Novel first-row transition-metal phosphates: hydrothermal synthesis and crystal structures
Two new compounds, sodium copper nickel diorthophosphate, Na2CuNi(PO4)2 (I), and dimanganese copper diorthophosphate, Mn2Cu(PO4)2 (II), were synthesized hydrothermally, yielding single crystals, and were studied by X-ray diffraction. In the crystal structures, various transition metals of d-elements occupy symmetrically independent crystallographic positions with different coordination geometries. In the crystal structure of Na2NiCu(PO4)2, NiO6 and CuO6 octahedra share edges to form chains that PO4 groups link into a framework with cavities filled with Na atoms. Layered cationic fragments formed from dimers of MnO5 trigona...
Source: Acta Crystallographica Section C - April 11, 2022 Category: Chemistry Authors: Kiriukhina, G.V. Yakubovich, O.V. Verchenko, P.A. Volkov, A.S. Dimitrova, O.V. Tags: transition-metal phosphate crystal structure double-metal phosphate coordination geometry hydrothermal synthesis magnetic material research papers Source Type: research
Crystal structures of cocrystals of 2,7-dihydroxynaphthalene with isoniazid and piracetam
Cocrystals of 2,7-dihydroxynaphthalene (DHN, or naphthalene-2,7-diol) with isoniazid (pyridine-4-carbohydrazide) (INH), denoted DHN – INH [C10H8O2 · C6H7N3O, (I)], and piracetam [2-(2-oxopyrrolidin-1-yl)acetamide] (PIR), denoted DHN – PIR [C10H8O2 · C6H10N2O2, (II)], were obtained by the solvent-assisted grinding method and characterized by IR spectroscopy, powder X-ray diffraction and single-crystal X-ray diffraction. Cocrystal (I) crystallized in the triclinic space group P\overline{1} and showed a 2:2 stoichiometry. DHN and INH molecules are connected by O — H...N(pyridine) and O — H...N(hydrazide) hydrogen bo...
Source: Acta Crystallographica Section C - April 11, 2022 Category: Chemistry Authors: Gonz á lez-Gonz á lez, J.S. Valiente Flores, M.E. Flores-Alamo, M. L ó pez-Mac í as, E. Mart í nez-Mart í nez, F.J. Garc í a-Ortega, H. Tags: cocrystal piracetam isoniazid 2,7-dihydroxynaphthalene crystal structure IR spectroscopy API active pharmaceutical ingredient solvent-assisted grinding research papers Source Type: research
Investigating pair distribution function use in analysis of nanocrystalline hydroxyapatite and carbonate-substituted hydroxyapatite
Hydroxyapatite (HA) is a complex material, which is often nanocrystalline when found within a biological setting. This work has directly compared the structural characteristics derived from data collected using a conventional laboratory-based X-ray diffractometer with those collected from a dedicated pair distribution function (PDF) beamline at Diamond Light Source. In particular, the application of PDF analysis methods to carbonated HA is evaluated. 20 synthetic samples were measured using both X-ray diffraction (XRD) and PDFs. Both Rietveld refinement (of laboratory XRD data) and real-space refinement (of PDF data) were ...
Source: Acta Crystallographica Section C - April 5, 2022 Category: Chemistry Authors: Arnold, E.L. Keeble, D.S. Evans, J.P.O. Greenwood, C. Rogers, K.D. Tags: powder diffraction bone mineral carbonate-substituted hydroxyapatite X-ray diffraction total scattering pair distribution function research papers Source Type: research
Synthesis, crystal structure and bioactivities of α -asaronol
α -Asaronol [or (E)-3 ′ -hydroxyasarone; systematic name: (E)-3-(2,4,5-trimethoxyphenyl)prop-2-en-1-ol; C12H16O4] was synthesized towards the development of a potential antiepileptic drug. Following purification by recrystallization, single crystals of α -asaronol were obtained by a liquid interface diffusion method at room temperature. The product was characterized by 1H and 13C NMR, and FT – IR spectroscopic analysis. X-ray crystallography revealed the title crystal to belong to the orthorhombic space group P212121. Preliminary bioassays with mouse neuroblastoma N2a cells demonstrated the neuroprotective activities...
Source: Acta Crystallographica Section C - April 5, 2022 Category: Chemistry Authors: Zhang, Q.-Z. Zhong, Z.-H. Hao, D. Feng, M.-N. Wang, S.-C. Han, Q.-L. Bai, Y. Xu, D. Liao, S. Xiao, C. Zhang, X.-L. Zheng, X. Tags: α -asaronol crystal structure synthesis crystal growth X-ray crystallography neuroprotective activity research papers Source Type: research
Crystal structures of three β -halolactic acids: hydrogen bonding resulting in differing Z ′
The crystal structures of three β -halolactic acids have been determined, namely, β -chlorolactic acid (systematic name: 3-chloro-2-hydroxypropanoic acid, C3H5ClO3) (I), β -bromolactic acid (systematic name: 3-bromo-2-hydroxypropanoic acid, C3H5BrO3) (II), and β -iodolactic acid (systematic name: 2-hydroxy-3-iodopropanoic acid, C3H5IO3) (III). The number of molecules in the asymmetric unit of each crystal structure (Z ′ ) was found to be two for I and II, and one for III, making I and II isostructural and III unique. The difference between the molecules in the asymmetric units of I and II is due to the direction of t...
Source: Acta Crystallographica Section C - March 30, 2022 Category: Chemistry Authors: Gordon, M.N. Liu, Y. Shafei, I.H. Brown, M.K. Skrabalak, S.E. Tags: crystal structure Z ′ hydrogen bonding halogen bonding Hirshfeld surface halolactic acid research papers Source Type: research
Synthesis and properties of a novel decacyclic S,N-heteroacene
S,N-Heteroacene materials with fused multicyclic heteroaromatics have become increasingly attractive for organic optoelectronic device applications. In this work, the Cadogan ring-closure reaction between the benzene moiety of thieno[3,2-b]indole and 5,6-dinitrobenzo[c][1,2,5]thiadiazole was employed to prepare the novel decacyclic S,N-heteroacene 15,16-dibutyl-14,17-didodecyldithieno[2 ′ ′ ,3 ′ ′ :2 ′ ,3 ′ ]indolo[6 ′ ,7 ′ :4,5]pyrrolo[3,2-e:2 ′ ,3 ′ -g][2,1,3]benzothiadiazole (TIP), C58H76N6S3. The conjugated backbone of TIP is extended in comparison with its octacyclic analogue as the central unit wi...
Source: Acta Crystallographica Section C - March 28, 2022 Category: Chemistry Authors: Li, G. Wang, W. Zhan, C. Xiao, S. Tags: S,N-heteroacene Cadogan reaction crystal structure single-crystal X-ray diffraction π – interaction — H... optoelectronic device research papers Source Type: research
Structural studies of various olmesartan solvates
Seven solvates of the angiotensin II receptor blocker agent olmesartan (C24H26N6O3), namely, the methanol (C24H26N6O3 · CH4O), ethanol (C24H26N6O3 · C2H6O), isopropanol (C24H26N6O3 · C3H8O), isobutanol (C24H26N6O3 · C4H10O), 2-ethoxyethanol (C24H26N6O3 · C4H10O2), chloroform (C24H26N6O3 · CHCl3) and acetonitrile (C24H26N6O3 · C2H3N) solvates, were successfully obtained. The crystal structures were determined using the single-crystal X-ray diffraction technique and the structural features are described, each solvate containing one molecule of olmesartan and one of solvent in the asymmetric unit. The samples were also...
Source: Acta Crystallographica Section C - March 25, 2022 Category: Chemistry Authors: Grosu, I.G. Martin, F. Turza, A. Miclaus, M. Kacso, I. Borodi, G. Tags: olmesartan isostructural solid form crystal structure angiotensin II receptor blocker agent research papers Source Type: research
Synthesis, structural analysis, and docking studies with SARS-CoV-2 of a trinuclear zinc complex with N-phenylanthranilic acid ligands
The structure of a trinuclear zinc complex, hexakis( μ 2-2-anilinobenzoato)diaquatrizinc(II), [Zn2(C13H10NO2)6(H2O)2] or (NPA)6Zn3(H2O)2 (NPA is 2-anilinobenzoate or N-phenylanthranilate), is reported. The complex crystallizes in the triclinic space group P\overline{1} and the central ZnII atom is located on an inversion center. The NPA ligand is found to coordinate via the carboxylate O atoms with unique C — O bond lengths that support an unequal distribution of resonance over the carboxylate fragment. The axial H2O ligands form hydrogen bonds with neighboring molecules that stabilize the supramolecular system in rigid...
Source: Acta Crystallographica Section C - March 8, 2022 Category: Chemistry Authors: Mbani O., A.L. Bonnand, E.F. Paboudam, A.G. Brannon, J.P. Gardner-Ricossa, K.D. Stieber, S.C.E. Agwara, M.O. Tags: trinuclear phenylanthranilic acid NPA zinc inorganic chemistry organometallic SARS-CoV-2 molecular docking crystal structure research papers Source Type: research
d-Mannosamine hydrochloride (2-amino-2-deoxy-d-mannose hydrochloride): ionic hydrogen bonding in saccharides involving chloride and aminium ions
d-Mannosamine hydrochloride (2-amino-2-deoxy-d-mannose hydrochloride), C6H14NO5+ · Cl − , (I), crystallized from a methanol/ethyl acetate/n-hexane solvent mixture at room temperature in a 4C1 chair conformation that is slightly distorted towards the C3,O5B form. A comparison of the structural parameters of (I) with the corresponding parameters in α -d-glucosamine hydrochloride, (II), and β -d-galactosamine hydrochloride, (III)/(III ′ ), was undertaken to evaluate the effects of ionic hydrogen bonding on structural properties. Three types of ionic hydrogen bonds are present in the crystals of (I) – (III)/(III ′ )...
Source: Acta Crystallographica Section C - March 4, 2022 Category: Chemistry Authors: Lin, J. Oliver, A.G. Serianni, A.S. Tags: d-mannosamine hydrochloride 2-amino-2-deoxy-d-mannose hydrochloride crystal structure anomeric disorder ionic hydrogen bonding research papers Source Type: research
Synthesis and structure of two isomers of a molybdenum(II) 2-butyne complex stabilized by bioinspired S,N-bidentate ligands
The synthesis and structural determination of two isomers of the molybdenum(II) complex ( η 2-but-2-yne)carbonylbis[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)benzenethiolato- κ 2N,S]molybdenum(II), [Mo(C11H12NOS)2(C4H6)(CO)] or Mo(CO)(C2Me2)(S-Phoz)2, are presented. The N,N-cis – S,S-trans isomer 1 shows quite different bond lengths to the metal atom [Mo — N = 2.4715 (10) versus 2.3404 (11) Å ; Mo — S = 2.4673 (3) versus 2.3665 (3) Å ]. In the N,N-trans – S,S-cis isomer 2, which is isotypic with the corresponding W complex, the Mo — N bond lengths [2.236 (2) and 2.203 (...
Source: Acta Crystallographica Section C - March 4, 2022 Category: Chemistry Authors: Ehweiner, M.A. Belaj, F. M ö sch-Zanetti, N.C. Tags: isomer 2-butyne complex molybdenum(II) benzenethiol crystal structure research papers Source Type: research
An X-ray investigation of stereoselectivity in the interactions of [Co(en)3]3+ with [Co(ox)3]3 − (en is ethane-1,2-diamine and ox is oxalate)
The X-ray structure of racemic tris(ethane-1,2-diamine- κ 2N,N ′ )cobalt(III) tris(oxalato- κ 2O1,O2)cobaltate(III) pentahydrate, [Co(C2H8N2)3][Co(C2O4)3] · 5H2O or [Co(en)3][Co(ox)3] · 5H2O, has been determined. Hydrogen-bonding interactions along the C3-axis of the [Co(en)3]3+ cation with the [Co(ox)3]3 − anion are heterochiral, while those perpendicular to this axis are homochiral. Implications for the interpretation of chiral discriminations and induction in electron-transfer reactions in solution are discussed. (Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - March 4, 2022 Category: Chemistry Authors: Gallagher, M.K. Baker, J. Black, R. Oliver, A.G. Lappin, A.G. Tags: hydrogen bonding chiral interactions crystal structure cobalt ethanediamine research papers Source Type: research
Experimental and theoretical investigations on a furan-2-carboxamide-bearing thiazole: synthesis, molecular characterization by IR/NMR/XRD, electronic characterization by DFT, Hirshfeld surface analysis and biological activity
A thiazole-based heterocyclic amide, namely, N-(thiazol-2-yl)furan-2-carboxamide, C8H6N2O2S, was synthesized and investigated for its antimicrobial activity. The structure was characterized by elemental analysis and IR, 1H NMR, and 13C NMR spectroscopy. The molecular and electronic structures were investigated experimentally by single-crystal X-ray diffraction (XRD) and theoretically by density functional theory (DFT) modelling. The compound crystallized in the monoclinic space group P21/n and the asymmetric unit contains two symmetrically independent molecules. Several noncovalent interactions were recorded by XRD and ana...
Source: Acta Crystallographica Section C - February 28, 2022 Category: Chemistry Authors: Ç akmak, Ş . Ko ş ar K ı rca, B. Veyiso ğ lu, A. Yakan, H. Ersanl ı , C.C. K ü t ü k, H. Tags: thiazolamide antimicrobial activity spectroscopic evaluation biological activity furan carboxamide XRD Hirshfeld surface crystal structure research papers Source Type: research
A new bioactive cocrystal of coumarin-3-carboxylic acid and thiourea: detailed structural features and biological activity studies
Cocrystallization is a phenomenon widely used to enhance the biological and physicochemical properties of active pharmaceutical ingredients (APIs). The present study deals with the synthesis of a cocrystal of coumarin-3-carboxylic acid (2-oxochromene-3-carboxylic acid, C10H6O4), a synthetic analogue of the naturally occurring antioxidant coumarin, with thiourea (CH4N2S) using the neat grinding method. The purity and homogeneity of the coumarin-3-carboxylic acid – thiourea (1/1) cocrystal was confirmed by single-crystal X-ray diffraction, FT – IR analysis and thermal stability studies based on differential scanning calo...
Source: Acta Crystallographica Section C - February 16, 2022 Category: Chemistry Authors: Shahbaz, M. Khan, U.A. Chaudhary, M.I. Yousuf, S. Tags: antileishmanial crystal engineering cocrystal antioxidant DFT DPPH radical scavenger crystal structure coumarin-3-carboxylic acid thiourea research papers Source Type: research
Insights on structure and interactions of 2-amino-4-methoxy-6-methylpyrimidinium salts with 4-aminosalicylate and 5-chlorosalicylate: a combined experimental and theoretical charge – density analysis
The proton-transfer complexes 2-amino-4-methoxy-6-methylpyrimidinium (2A4M6MP) 4-aminosalicylate (4AMSA), C6H10N3O+ · C7H6NO3 − , I, and 5-chlorosalicylate (5ClSA), C6H10N3O+ · C7H4ClO3 − , II, were synthesized by slow evaporation and crystallized. The crystal structures of both I and II were determined by single-crystal X-ray structure analysis. The crystal structures of both salts exhibit O — H...O, N — H...O, N — H...N and C — H...O interactions in their crystals. The 4AMSA and 5ClSA anions in combination with the 2A4M6MP cations form distinct synthons, which are represented by the graph-set notations R22(...
Source: Acta Crystallographica Section C - February 14, 2022 Category: Chemistry Authors: Suganya, S. Saravanan, K. Hemalatha, B. Jaganathan, R. Kumaradhas, P. Tags: salt pyrimidinium salicylate proton transfer intermolecular interaction crystal structure Hirshfeld surface fingerprint plot charge density research papers Source Type: research
Synthesis and structures of three benzoannelated macrobicyclic diamides
We report the synthesis and structures of 9,10,20,21-tetrahydro-5,14-(ethanooxyethano)dibenzo[e,q][1,4,10,13,7,16]tetraoxadiazacyclooctadecine-6,13-dione [systematic name: 8,11,21,24,29-pentaoxa-1,18-diazatetracyclo[16.8.5.02,7.012,17]hentriaconta-2,4,6,12(17),13,15-hexaene-19,26-dione C24H28N2O8, I], 6,7,9,10,12,13,20,21-octahydro-5,14-(ethanooxyethano)dibenzo[e,q][1,4,10,13,7,16]tetraoxadiazacyclooctadecine-23,27-dione (8,11,21,24,29-pentaoxa-1,18-diazatetracyclo[16.8.5.02,7.012,17]hentriaconta-2,4,6,12,14,16-hexaene-27,31-dione; C24H28N2O7, II), and 9,10,20,21-tetrahydro-5,14-(ethanooxyethanooxyethano)dibenzo[e,q][1,4,1...
Source: Acta Crystallographica Section C - February 14, 2022 Category: Chemistry Authors: Smith, G.L.N. Taylor, R.W. Tags: benzoannelated macrobicyclic diamides high dilution crystal structure cryptand research papers Source Type: research
