Metal halide coordination compounds with quinazolin-4(3H)-one
Three coordination compounds of quinazolin-4(3H)-one (quinoz; C8H6N2O) with divalent group 12 halides are reported. In all complexes, coordination occurs via the nitrogen atom ortho to the quinazolinone carbonyl group. In the two chain polymers with composition [MX2(quinoz)], viz. (M = Cd, X = Br), catena-poly[[[quinazolin-4(3H)-one- κ N3]cadmium(II)]-di- μ -bromido], [CdBr2(C8H6N2O)]n (I), and M = Hg, X = Cl, catena-poly[[[quinazolin-4(3H)-one- κ N3]mercury(II)]-di- μ -chlorido], [HgCl2(C8H6N2O)]n (II), the divalent cations are five-coordinate, with four bridging halide and one terminal quinoz ligand. The CdII atom in...
Source: Acta Crystallographica Section E - June 6, 2023 Category: Chemistry Authors: Turgunov, K.K. Englert, U. Tags: crystal structure cadmium(II) coordination polymer halide-bridged coordination polymers mercury(II) coordination polymer quinazolinone coordination tetrahedral cadmium(II) complex. research communications Source Type: research
Crystal structure and Hirshfeld-surface analysis of a monoclinic polymorph of 2-amino-5-chlorobenzophenone oxime at 90 K
The synthesis and crystal structure of a monoclinic polymorph of 2-amino-5-chlorobenzophenone oxime, C13H11ClN2O, are presented. The molecular conformation results from twisting of the phenyl and 2-amino-5-chloro benzene rings attached to the oxime group, which subtend a dihedral angle of 80.53 (4) ° . In the crystal, centrosymmetric dimers are formed as a result of pairs of strong O — H...N hydrogen bonds. A comparison is made to a previously known triclinic polymorph, including differences in atom – atom contacts obtained via a Hirshfeld-surface analysis. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - June 6, 2023 Category: Chemistry Authors: Geetha, D. Kavitha, C.N. Divakara, T.R. Basavaraju, Y.B. Yathirajan, H.S. Parkin, S. Tags: crystal structure benzophenone oxime polymorph Hirshfeld surface research communications Source Type: research
Golden oldies: ten crystallography articles that we think must be read
We have selected a set of ten `golden oldies', diverse crystallography articles to illustrate important moments in the development of our field of science and which form landmark papers in crystallography. They are a mixture of `science pull and technology push'. For each of our choices, we firstly created a new title that emphasizes how the paper's importance worked out from today's perspective. Then we describe the core details and impacts of each paper, with some quotations and a selected figure or two. Ten is an arbitrary number of highlights and our choice is personal. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - June 6, 2023 Category: Chemistry Authors: Massera, C. Helliwell, J.R. Tags: landmark papers in crystallography science pull technology push research communications Source Type: research
Synthesis, crystal structure, Hirshfeld surface analysis and DFT study of the 1,1 ′ -(buta-1,3-diyne-1,4-diyl)bis(cyclohexan-1-ol)
The title compound, C16H22O2, was synthesized in order to obtain its guest-free form because `wheel-and-axle'-shaped molecules tend to crystallize from solutions as solvates or host – guest molecules. It crystallizes in the monoclinic space group P2/c with two crystallographically non-equivalent molecules, one situated on an inversion center and the other on a twofold axis. The rod-like 1,3-diyne fragments have the usual linear geometry. In the crystal, O — H ... O bonds form eight-membered rings of the R44(8) type, linking molecules into layers. The Hirshfeld surface analysis indicates that the largest contributions a...
Source: Acta Crystallographica Section E - June 2, 2023 Category: Chemistry Authors: Tirkasheva, S.I. Ziyadullaev, O.E. Eshimbetov, A.G. Ibragimov, B.T. Ashurov, J.M. Tags: synthesis 1,1 ′ -(buta-1,3-diyne-1,4-diyl)bis(cyclohexan-1-ol) crystal structure hydrogen bond Hirshfeld surface analysis DFT study. research communications Source Type: research
Crystal structure of Ag3Dy2(NO3)9 and quantitative comparison to isotypic compounds
Single crystals of Ag3Dy2(NO3)9 (trisilver didysprosium nonanitrate) were obtained from a mixture of AgNO3 and Dy(NO3)3 · 5 H2O. The new compound crystallizes in space group P4132 (No. 213) with a = 13.2004 (4) Å , V = 2300.2 (2) Å 3, Z = 4. The Ag and Dy cations are coordinated by five and six bidentate nitrate anions, respectively. Ag3Dy2(NO3)9 is isostructural to several compounds that include alkali metals or ammonium and lanthanide cations, but silver and dysprosium are included for the first time and feature the smallest ion radii observed for this structure type to date. Crystal structures of isot...
Source: Acta Crystallographica Section E - June 2, 2023 Category: Chemistry Authors: Klein, W. Tags: crystal structure dysprosium silver nitrate research communications Source Type: research
Crystal structure and Hirshfeld surface analysis of (1H-imidazole- κ N3)[N-(2-oxidobenzylidene)tyrosinato- κ 3O,N,O ′ ]copper(II)
The title copper(II) complex, [Cu(C16H13NO4)(C3H4N2)], consists of a tridentate ligand synthesized from l-tyrosine and salicylaldehyde. One imidazole molecule is additionally coordinating to the copper(II) ion. The crystal structure features N — H...O, O — H...O and C — H...O hydrogen bonds. The Hirshfeld surface analysis indicates that the most important contributions to the packing are from H...H (37.9%), C...H (28.2%) and O...H/H...O (21.2%) contacts. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - June 2, 2023 Category: Chemistry Authors: Suzuki, S. Akiyama, Y. Nakane, D. Akitsu, T. Tags: Schiff base complex copper amino acid Hirshfeld analysis crystal structure research communications Source Type: research
Structure of (R,R)-4-bromo-2-{4-[4-bromo-1-(4-toluenesulfonyl)-1H-pyrrol-2-yl]-1,3-dinitrobutan-2-yl}-1-(4-toluenesulfonyl)-1H-pyrrole, another ostensible by-product in the synthesis of geminal-dimethyl hydrodipyrrins
The crystal structure of (R,R)-4-bromo-2-{4-[4-bromo-1-(4-toluenesulfonyl)-1H-pyrrol-2-yl]-1,3-dinitrobutan-2-yl}-1-(4-toluenesulfonyl)-1H-pyrrole (1, C26H24Br2N4O8S2) is presented. The title compound was isolated in suitable yield as a by-product in our synthesis of geminal-dimethyl hydrodipyrrins. We observe an unforeseen enantiomeric resolution both in the bulk sample and the crystal of 1, with distinct C — H...O (Cmethyl — H...Onitro, Csp3 — H...Osulfonyl) interactions observed in the enantiomers present, along with other interactions, namely C5-pyrrolyl — H...Osulfonyl, forming a polymer along the crystallogra...
Source: Acta Crystallographica Section E - June 2, 2023 Category: Chemistry Authors: Sample, H.C. Twamley, B. Senge, M.O. Tags: crystal structure enantiomer resolution pyrrole by-product research communications Source Type: research
David G. Watson (1934 – 2023)
(Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - May 31, 2023 Category: Chemistry Authors: Clegg, W. Tags: obituary obituaries Source Type: research
Synthesis and crystal structure of bis(2-phthalimidoethyl)ammonium chloride dihydrate
The title compound {systematic name: bis[2-(1,3-dioxoisoindol-2-yl)ethyl]azanium chloride dihydrate}, C20H18N3O4+ · Cl − · 2H2O, is a phthalimide-protected polyamine that was synthesized by a previous method. It was characterized by ESI – MS, 1H NMR, and FT – IR. Crystals were grown from a solution of H2O and 0.1 M HCl. The central nitrogen atom is protonated and forms hydrogen bonds with the chloride ion and a water molecule. The two phthalimide units make a dihedral angle of 22.07 (3) ° . The crystal packing features a hydrogen-bond network, two-coordinated chloride, and off-set π – π stacking. (Source: ...
Source: Acta Crystallographica Section E - May 26, 2023 Category: Chemistry Authors: Young, B.S. Lee, J.L. Gembicky, M. Bailey, J. Smith, G.L.N. Tags: crystal structure phthalimides π – interactions tripodal ligand research communications Source Type: research
Synthesis and crystal structure of 2-[(2,3,5,6-tetrafluoropyridin-4-yl)amino]ethyl methacrylate
In the title compound, C11H10F4N2O2, the conformation about the N — C — C — O bond is gauche [torsion angle = 61.84 (13) ° ]. In the crystal, N — H...O hydrogen bonds link the molecules into [010] chains, which are cross-linked by C — H...F and C — H... π contacts. Hirshfeld surface analysis was conducted to aid in the visualization of these various influences on the packing. This analysis showed that the largest contribution to the surface contacts arises from F...H/H...F interactions (35.6%), followed by O...H/H...O (17.8%) and H...H (12.7%). (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - May 26, 2023 Category: Chemistry Authors: Overstreet, S.M.J. Genzia, I.M. Nguyen, A. Auleciems, Z.J. Jennings, A.R. Peloquin, A.J. Tags: crystal structure perfluoropyridine — H...F interaction research communications Source Type: research
Crystal structure and Hirshfeld surface analysis of 5-oxo-7-phenyl-2-(phenylamino)-1H-[1,2,4]triazolo[1,5-a]pyridine-6,8-dicarbonitrile dimethyl sulfoxide monosolvate
In the title compound, C20H12N6O · C2H6OS, the [1,2,4]triazolo[1,5-a]pyridine ring system is almost planar and makes dihedral angles of 16.33 (7) and 46.80 (7) ° , respectively, with the phenylamino and phenyl rings. In the crystal, molecules are linked by intermolecular N — H...O and C — H...O hydrogen bonds into chains along the b-axis direction through the dimethyl sulfoxide solvent molecule, forming C(10)R21(6) motifs. These chains are connected via S — O... π interactions, π – π stacking interactions between the pyridine rings [centroid-to-centroid distance = 3.6662 (9) Å ] and van der Wa...
Source: Acta Crystallographica Section E - May 26, 2023 Category: Chemistry Authors: Naghiyev, F.N. Khrustalev, V.N. Mamedov, H.M. Akkurt, M. Khalilov, A.N. Bhattarai, A. Mamedov, İ .G. Tags: crystal structure [1,2,4]triazolo[1,5-a]pyridine hydrogen bond Hirshfeld surface analysis research communications Source Type: research
2-[3-(1H-Benzimidazol-2-yl)propyl]-1H-benzimidazol-3-ium 3,4,5-trihydroxybenzoate – 1,3-bis(1H-benzimidazol-2-yl)propane – ethyl acetate (2/1/2.94): co-crystallization between a salt, a neutral molecule and a solvent
The chemical formula of the title compound, 2C17H17N4+ · 2C7H5O5 − · C17H16N4 · 2.94C4H8O2, was established by X-ray diffraction of a single-crystal obtained by reacting 1,3-bis(benzimidazol-2-yl)propane (L) and gallic acid (HGal) in ethyl acetate. The molecular structure can be described as a salt (HL)+(Gal) − co-crystallized with a molecule L, with a stoichiometric relation of 2:1. Moreover, large voids in the crystal are filled with ethyl acetate, the amount of which was estimated by using a solvent mask during structure refinement, affording the chemical formula (HL+ · Gal − )2 · L · (C4H8O2)2.94. The arran...
Source: Acta Crystallographica Section E - May 23, 2023 Category: Chemistry Authors: Palacios Rodr í guez, J.C. Mendoza, A. Sosa Rivadeneyra, M. Bern è s, S. Tags: crystal structure co-crystal hydrogen bonds supramolecular structure solvent mask research communications Source Type: research
Synthesis and crystal structure studies of 5-(trifluoromethyl)-1,3,4-thiadiazol-2(3H)-one at 180 K
The synthesis and crystal structure of C3HF3N2OS, systematic name 5-(trifluoromethyl)-1,3,4-thiadiazol-2(3H)-one (5-TMD-2-one), a compound containing the pharmacologically important heterocycle 1,3,4-thiadiazole, is presented. The asymmetric unit comprises six independent molecules (Z ′ = 6), all of which are planar. The r.m.s. deviations from each mean plane range from 0.0063 to 0.0381 Å , not including the CF3 fluorine atoms. Within the crystal, two of the molecules form hydrogen-bonded dimers that in turn combine with inversion-related copies to form tetrameric constructs. Similar tetramers, but lacking inversion...
Source: Acta Crystallographica Section E - May 19, 2023 Category: Chemistry Authors: Geetha, D. Mohan Kumar, T.M. Anil Kumar, H.G. Shreenivas, M.T. Basavaraju, Y.B. Yathirajan, H.S. Parkin, S. Tags: 1,3,4-thiadiazole heterocycle high Z ′ = 6 hydrogen bonding disorder crystal structure research communications Source Type: research
Syntheses, crystal structures and Hirshfeld surface analysis of 2-(benzylsulfanyl)-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole and 2-[(2-chloro-6-fluorobenzyl)sulfanyl]-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole
The title compounds were synthesized by alkylation of 5-[(4-dimethylamino)phenyl]-1,3,4-oxadiazole-2-thiol with benzyl chloride or 2-chloro-6-fluorobenzyl chloride in the presence of potassium carbonate. The yields of 2-(benzylsulfanyl)-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole, C17H17N3OS (I), and 2-[(2-chloro-6-fluorobenzyl)sulfanyl]-5-[4-(dimethylamino)phenyl]-1,3,4-oxadiazole, C17H15ClFN3OS (II), were 96 and 92%, respectively. In the crystal structures of (I) and (II), C – H... π interactions are observed between neighboring molecules. Hirshfeld surface analysis indicates that H...H and H...C/C...H interactions m...
Source: Acta Crystallographica Section E - May 19, 2023 Category: Chemistry Authors: Okmanov, R.Y. Ziyaev, A.A. Abdukarimov, A.S. Toshmurodov, T.T. Kholikov, T.S. Tags: synthesis 1,3,4-oxadiazole crystal structure Hirshfeld surface analysis research communications Source Type: research
Synthesis and structure of photodegradable 1-(4,5-dimethoxy-2,3-dinitrophenyl)-2-methylpropyl N-butylcarbamate
The reaction of 1-(4,5-dimethoxy-2,3-dinitrophenyl)-2-methylpropan-1-ol and butylisocyanate using dibutyltin dilaurate as a catalyst afforded 1-(4,5-dimethoxy-2,3-dinitrophenyl)-2-methylpropyl N-butylcarbamate, C17H25N3O8, which released butylamine upon photoirradiation. Single crystals of the title compound were grown in a 1:1 mixed solution of hexane and ethyl acetate. Two nitro groups and one methoxy group are twisted out of the plane of the aromatic ring in the novel photo-protecting group. Intermolecular hydrogen bonds are observed between N-butylcarbamate moieties parallel to the a axis. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - May 16, 2023 Category: Chemistry Authors: Honda, T. Ito, M. Yamaguchi, K. Kasuga, N.C. Sato, H. Tags: photolabile carbamate 2,3-dinitrobenzyl group intermolecular hydrogen bonding crystal structure research communications Source Type: research
