A new, deep quinoxaline-based cavitand receptor for the complexation of benzene

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

Synthesis, X-ray crystal structure, Hirshfeld surface analysis and DFT studies of (E)-N′-(2-bromo­benzyl­idene)-4-methylbenzohydrazide

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.

Crystal structure of a new 2,6-bis­(imino)­pyridine derivative: (1E,1′E)-1,1′-(pyridine-2,6-di­yl)bis­[N-(4-chloro­phen­yl)ethan-1-imine]

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

Crystal structure, Hirshfeld surface analysis and electrostatic potential study of naturally occurring cassane-type diterpenoid Pulcherrimin C monohydrate at 100 K

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.

Crystal structure and Hirshfeld surface analysis of (E)-3-(2-chloro­phen­yl)-1-(2,5-di­chloro­thio­phen-3-yl)prop-2-en-1-one

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.

The crystal structure of 1-(2-iodo­benzo­yl)-4-(pyrimidin-2-yl)piperazine: a three-dimensional hydrogen-bonded framework, augmented by π–π stacking inter­actions and I⋯N halogen bonds

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 structure and Hirshfeld surface analysis of poly[[di-μ₃-glycine-lithium] perchlorate]

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.

Redetermination of the crystal structure of tetra­lithium octa­fluorido­zirconate(IV), Li₄ZrF₈, from single-crystal X-ray data

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.

Crystal structure of tris­(2,2′-bi­pyridine)­cobalt(II) bis­(1,1,3,3-tetra­cyano-2-eth­oxy­propenide)

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).

Crystal structure and Hirshfeld surface analysis of (2E)-1-(3-bromo­phen­yl)-3-(4-fluoro­phen­yl)prop-2-en-1-one

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.

Crystal structure of {2-methyl-2-[(pyridin-2-yl­meth­yl)amino]­propan-1-ol-κ³N,N′,O}bis­(nitrato-κO)copper(II) from synchrotron data

The Cu^II 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.

Crystal structure and Hirshfeld surface analysis of N-{2-[(E)-(4-methyl­benzyl­idene)amino]­phen­yl}-2-(5-methyl-1-H-pyrazol-3-yl)acetamide hemihydrate

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 O_water—H⋯N, N—H⋯O_water 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.

Crystal structure of 4-[(2-hy­droxy-3-meth­oxy­benz­yl)amino]­benzoic acid hemihydrate

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.

Crystal structure of 2-[(2E)-2-methyl-3-phenyl­prop-2-en-1-yl­idene]-N-phenyl­hydrazinecarboxamide

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.

Hydrogen-bonded mol­ecular salts of reduced benzo­thia­zole derivatives with carboxyl­ates: a robust (8) supra­molecular motif (even when disordered)

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.

An unsymmetrical dinuclear scandium complex comprising salophen ligands [H₂salophen = N,N′-bis­(salicyl­idene)-1,2-phenyl­enedi­amine]

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).

Crystal structures of [IrCl₂(NHCHPh)((dppm)(C(N₂dppm))-κ³P,C,P′)]Cl·5.5MeCN and [IrI(NHCHPh)(((dppm)C(N₂))-κ²P,C)(dppm-κ²P,P′)]I(I₃)·0.5I₂·MeOH·0.5CH₂Cl₂: triazene fragmentation in a PCN pincer iridium complex

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.

Crystal structure of (1,3-thia­zole-2-carboxyl­ato-κN)(1,3-thia­zole-2-carb­oxy­lic acid-κN)silver(I)

The Ag^I 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.

Crystal structure of 7′-(4-chloro­phen­yl)-2′′-(4-meth­oxy­phen­yl)-7′,7a',7′′,8′′-tetra­hydro-1′H,3′H,5′′H-di­spiro­[indoline-3,5′-pyrrolo­[1,2-c]thia­zole-6′,6′′-quinoline]-2,5′′-dione and an unknown solvent

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 structures of benzyl­ammonium phenyl­acetate and its hydrate

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 closely related 1-[(1,3-benzodioxol-5-yl)methyl]-4-(halobenzo­yl)piperazines: similar mol­ecular structures but different inter­molecular inter­actions

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.

Crystal structures of 1′-amino­cobaltocenium-1-carb­oxy­lic acid chloride monohydrate and of its azo dye 1′-[2-(1-amino-2,6-di­methylphenyl)diazen-1-yl]cobaltocenium-1-carb­oxy­lic acid hexa­fluorido­phosphate monohydrate

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.

Re-investigation and correct symmetry of Ca₃CoAl₄O₁₀

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

The crystal structures of 6′-(4-chloro­phen­yl)- and 6′-(4-meth­oxy­phen­yl)-6a′-nitro-6a′,6b′,7′,9′,10′,12a′-hexa­hydro-2H,6′H,8′H-spiro­[ace­naphthyl­ene-1,12′-chromeno[3,4-a]indolizin]-2-one

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.

Sodium rubidium hydrogen citrate, NaRbHC₆H₅O₇, and sodium caesium hydrogen citrate, NaCsHC₆H₅O₇: crystal structures and DFT comparisons

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].

Synthesis, crystal structure and Hirshfeld surface analysis of 3-(4,4-di­methyl-2,3,4,5-tetra­hydro-1H-1,5-benzodiazepin-2-yl­idene)-6-methyl-3,4-di­hydro-2H-pyran-2,4-dione

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.

Crystal structure of trans-bis­[2-(1H-benzotriazol-1-yl)acetato-κO]bis­(ethano­lamine-κ²N,O)copper(II)

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

Crystal structure and Hirshfeld surface analysis of (E)-1-[2,2-di­chloro-1-(4-nitro­phen­yl)ethen­yl]-2-(4-fluoro­phen­yl)diazene

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

Crystal structure of benzyl 2-naphthyl ether, a sensitiser for thermal paper

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.

Crystal structures of 6a,6b,7,11a-tetra­hydro-6H,9H-spiro­[chromeno[3′,4′:3,4]pyrrolo­[1,2-c]thia­zole-11,3′-indoline]-2′,6-dione and 5′-methyl-6a,6b,7,11a-tetra­hydro-6H,9H-spiro­[chromeno[3′,4′:3,4]pyrrolo­[1,2-c]thia­zole-11,3′-indoline]-2′,6-dione

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.

Synthesis, mol­ecular and crystal structure of 1-(1,2-di­hydro­phthalazin-1-yl­idene)-2-[1-(thio­phen-2-yl)ethyl­idene]hydrazine

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.

Crystal structure of 6-(4-chloro­phen­yl)-6a-nitro-6a,6b,8,9,10,12a-hexa­hydro-6H,7H-spiro[chromeno[3,4-a]indolizine-12,11′-indeno­[1,2-b]quinoxaline]

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.

Crystal structures of Ca_4+xY_3–xSi₇O_15+xN_5–x (0 ≤ x ≤ 1) comprising of an isolated [Si₇(O,N)₁₉] unit

The solid solution series Ca_4+xY_3–xSi₇O_15+xN_5–x with x = 0, 0.5 and 1, crystallizes isotypically with a [Si₇(O,N)₁₉] unit as a characteristic building unit.

Crystal structure and Hirshfeld surface analysis of a bromo­chalcone: (E)-1-(3-bromo­phen­yl)-3-(2,6-di­chloro­phen­yl)prop-2-en-1-one

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.

Crystal structure of (2-acetyl­ferrocen-1-yl)boronic acid

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

Inter­molecular inter­actions in a phenol-substituted benzimidazole

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.

Crystal structure of a host–guest complex between mephedrone hydro­chloride and a tetra­phospho­nate cavitand

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.

Crystal structure of the co-crystal salt 2-amino-6-bromo­pyridinium 2,3,5,6-tetra­fluoro­benzoate

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

Crystal structure determination of two pyridine derivatives: 4-[(E)-2-(4-meth­oxy­phen­yl)ethen­yl]-1-methyl­pyridin-1-ium hexa­fluoro-λ⁶-phosphane and 4-[(E)-2-[4-(di­methyl­amino)­phen­yl]ethen­yl]-1-phenyl-1λ⁵-pyridin-1-ylium hexa­fluoro-λ⁶-phosphane

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 two anti­psychotic agents: a simple 1:1 salt with trihexyphenidyl and a 1:2 acid salt containing a very short O—H⋯O hydrogen bond with chlorprothixene

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.

Crystal structure of bis­(4-benzoyl­pyridine-κN)bis­(methanol-κO)bis­(thio­cyanato-κN)nickel(II) methanol monosolvate

In the crystal structure of the title compound, the Ni^II 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.

Crystal structure of bromido­penta­kis­(tetra­hydro­furan-κO)magnesium bis­[1,2-bis­(di­phenyl­phosphan­yl)benzene-κ²P,P′]cobaltate(−1) tetra­hydro­furan disolvate

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.