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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

February 2019 issue

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Cover illustration: Resorcinarene-based cavitands are macrocyclic synthetic compounds that are useful receptors for molecular recognition and versatile building blocks for crystal engineering. In particular, when the bridging groups connecting the phenolic hydroxyl moieties of the resorcinarene scaffold are quinoxaline rings, these cavitands become ideal hosts to interact with aromatic compounds, exploiting the [pi]-basicity and hydrophobicity of their cavity. The present paper reports the synthesis of a new, deep cavitand bearing four 1,4 dioxane rings on the quinoxaline walls, and analyses in detail the molecular and crystal structure of its supramolecular complex with benzene. See: R. Pinalli, J. W. Trzcinski, E. Dalcanale & C. Massera [Acta Cryst. (2019). E75, 103-108].

research communications


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A new, deep tetra­quinoxaline-based cavitand has been synthesized, and its solid-state complex with benzene has been studied through X-ray diffraction analysis.

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The title mol­ecule displays a trans configuration with respect to the C=N double bond. The dihedral angle between the bromo- and the methyl-substituted benzene rings is 16.1 (3)°. In the crystal, mol­ecules are connected by N—H⋯O and weak C—H⋯O hydrogen bonds, forming R_{2}^{1}(6) ring motifs and generating chains along the a–axis direction.

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This new 2,6-bis­(imino)­pyridine derivative with terminal 4-chloro­phenyl rings crystallizes with two independent mol­ecules in the asymmetric unit.

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Single crystal X-ray diffraction analysis and Hirshfeld surface analysis of the title compound were carried out to analyse qu­anti­tatively the inter­molecular inter­actions involved in the crystal packing. The electrostatic potential surface was generated over the Hirshfeld surface to visualize the potential active sites.

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The mol­ecular structure of the title compound consists of a 2,5-di­chloro­thio­phene ring and a 2-chloro­phenyl ring linked via a prop-2-en-1-one spacer. The mol­ecule has an E configuration about the C=C bond and the carbonyl group is syn with respect to the C=C bond. In the crystal, the mol­ecules are linked along the a-axis direction through van der Waals forces and by face-to-face π-stacking between the thio­phene rings and between the benzene rings of neighbouring mol­ecules along the b axis into zigzag sheets lying parallel to the bc plane.

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Mol­ecules of the title compound are linked into a complex three-dimensional network by a combination of C—H⋯O and C—H⋯π(arene) hydrogen bonds.

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Crystal and mol­ecular structure of bis­(glycinium)lithium perchlorate salt is reported and inter­molecular N— H⋯O and C—H⋯O hydrogen bonds stabilize the salt in the crystalline state.

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The structure of tetra­lithium octa­fluorido­zirconate has been redetermined by high-resolution single-crystal X-ray diffraction. This result is largely consistent with a prior report, but with significant improvements in precision.

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Polynitrile anions are known for their ability to combine with transition metals and co-ligands to form ternary systems. Here we report on the crystal structure of tris­(2–2′-bi­pyridine)­cobalt(II) bis­(1,1,3,3-tetra­cyano-2-eth­oxy­propenide).

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In the title compound, the 3-bromo­phenyl and 4-fluoro­phenyl rings, linked via a prop-2-en-1-one spacer, make a dihedral angle of 48.90 (15)°. In the crystal, mol­ecules are linked by C—H⋯π inter­actions between the bromo­phenyl and fluoro­phenyl rings of mol­ecules, resulting in a two-dimensional layered structure parallel to the ab plane.

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The CuII ion in the title compound shows a distorted square-pyramidal coordination geometry. In the crystal, the mol­ecules are connected by N—H⋯O, O—H⋯O, C—H⋯O and π–π inter­actions, forming a three-dimensional supra­molecular network.

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The asymmetric unit of the title compound contains two independent organic mol­ecules which differ primarily in the dihedral angle between the aromatic rings, viz. 7.79 (7) and 29.89 (7)°. In the crystal, the components are linked by Owater—H⋯N, N—H⋯Owater and N—H⋯N hydrogen bonds, forming chains along the [100] direction. The chains are linked by C—H⋯O and C—H⋯N hydrogen bonds, forming layers parallel to the ab plane. Finally, the layers are linked by C—H⋯π inter­actions, forming a three-dimensional structure.

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In the crystal, the system of O—H⋯O hydrogen bonds, including bridging water mol­ecules residing on crystallographic twofold axes, results in a two-dimensional layered structure. Within the layers, there are also weak N—H⋯π inter­actions involving the vanilline benzene ring.

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The title compound crystallizes with two independent mol­ecules in the asymmetric unit. The semicarbazone moieties of which are essentially planar with the terminal phenyl rings twisted away from them. In the crystal, N—H⋯O hydrogen-bonding inter­actions link the two mol­ecules into a centrosymmetric dimer, with adjacent dimers linked by weak C—H⋯O inter­actions to form a cage-like structure. These cage structures are inter­connected by weak C—H⋯π inter­actions, forming supra­molecular chains along the c-axis direction.

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The syntheses and structures of five mol­ecular salts of protonated 4,4,7,7-tetra­methyl-3a,5,6,7a-tetra­hydro­benzo­thia­zol-2-yl­amine (C11H19N2S+) with different deprotonated carb­oxy­lic acids (4-methyl­benzoic acid, 4-bromo­benzoic acid, 3,5-di­nitro­benzoic acid, fumaric acid and succinic acid) are reported·In every case, the cation protonation occurs at the N atom of the thia­zole ring and the six-membered ring adopts a half-chair conformation (in some cases, the deviating methyl­ene groups are disordered over two sets of sites). The C—N bond lengths of the nominal –NH+=C—NH2 fragment of the cation are indistinguishable, indicating a significant contribution of the –NH—C=N+H2 resonance form to the structure.

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Scandium nitrate tetra­hydrate reacts with H2salophen [N,N′-bis­(salicyl­idene)-1,2-phenyl­enedi­amine] in ethanol to give the unsymmetrical dinuclear complex Sc(NO3)2(μ-salophen)Sc(salophen)(EtOH).

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In this communication, two compounds and their respective crystal structures, obtained via fragmentation of the triazene moiety in a PCN pincer iridium complex, are discussed. One showcases a novel (dppm)C(N2dppm) PCP pincer, the other contains a (dppm)C(N2) diazo­methyl­ene­phospho­rane moiety.

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The AgI ion is coordinated by two heterocyclic N atoms from two ligands in a linear configuration, forming a discrete coordination complex. There is an O—H⋯O hydrogen bond between 2-tza and 2tzaH of adjacent complexes. The hydrogen atom is shared between the two oxygen atoms.

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The title compound crystallizes with two independent mol­ecules in the asymmetric unit. They differ essentially in the orientation of the 4-meth­oxy­phenyl ring with respect to the pyridine ring of the quinoline moiety.

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The crystal packing of benzyl­ammonium phenyl­acetate (1) and its hydrate (2) is governed by hydrogen bonds formed between the ammonium and acetate groups and the water mol­ecule of crystallization (in 2 only). The benzyl moieties for hydro­phobic layers with the aromatic rings adopting edge-to-face arrangements.

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Three 1-[(1,3-benzodioxol-5-yl)methyl]-4-(halobenzo­yl)piperazines adopt very similar mol­ecular conformations but, while the mol­ecules of the 3-fluoro­benzoyl are linked by hydrogen bonds into a three-dimensional structure, there are no hydrogen bonds in either of the 2,6-di­fluoro­benzoyl and 2,4-di­chloro­benzoyl analogues.

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Two asymmetrically substituted cobaltocenium carb­oxy­lic acid compounds were synthesized and their crystal structures determined. Both crystallize as hydrates and exhibit an extended hydrogen-bonding network.

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The crystal structure of Ca3CoAl4O10 was redetermined from single-crystal X-ray data and is isotypic with Ca3MgAl4O10.

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The conformations of the title compounds, (I) and (II), are very similar. The pyran rings adopt envelope conformations, the piperidine rings have chair conformations and the pyrrolidine rings adopt twist conformations. Intra- and inter­molecular C—H⋯O hydrogen bonds occur. Compound (II) crystallizes with two independent mol­ecules in the asymmetric unit which are linked by C—H⋯O hydrogen bonds.

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The crystal structures of sodium rubidium hydrogen citrate and sodium caesium hydrogen citrate have been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. In NaRbHC6H5O7, the Na and Rb cation coordination spheres form triple chains along the a-axis direction, and chains of very strong O—H—O hydrogen bonds run along [111], while in NaCsHC6H5O7 the Na and Cs coordination polyhedra form layers parallel to (101), and there are chains of very short and strong hydrogen bonds along [100].

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The title compound is built up from the benzodiazepine ring system linked to the pyridyl and pendant di­hydro­pyran rings. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds link the mol­ecules into a three-dimensional network. A weak C—H ⋯ π inter­action is also observed.

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The copper(II) atom shows a typical Jahn–Teller distorted [4 + 2] octa­hedral coordination sphere.

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The dihedral angle between the 4-fluoro­phenyl ring and the nitro-substituted benzene ring of the title compound is 63.29 (8)°. In the crystal, mol­ecules are linked by C—H⋯O hydrogen bonds into chains parallel to the c axis. The crystal packing is further stabilized by C—Cl⋯π, C—F⋯π and N—O⋯π inter­actions

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We report the crystal structure of benzyl 2-naphthyl ether, which is used as a sensitiser for thermal paper. In the crystal, one mol­ecule inter­acts with six neighbouring mol­ecules via C—H⋯π inter­molecular inter­actions to form a herringbone mol­ecular arrangement.

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The title compounds, (I) and (II), differ by the presence of a methyl group in position 5 on the 1H-indole-2-one ring of compound (II). There is also a significant difference in the conformation of the five-membered thia­zolidine ring in the two compounds.

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The two independent mol­ecules in the asymmetric unit of the title compound are connected via two N—H⋯N hydrogen bonds, forming dimers which inter­act by two bifurcated π–π stacking inter­actions to build tetra­meric motifs. These are packed via C—H ⋯N and C—H⋯π inter­actions, resulting in a three-dimensional architecture with a tilted herringbone packing mode.

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The title compound crystallized with two independent mol­ecules (A and B) in the asymmetric unit. They differ essentially in the conformation of the pyrrolidine and cyclo­pentene rings; respectively, twisted and flat in mol­ecule A, but envelope and twisted in mol­ecule B.

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The solid solution series Ca4+xY3–xSi7O15+xN5–x with x = 0, 0.5 and 1, crystallizes isotypically with a [Si7(O,N)19] unit as a characteristic building unit.

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In the title chalcone derivative, C15H9Cl2BrO, the two aryl rings are inclined to each other by 14.49 (17)°, and the olefinic double bond adopts an E configuration. In the crystal, the only short inter­molecular contacts are Cl⋯O contacts [3.173 (3) Å] that link the mol­ecules to form a 21 helix propagating along the b-axis direction.

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In the crystal structure of (2-acetyl­ferrocen-1-yl)boronic acid, centrosymmetric dimers held together by –B(OH)⋯O hydrogen bonds are present.

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The solid-state structure of 2-(4-hy­droxy­phen­yl)-1-[(4-hy­droxy­phen­yl)meth­yl]-5,6-dimethyl-1H-benzimidazole acetone disolvate exhibits O—H⋯N hydrogen bonds between benzimidazole units and O—H⋯O hydrogen bonds with one of the acetone solvate mol­ecules as the acceptor. Density functional theory is used to estimate the strength of the inter­actions.

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The mol­ecular recognition properties of the tetra­phospho­nate cavitand Tiiii[C3H7,CH3,C6H5] towards mephedrone hydro­chloride, an illicit drug belonging to the amphetamine family, have been analysed in the solid state through the detailed analysis of the crystal and mol­ecular structure of the resulting supra­molecular compound, and in solution via NMR studies.

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The title compound crystallized from an equimolar mixture of 2-amino-6-bromo­pyridine and 2,3,5,6-tetra­fluoro­benzoic acid in absolute ethanol.

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In both title pyridine derivatives, (I) and (II), the cation adopts an E configuration with respect to the C=C. In compound (I), the PF6 anion is disordered with occupancy factors of 0.614 (7):0.386 (7). In both the compounds, the crystal packing is stabilized by C—H⋯F inter­molecular inter­actions results into two-dimensional mol­ecular sheets, which are formed by R_{3}^{4}(14) ring motifs in compound (I), R_{6}^{6}(40) ring motifs in compound (II). In addition to that, the crystal packing is further stabilized by P—F⋯π inter­actions in compound (I) and π–π in compound (II).

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Co-crystallization of 3,5-di­nitro­benzoic acid with trihexyphenidyl [or 1-cyclo­hexyl-1-phenyl-3-(piperidin-1-yl)propan-1-ol], gives a 1:1 salt (I) but chlorprothixene [or (Z)-3-(2-chloro-9H-thioxanthen-9-yl)-N,N-di­methyl­propan-1-amine], gives a 1:2 acid salt (II) containing a very short O—H⋯O hydrogen bond. Multiple hydrogen bonds link the ions in (I) into a complex chain of rings and those in (II) link the ions into a sheet.

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In the crystal structure of the title compound, the NiII cations are octa­hedrally coordinated by two terminally N-bonded thio­cyanate anions, two methanol mol­ecules and two 4-benzoyl­pyridine coligands into discrete complexes that are linked by inter­molecular C—H⋯S, C—H⋯O and O—H⋯O hydrogen-bonding inter­actions into a three-dimensional network with channels in which the non-coordinating methanol solvate mol­ecules are located.

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The reduction of CoBr2 by the Grignard reagent p-tolyl­magnesium bromide in the presence of 1,2-bis­(di­phenyl­phosphan­yl)benzene (dbpz) resulted in the d10, formally Co−1 anion, [Co(dpbz)2]. The crystal structure of the [MgBr(THF)5]+ (THF is tetra­hydro­furan) salt showed the anion to be pseudo­tetra­hedral and packed in alternating layers of anions and cations.

Research communications

Research communications are designed to help authors bring out the science behind their structure determinations. Authors are encouraged to report more than one structure in the same communication and also to include the results of investigations with other techniques. The Research communications format makes Acta E the natural home for structure determinations with interesting science to report.

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