2+ with the ditopic ligand 2,5-bis(1H-1,2,4-triazol-1-yl)benzoic acid (Hdtba) resulted in the complex poly[aqua[ μ 3-2,5-bis(1H-1,2,4-triazol-1-yl)benzoato- κ 3N4:N4 ′ :O]chloridomanganese(II)] monohydrate], {[Mn(C11H7N6O2)Cl(H2O)] · H2O}n, (I). Coordination polymer I has been characterized by X-ray diffraction, IR spectroscopy, elemental analysis, thermogravimetry and susceptibility measurements. The topology of I corresponds to a three-dimensional (3,6)-conn net linked by {Mn2Cl2(COO)2} building blocks and dtba − anions. Significant antiferromagnetic exchange is observed within the dinuc...
Source: Acta Crystallographica Section C - November 16, 2021 Category: Chemistry Authors: Zhao, D. An, Y. Guo, T. Yan, J. Song, D. Tags: three-dimensional coordination polymer manganese(II) complex antiferromagnetism photoluminescence luminescence sensing crystal structure benzoic acid dichromate ion detection photochemical detection research papers Source Type: research
Co(NCS)2(abpt)2 and Ni(NCS)2(abpt)2 [abpt is 4-amino-3,5-bis(pyridin-2-yl)-1,2,4-triazole]: structural characterization of polymorphs A and B
The synthesis and structures of bis[4-amino-3,5-bis(pyridin-2-yl)-1,2,4-triazole- κ 2N2,N3]bis(thiocyanato- κ N)cobalt(II), [Co(NCS)2(C12H10N6)2] or Co(NCS)2(abpt)2, and bis[4-amino-3,5-bis(pyridin-2-yl)-1,2,4-triazole- κ 2N2,N3]bis(thiocyanato- κ N)nickel(II), [Ni(NCS)2(C12H10N6)2] or Ni(NCS)2(abpt)2, are reported. In both cases, two polymorphs, A and B, were identified and structurally characterized. For both polymorphs, the structures obtained with the different metals, i.e. CoII or NiII, were found to be isostructural. All of the structures contained an intramolecular N — H...N hydrogen bond, C — H...N interact...
Source: Acta Crystallographica Section C - November 16, 2021 Category: Chemistry Authors: Mason, H.E. Howard, J.A.K. Sparkes, H.A. Tags: polymorphism abpt crystal structure 4-amino-3,5-bis(pyridin-2-yl)-1,2,4-triazole research papers Source Type: research
