Crystal structures of (12E)-12-(4-benzylidene)-7,7,16-trimethyl-3-(4-methylphenyl)-1-oxa-16-azatetracyclo[11.2.1.02,11.04,9]hexadeca-2(11),4(9)-dien-5-one and (12E)-12-(4-bromobenzylidene)-73-(4-bromophenyl)-,7,16-trimethyl-10-oxa-16-azatetracyclo[11.2.1.02,11.04,9]hexadeca-2(11),4(9)-dien-5-one
The title compounds, C32H35NO2, (I), and C30H29Br2NO2, (II), differ by the presence of a bromine atom instead of a methyl atom in the para position of two benzene rings of compound (II). The two compounds have a structural overlap r.m.s. deviation of 0.27 Å . The pyran and seven-membered cycloheptene rings in both structures adopt boat and boat-sofa conformations, respectively. Intra- and intermolecular C — H...O hydrogen bonds are responsible for the consolidation of the crystal packing of both molecules. In addition to this, weak C — H... π interactions are also observed. The intermolecular interactions were qu...
Source: Acta Crystallographica Section E - March 28, 2023 Category: Chemistry Authors: Meenatchi, C.S. Vishnupriya, R. Suresh, J. Rubina, S.R. Selvanayagam, S. Bhandari, S.R. Tags: crystal structure azabicyclo derivatives superposition — H...O intramolecular interactions H...O intermolecular hydrogen bonds Hirshfeld surface analysis research communications Source Type: research
A mixed phosphine sulfide/selenide structure as an instructional example for how to evaluate the quality of a model
This paper compares variations on a structure model derived from an X-ray diffraction data set from a solid solution of chalcogenide derivatives of cis-1,2-bis(diphenylphosphanyl)ethylene, namely, 1,2-(ethene-1,2-diyl)bis(diphenylphoshpine sulfide/selenide), C26H22P2S1.13Se0.87. A sequence of processes are presented to ascertain the composition of the crystal, along with strategies for which aspects of the model to inspect to ensure a chemically and crystallographically realistic structure. Criteria include mis-matches between Fobs2 and Fcalc2, plots of |Fobs| vs |Fcalc|, residual electron density, checkCIF alerts, pitfall...
Source: Acta Crystallographica Section E - March 28, 2023 Category: Chemistry Authors: Parkin, S. Cunningham, J. Rawls, B. Bender, J.E. Staples, R.J. Biros, S.M. Tags: checkCIF alerts F2obs vs F2calc OMIT command outliers displacement ellipsoids solid solution disordered electron density standard interatomic distances crystal structure research communications Source Type: research
Enantiopure (S)-butan-2-yl N-(4-x-phenyl)thiocarbamates, x = NO2, OCH3, F, and Cl
The structures of (S)-butan-2-yl N-(4-nitrophenyl)thiocarbamate, C11H14N2O3S, (I), (S)-butan-2-yl N-(4-methoxyphenyl)thiocarbamate, C12H17NO2S, (II), (S)-butan-2-yl N-(4-fluorophenyl)thiocarbamate, C11H14FNOS, (III), and (S)-butan-2-yl N-(4-chlorophenyl)thiocarbamate, C11H14ClNOS, (IV), all at 100 K, have monoclinic (P21) symmetry with two independent molecules in the asymmetric unit. The Flack absolute structure parameters in all cases confirm the absence of inversion symmetry. The structures display N — H...S hydrogen bonds, resulting in R22(8) hydrogen-bonded ring synthons connecting the two independent molecules....
Source: Acta Crystallographica Section E - March 23, 2023 Category: Chemistry Authors: Kaminsky, W. Kaganyuk, M. Tags: enantiopure (S)-2butyl thiocarbamate isothiocyanate crystal structure research communications Source Type: research
Syntheses and crystal structures of four 4-(4-methoxyphenyl)piperazin-1-ium salts: trifluoroacetate, 2,3,4,5,6-pentafluorobenzoate, 4-iodobenzoate, and a polymorph with 4-methylbenzoate
Syntheses and X-ray crystal structures of four 4-(4-methoxyphenyl)piperazin-1-ium (MeOPP) salts, with 2,2,2-trifluoroacetate, C11H17N2O+ · C2F3O2 − (I), 2,3,4,5,6-pentafluorobenzoate, C11H17N2O+ · C7F5O2 · H2O (II), 4-iodobenzoate C11H17N2O+ · C7H4IO2 − · H2O (III), and 4-methylbenzoate, C11H17N2O+ · C8H7O2 − · H2O (IV) anions are presented. The salts form directly from equimolar quantities of N-(4-methoxyphenyl)piperazine and the corresponding organic acid in methanol and crystallize from 1:1 methanol/ethyl acetate. Salt I is anhydrous whereas II, III, and IV are all monohydrates. In all cases, the MeOPP cati...
Source: Acta Crystallographica Section E - March 23, 2023 Category: Chemistry Authors: Vinaya Basavaraju, Y.B. Yathirajan, H.S. Parkin, S. Tags: crystal structure piperazine piperazinium salt hydrogen bonding iodine – iodine close contacts polymorph research communications Source Type: research
Syntheses, crystal structures and Hirshfeld surface analysis of three salts of 1-(4-nitrophenyl)piperazine
The structures and Hirshfeld surface analysis of three salts of 1-(4-nitrophenyl)piperazine are discussed. In 4-(4-nitrophenyl)piperazin-1-ium salicylate (C10H14N3O2+ · C7H5O3 − ), there are strong hydrogen bonds between cation and anion and the 4-nitrophenyl substituent occupies an equatorial position in the piperazinium ring. The cation and anion are linked together by supramolecular interactions [graph-set notation of hydrogen bonding C_{2}^{2}(6) propagating in the a-axis direction]. Additionally, there is π – π stacking involving the salicylate anion and the piperazinium cation in adjacent asymmetric units as w...
Source: Acta Crystallographica Section E - March 21, 2023 Category: Chemistry Authors: Archana, S.D. Foro, S. Yathirajan, H.S. Kiran Kumar, H. Balerao, R. Butcher, R.J. Tags: crystal structure piperazinium salt Hirshfeld surface analysis salicylate graph-set notation axial and equatorial substitution patterns in piperazinium rings research communications Source Type: research
Crystal structure and Hirshfeld surface analysis of N-{N-[amino(dimethylamino)methyl]carbamimidoyl}-3-bromobenzenesulfonamide
The title compound, C10H14BrN5O2S, is the bromobenzenesulfonamide derivative of the type 2 diabetes drug metformin. The asymmetric unit contains two molecules with almost identical conformations but a different orientation of the bromophenyl moiety. Both molecules exhibit intramolecular N — H...N and N — H...O hydrogen bonds. The molecular packing features chain formation in the a-axis direction by alternating N — H...N and N — H...O interactions. In addition, ring motifs consisting of four molecules and π – π interactions between the phenyl rings contribute to the three-dimensional architecture. A Hirshfeld su...
Source: Acta Crystallographica Section E - March 21, 2023 Category: Chemistry Authors: Su, K. Luo, J. Van Meervelt, L. Tags: crystal structure metformin hydrogen-bond interactions π – Hirshfeld surface analysis research communications Source Type: research
Crystal structure and Hirshfeld surface analysis of mono/bis(aqua- κ O)[N-(2-oxidobenzylidene)valinato- κ 3O,N,O ′ ]copper(II): dimeric Schiff base copper(II) complexes having different numbers of coordinated water molecules
The molecular structure of the title compound, [Cu(C12H13N2O3)(H2O)2] · [Cu(C12H13N2O3)(H2O)], consists of two different molecules in the asymmetric unit. Both of the structures consist of a tridentate ligand synthesized from l-valine and salicylaldehyde, and one water molecule or two water molecules coordinating to CuII. They have a square-planar (molecule 1) or a square-pyramidal (molecule 2) coordination geometry. In the crystal, the molecules form intra- and intermolecular O — H...O hydrogen bonds involving the coordinated water molecules and other sites. A Hirshfeld surface analysis indicated that the most importan...
Source: Acta Crystallographica Section E - March 21, 2023 Category: Chemistry Authors: Akiyama, Y. Suzuki, S. Suda, S. Takiguchi, Y. Nakane, D. Akitsu, T. Tags: Schiff base complex copper amino acid Hirshfeld analysis crystal structure research communications Source Type: research
2,2 ′ :4,4 ′ ′ :4 ′ ,4 ′ ′ ′ -Quaterpyridine: synthesis, crystal-structure description, and Hirshfeld surface analysis
The title compound, 2,2 ′ :4,4 ′ ′ :4 ′ ,4 ′ ′ ′ -quaterpyridine (Qtpy), C20H14N4, crystallizes in the triclinic P\overline{1} space group and has half of the molecule in the asymmetric unit, corresponding to 4,4 ′ -bipyridine (4,4 ′ -bpy) that serves as the building block for the molecule. C4,4 ′ -bpy — N — C4,4 ′ -bpy and/or N — C4,4 ′ -bpy — C4,4 ′ -bpy bond-angle parameters show that the 4,4 ′ -bpy ligands are highly rigid, displaying values lower than the linear bond angle of 180 ° . In the crystal, the 4,4 ′ -bpy units are seen to be facing each other in relatively close proximi...
Source: Acta Crystallographica Section E - March 21, 2023 Category: Chemistry Authors: Aderinto, S.O. Thomas, J.A. Robertson, C.C. Tags: crystal structure quaterpyridine Hirshfeld surface analysis research communications Source Type: research
3,3 ′ -(Phenylmethylene)bis(1-ethyl-3,4-dihydro-1H-2,1-benzothiazine-2,2,4-trione): single-crystal X-ray diffraction study, quantum-chemical calculations and Hirshfeld surface analysis
The title compound, C27H26N2O6S2, possesses potential antimicrobial, analgesic, and anti-inflammatory activity. This compound has three tautomeric forms, which relative energies were estimated with quantum-chemical calculations. All these tautomers (dienol form 7A, keto – enol form 7B, and diketo form 7C) were optimized by the M06 – 2X/cc-pVTZ method in a vacuum, using the PCM model with chloroform and DMSO as solvent. The diketo form of the title compound proved to be the most energetically favourable as compared to the keto – enol or dienol forms. The diketo form can exist as three possible stereoisomers with the s...
Source: Acta Crystallographica Section E - March 21, 2023 Category: Chemistry Authors: Shyshkina, M.O. Lega, D.A. Shemchuk, L.M. Starchikova, I.L. Shemchuk, L.A. Tags: 2,1-benzothiazine 2,2-dioxide keto-enol tautomerism molecular structure crystal structure Hirshfeld surface analysis quantum-chemical calculations research communications Source Type: research
Crystal structure of tert-butyl 3,6-diiodocarbazole-9-carboxylate
The molecular structure of tert-butyl 3,6-diiodocarbazole-9-carboxylate, C17H15I2NO2, features a nearly planar 13-membered carbazole ring with C — I bond lengths of 2.092 (4) and 2.104 (4) Å . The carbamate group has key bond lengths of 1.404 (6) Å (N — C), 1.330 (5) Å (O — C), and 1.201 (6) Å (C=O). The crystal contains intermolecular π – π interactions, as well as both type I and type II intermolecular I...I interactions. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - March 15, 2023 Category: Chemistry Authors: Sielaff, E.N. Staples, R.J. Biros, S.M. Tags: crystal structure carbazole halogen – halogen interaction π research communications Source Type: research
Crystal structure of [tBuMgCl]2[MgCl2(Et2O)2]2
The title compound, di- μ 3-chlorido-tetra- μ 2-chlorido-tetrakis(diethyl ether- κ O)bis(1,1-dimethylethyl)tetramagnesium, [Mg4(C4H9)2Cl6(C4H10O)4], features an Mg4Cl6 open-cube cluster. The two four-coordinate Mg2+ ions show an almost tetrahedral coordination, whereas the two six-coordinate Mg2+ ions have their ligands in an octahedral environment. The Mg — Cl bond lengths differ depending on the coordination number (2 or 3) of the bridging μ -Cl − ligands. There are few comparable structures deposited in the Cambridge Structural Database. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - March 15, 2023 Category: Chemistry Authors: Metzler, M. Bolte, M. Wagner, M. Lerner, H.-W. Tags: crystal structure Grignard reagent open-cube cluster research communications Source Type: research
Crystal structures of three homologues with increasing ring size: 2-methoxy-4-(thiophen-2-yl)-5,6,7,8-tetrahydroquinoline-3-carbonitrile, 2-methoxy-4-(thiophen-2-yl)-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carbonitrile and 2-methoxy-4-(thiophen-2-yl)-5,6,7,8,9,10-hexahydrocycloocta[b]pyridine-3-carbonitrile
The title compounds, C15H14N2OS (1a), C16H16N2OS (1b), and C17H18N2OS (1c), form a homologous series in which the size of the saturated ring increases from six- to eight-membered (with four, five and six methylene groups respectively). For 1b and 1c, the central (CH2)n moieties are all displaced to the same side of their ring, and the CH2 — CH2 — CH2 angles are much wider than the standard sp3 value; a database search indicates that these are general features of such ring systems. For 1a, the thiophene ring lies with the sulfur atom on the opposite side of the Cthiophene — Cpyridine bond to the cyano group, in contra...
Source: Acta Crystallographica Section E - March 15, 2023 Category: Chemistry Authors: Hebishy, A.M.S. Elgemeie, G.H. Gouda, L.M. Jones, P.G. Tags: crystal structure pyridine thiophene nitrile hydrogen bond research communications Source Type: research
Synthesis and crystal structure of N-(5-acetyl-4-methylpyrimidin-2-yl)benzenesulfonamide
N-(5-Acetyl-4-methylpyrimidin-2-yl)benzenesulfonamide, C13H13N3O3S, was sythesized and characterized by single-crystal X-ray diffraction. In the crystal, π – π interactions between the phenyl and pyrimidine groups of neighbouring molecules form molecular chains parallel to [010]. Adjacent molecular chains are linked by N — H...N hydrogen-bonding interactions between the pyrimidine and amine groups of neighbouring molecules, resulting in a three-dimensional network. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - March 15, 2023 Category: Chemistry Authors: Mohamed-Ezzat, R.A. Kariuki, B.M. Azzam, R.A. Tags: synthesis pyrimidine sulfonamide crystal structure X-ray diffraction research communications Source Type: research
Garnet-type Na3Te2(FeO4)3
Na3Te2(FeO4)3 or Na3Te2Fe3O12, trisodium ditellurium(VI) triiron(III) dodecaoxide, was obtained in the form of single-crystals under hydrothermal conditions. Na3Te2(FeO4)3 adopts the garnet structure type in space group Ia\overline{3}d and comprises one Na (multiplicity 24, Wyckoff letter c, site symmetry 2.22), one Te (16 a, .\overline{3}.), one Fe (24 d, \overline{4}..) and one O atom (96 h, 1) in the asymmetric unit. The three-dimensional framework structure is built of [TeO6] octahedra and [FeO4] tetrahedra by vertex-sharing. The larger Na+ cations are situated in the interstices of the framework and are eightfold coor...
Source: Acta Crystallographica Section E - March 15, 2023 Category: Chemistry Authors: Eder, F. Weil, M. Tags: crystal structure garnet oxidotellurate(VI) isotypism structural similarity research communications Source Type: research
Crystal structure of trimethyl({tris[(phenylsulfanyl)methyl]silyl}methoxy)silane and Hirshfeld surface analysis of 3-bromo-2,2-bis(bromomethyl)propan-1-ol
Trimethyl({tris[(phenylsulfanyl)methyl]silyl}methoxy)silane (3), C26H32OS3Si, is a new ligand for transition-metal coordination chemistry derived from 3-bromo-2,2-bis(bromomethyl)propan-1-ol (1), C5H9Br3O, through silylation and following exchange of bromine groups with NaSPh. Silylated thioether ligand 3 crystallizes in the centrosymmetric space group C2/c. Bromomethylalcohol 1 crystallizes in the space group P\overline{1} in the triclinic crystal system with four molecules in the asymmetric unit. Analysis of the Hirshfeld surface shows structure-defining interactions for bromomethylalcohol 1, resulting in intermolecular ...
Source: Acta Crystallographica Section E - March 15, 2023 Category: Chemistry Authors: Wappelhorst, J.F. Wattenberg, J. Strohmann, C. Tags: crystal structure thioether ligand Hirshfeld surface analysis research communications Source Type: research
