February 2019 issue
A new, deep tetraquinoxaline-based cavitand has been synthesized, and its solid-state complex with benzene has been studied through X-ray diffraction analysis.
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 (6) ring motifs and generating chains along the a–axis direction.
This new 2,6-bis(imino)pyridine derivative with terminal 4-chlorophenyl rings crystallizes with two independent molecules in the asymmetric unit.
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.
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.
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.
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.
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.
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).
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.
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.
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  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.
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.
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.
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.
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).
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.
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.
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.
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.
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.
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.
The crystal structure of Ca3CoAl4O10 was redetermined from single-crystal X-ray data and is isotypic with Ca3MgAl4O10.
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.
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 , 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 .
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.
The copper(II) atom shows a typical Jahn–Teller distorted [4 + 2] octahedral coordination sphere.
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
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.
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.
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.
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.
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.
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.
In the crystal structure of (2-acetylferrocen-1-yl)boronic acid, centrosymmetric dimers held together by –B(OH)⋯O hydrogen bonds are present.
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.
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.
The title compound crystallized from an equimolar mixture of 2-amino-6-bromopyridine and 2,3,5,6-tetrafluorobenzoic acid in absolute ethanol.
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 (14) ring motifs in compound (I), (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).
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.
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.
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.