Synthesis and structure of 2,4,6-tri­cyclo­butyl-1,3,5-trioxane

The synthesis and structure of the substituted trioxane compound 2,4,6,-tri­cyclo­butyl-1,3,5-trioxane is described. The three cyclo­butane rings attached to the 1,3,5-trioxane six-membered ring are all in a cis arrangement. The compound may find application as a stable trimeric form of the fragile cyclo­butane carbaldehyde.

Crystal structure and DFT study of a zinc xanthate complex

In the title compound, the Zn^II ion is coordinated by two N atoms of the N,N,N′,N′-tetra­methyl­ethylenedi­amine ligand and two S atoms from two 2-meth­oxy­ethyl xanthate ligands. Two C—H⋯O and two C—H⋯S intra­molecular inter­actions occur. In the crystal, mol­ecules are linked by C—H⋯O and C—H⋯S hydrogen bonds, forming a three-dimensional supra­molecular architecture.

The crystal structures of two novel polymorphs of bis­(oxonium) ethane-1,2-di­sulfonate

Two novel crystal forms of bis­(oxonium) ethane-1,2-di­sulfonate, 2H₃O⁻·C₂H₄O₆S₂²⁻, are reported. Polymorph II has monoclinic (P2₁/n) symmetry, while the symmetry of form III is triclinic (P). Both structures display extensive networks of O—H⋯O hydrogen bonds.

Synthesis, crystal structure and Hirshfeld surface analysis of 4-[3-(4-hy­droxy­phen­yl)-4,5-di­hydro-1H-pyrazol-5-yl]-2-meth­oxy­phenol monohydrate

In the title pyrazoline derivative, the pyrazoline ring makes angles of 86.73 (12) and 13.44 (12)° with the tris­ubstituted and disubstituted benzene rings, respectively. In the crystal structure, the mol­ecules are connected into chains running in the b-axis direction by O—H⋯N hydrogen bonding. Parallel chains inter­act through N—H⋯O hydrogen bonds and π–π stacking of the tris­ubstituted phenyl rings.

Crystal structures, syntheses, and spectroscopic and electrochemical measurements of two push–pull chromophores: 2-[4-(di­methyl­amino)­benzyl­idene]-1H-indene-1,3(2H)-dione and (E)-2-{3-[4-(di­meth­ylamino)­phen­yl]allyl­idene}-1H-indene-1,3(2H)-dione

The title pull–push chromophores, 2-[4-(di­methyl­amino)­benzyl­idene]-1H-indene-1,3(2H)-dione (ID[1]) and (E)-2-{3-[4-(di­methyl­amino)­phen­yl]allyl­idene}-1H-indene-1,3(2H)-dione (ID[2]), with donor–π-bridge–acceptor structures, are almost planar for the mol­ecule with a short π-bridge (ID[1]) but less planar for the mol­ecule with a longer bridge (ID[2]).

Crystal structure, Hirshfeld surface analysis and physicochemical characterization of bis­[4-(di­methyl­amino)­pyridinium] di-μ-chlorido-bis­[di­chlorido­mercurate(II)]

The two independent organic cations in the asymmetric unit of the chloro­mercurate(II) salt exhibit essentially the same features with almost planar pyridinium and di­methyl­amino groups. In the crystal, N—H⋯Cl and C—H⋯Cl hydrogen bonds as well as π–π and Cl⋯Cl inter­actions link the organic cations and inorganic anions into a three-dimensional network.

One-dimensional ladder gallium coordination polymer

The one-dimensional [Ga(HPDC)(OH)(H₂O)]_n ladder-type coordination polymer can be prepared using three distinct synthetic approaches (hydro­thermal, microwave-assisted and a one-pot process) with crystallite size varying according to the method employed.

Crystal structure of benzyl N′-[(1E,4E)-1,5-bis­(4-meth­oxy­phen­yl)penta-1,4-dien-3-yl­idene]hydrazine-1-carbodi­thio­ate

The title compound comprises four crystallographically different mol­ecules that are composed of a 1,5-bis­(4-meth­oxy­phen­yl)penta-1,4-dien-3-ylidenyl group and a benzyl ring connected by a hydrazine-1-carbodi­thio­ate bridge. In the crystal, mol­ecules are connected into a three-dimensional network through C—H⋯O, N—H⋯S and C—H⋯π inter­actions.

Crystal structure, DFT calculation, Hirshfeld surface analysis and energy framework study of 6-bromo-2-(4-bromo­phen­yl)imidazo[1,2-a]pyridine

The mol­ecular system displays a planar conformation between the phenyl and imidazo[1,2-a] pyridine rings. Weak C—H⋯π and π–π inter­actions as well as short contacts consolidate the three-dimensional network structure.

Crystal structure and Hirshfeld surface analysis of 2-amino­pyridinium hydrogen phthalate

New proton-transfer single crystals of 2-amino­pyridinium phthalate were obtained with the aim of synthesizing a new non-linear optical (NLO) material, which is achieved with the help of extensive hydrogen-bonding inter­actions between the ions.

Tetra-n-butyl­ammonium orotate monohydrate: knowledge-based comparison of the results of accurate and lower-resolution analyses and a non-routine disorder refinement

The analysis of a hydro­phobic–hydro­philic ion-pair structure at two temperatures permits the comparative evaluation of the accurate geometric results obtained at low temperature and less accurate results at room temperature using a knowledge-based approach.

Crystal structure, DFT and Hirshfeld surface analysis of 2-amino-4-(2-chloro­phen­yl)-7-hy­droxy-4H-benzo[1,2-b]pyran-3-carbo­nitrile

The crystal and mol­ecular structures of the pyran derivative 2-amino-4-(2-chloro­phen­yl)-7-hy­droxy-4H-benzo[1,2-b]pyran-3-carbo­nitrile is reported. Hirshfeld surface analysis was performed on the mol­ecule and frontier orbitals were investigated with density functional theory calculations.

High-pressure synthesis and crystal structure of SrGa₄As₄

SrGa₄As₄ was synthesized under high-pressure/high-temperature conditions. The crystal structure com­prises a network of Ga^IIIAs₄ tetra­hedra and ethane-like Ga^II₂As₆ groups with Ga—Ga bonds.

Crystal structure and luminescence properties of 2-[(2′,6′-dimeth­oxy-2,3′-bipyridin-6-yl)­oxy]-9-(pyridin-2-yl)-9H-carbazole

In the title com­pound, the dihedral angle between the planes of the bi­pyridine and carbazole moieties connected by an O atom is 68.45 (3)°. The bi­pyridine ring system, with two meth­oxy substituents, is approximately planar. The pyridine ring in the pyridyl-substituted carbazole fragment is tilted by 56.65 (4)° with respect to the mean plane of the carbazole moiety. The title com­pound exhibits a high energy gap and triplet energy.

Crystal structure, Hirshfeld surface analysis and inter­action energy and DFT studies of (2Z)-4-benzyl-2-(2,4-di­chloro­benzyl­idene)-2H-1,4-benzo­thia­zin-3(4H)-one

The title compound contains 1,4-benzo­thia­zine and 2,4-di­chloro­benzyl­idene units, where the di­hydro­thia­zine ring adopts a screw-boat conformation. In the crystal, inter­molecular C—H_Bnz⋯O_Thz (Bnz = benzene and Thz = thia­zine) hydrogen bonds form corrugated chains extending along the b-axis direction which are tied into layers parallel to the bc plane by inter­molecular C—H_Methy⋯S_Thz (Methy = methyl­ene) hydrogen bonds, enclosing (22) ring motifs.

Unexpected reactions of NHC*—Cu^I and —Ag^I bromides with potassium thio- or seleno­cyanate

This article reports the unexpected reactions of Cu and Ag NHC bromides with potassium thio- or seleno­cyanates. It contains the first report of the boomerang-shaped [Ag(SCN)₃]²⁻ ion.

Bis[2-(4,5-di­phenyl-1H-imidazol-2-yl)-4-nitrophenolato]copper(II) dihydrate: crystal structure and Hirshfeld surface analysis

A coordination geometry inter­mediate between square-planar and tetra­hedral, defined by an N₂O₂ donor set, is found in the title Cu^II complex. Conventional O—H⋯O and N—H⋯O hydrogen bonding leads to a supra­molecular layer in the crystal.

Crystal structure, Hirshfeld surface analysis and inter­action energy and DFT studies of methyl 4-[3,6-bis­(pyridin-2-yl)pyridazin-4-yl]benzoate

The pyridazine ring deviates slightly from planarity. In the crystal, ribbons consisting of inversion-related chains of mol­ecules extending along the a-axis direction are formed by C—H_Mthy⋯O_Carbx (Mthy = methyl and Carbx = carboxyl­ate) hydrogen bonds. The ribbons are connected into layers parallel to the bc plane by inversion-related C—H_Bnz⋯π(ring) inter­actions.

Crystal structures and Hirshfeld surface analyses of 4-benzyl-6-phenyl-4,5-di­hydro­pyridazin-3(2H)-one and methyl 2-[5-(2,6-di­chloro­benz­yl)-6-oxo-3-phenyl-1,4,5,6-tetra­hydropyridazin-1-yl]acetate

In each asymmetric unit of the title compounds, one independent mol­ecule is present. In the crystal structure of 4-benzyl-6-phenyl-4,5-di­hydro­pyridazin-3(2H)-one, adjacent mol­ecules are linked by a pair of N—H⋯O hydrogen bonds, forming inversion dimers with an (8) ring motif. The crystal structure of methyl 2-[5-(2,6-di­chloro­benz­yl)-6-oxo-3-phenyl-1,6-di­hydro-pyridazin-1-yl]acetate displays inter­molecular C—H⋯O inter­actions.

Crystal structure, synthesis and thermal properties of bis­(aceto­nitrile-κN)bis­(4-benzoyl­pyridine-κN)bis­(iso­thio­cyanato-κN)nickel(II)

In the crystal structure of the title com­pound, the Ni^II cations are octa­hedrally coordinated into discrete solvate com­plexes, that upon heating loses the aceto­nitrile ligands and transforms into an unknown modification of [Ni(NCS)₂(4-benzoyl­pyridine)₂].

Crystal structures of two solvated 2-aryl-3-phenyl-2,3-di­hydro-4H-pyrido[3,2-e][1,3]thia­zin-4-ones

The synthesis and crystal structures of two solvated 2-aryl-3-phenyl-2,3-di­hydro-4H-pyrido[3,2-e][1,3]thia­zin-4-ones are reported. Both are racemic mixtures (centrosymmetric crystal structures) of the individual com­pounds and incorporate solvent mol­ecules in their structures.

Crystal structures of the two isomeric hydrogen-bonded cocrystals 2-chloro-4-nitro­benzoic acid–5-nitro­quinoline (1/1) and 5-chloro-2-nitro­benzoic acid–5-nitro­quinoline (1/1)

The structures of the two isomeric hydrogen-bonded 1:1 cocrystals of 5-nitro­quinoline with 2-chloro-4-nitro­benzoic acid and 5-chloro-2-nitro­benzoic acid have been determined at 190 K. In each crystal, the acid and base mol­ecules are linked by a short O—H⋯N hydrogen bond.

The first structural characterization of the proton­ated aza­cyclam ligand in catena-poly[[[(perchlorato)copper(II)]-μ-3-(3-carb­oxy­prop­yl)-1,5,8,12-tetra­aza-3-azonia­cyclo­tetra­deca­ne] bis­(per­chlorate)]

The title com­pound is one-dimensional coordination polymer built up of tetra­gonally distorted CuN₄O₂ octa­hedra formed by four N atoms of the aza­macrocyclic ligand in the equatorial plane and O atoms of the protonated carb­oxy­lic acid group and the per­chlorate anion in the axial positions. In the crystal, [010] polymeric chains are crosslinked by N—H⋯O hydrogen bonds to form sheets lying parallel to the (001) plane.

Crystal structures and hydrogen-bonding analysis of a series of solvated ammonium salts of molybdenum(II) chloride clusters

The crystal structures of four different ammonium salts of the molybdenum halide cluster anion, [Mo₆Cl₈Cl₆]²⁻, are reported. They display varying degrees of hydrogen bonding between ammonium ions and the respective solvent mol­ecules.

Crystal structure of a 1:1 cocrystal of nicotinamide with 2-chloro-5-nitro­benzoic acid

In the 1:1 cocrystal of nicotinamide and 2-chloro-5-nitro­benzoic acid, the mol­ecules form hydrogen bonds through O—H⋯N, N—H⋯O, and C—H⋯O inter­actions along with N—H⋯O dimer hydrogen bonds of nicotinamide. Further additional weak π–π inter­actions stabilize the mol­ecular assembly of this cocrystal.

Crystal structure and Hirshfeld surface analysis of 2-(4-nitro­phen­yl)-2-oxo­ethyl benzoate

The title com­pound, 2-(4-nitro­phen­yl)-2-oxoethyl benzoate, is relatively planar with the two aromatic rings being inclined to each other by 3.09 (5)°.

Crystal structure and Hirshfeld surface analysis of (2E,2′E)-1,1′-[seleno­bis­(4,1-phenyl­ene)]bis­[3-(4-chloro­phen­yl)prop-2-en-1-one]

In the title organoselenium com­pound, the C—Se—C angle is 99.0 (2)°, with the dihedral angle between the planes of the attached benzene rings being 79.1 (3)°.

Crystal structure and Hirshfeld surface analysis of 2,2′-{(1E,1′E)-[ethane-1,2-diylbis(aza­nylyl­idene)]bis­(methanylyl­idene)}bis­[4-(tri­fluoro­meth­oxy)phenol]copper(II) hydro­quinone hemisolvate

The title structure has a square-planar coordination sphere around the copper(II) ion. In the crystal, mol­ecules are linked by weak C—H⋯O and C—H⋯π hydrogen bonds and very weak π-stacking inter­actions, forming a three-dimensional supra­molecular architecture.

Crystal structure and Hirshfeld surface analysis of (E)-6-(4-hy­droxy-3-meth­oxy­styr­yl)-4,5-di­hydro­pyridazin-3(2H)-one

In the title com­pound, inter­molecular C—H⋯O, O—H⋯O and N—H⋯O hydrogen bonds link the mol­ecules into a three-dimensional supra­molecular network.

Synthesis and crystal structure of (E)-2-({2-[aza­niumyl­idene(methyl­sulfan­yl)meth­yl]hydrazinyl­idene}meth­yl)benzene-1,4-diol hydrogen sulfate

The title mol­ecular salt was obtained through the protonation of the azomethine N atom in a sulfuric acid medium. The crystal com­prises two entities, a thio­semicarbazide cation and a hydrogen sulfate anion. The cation is essentially planar and is further stabilized by a strong intra­molecular O—H⋯N hydrogen bond.

Different packing motifs mediated by weak inter­actions and polymorphism in the crystal structures of five 2-(benzyl­idene)benzosuberone derivatives

The title com­pounds, which differ in the substituent at the 4-position of the pendant benzene ring, show different packing motifs mediated by weak C—H⋯X (X = O or N) inter­actions. One of them is a polymorph of a known structure.

Crystal structure and photoluminescence properties of catena-poly[[bis­(1-benzyl-1H-imidazole-κN³)cadmium(II)]-di-μ-azido-κ⁴N¹:N³]

The crystal structure and photoluminescence properties of a new one-dimensional Cd^II coordination polymer constructued by azide and 1-benzyl­imidazole (bzi) are reported.

Crystal structure, Hirshfeld surface analysis and DFT studies of ethyl 2-{4-[(2-eth­oxy-2-oxoeth­yl)(phen­yl)carbamo­yl]-2-oxo-1,2-di­hydro­quinolin-1-yl}acetate

The title com­pound, C₂₄H₂₄N₂O₆, consists of ethyl 2-(1,2,3,4-tetra­hydro-2-oxoquinolin-1-yl)acetate and 4-[(2-eth­oxy-2-oxoeth­yl)(phen­yl]carbomoyl units, where the oxo­quinoline unit is almost planar and the acetate substituent is nearly perpendicular to its mean plane. In the crystal, C—H_Oxqn⋯O_Ethx and C—H_Ph­yl⋯O_Carbx (Oxqn = oxoquinolin, Ethx = eth­oxy, Phyl = phenyl and Carbx = carboxyl­ate) weak hydrogen bonds link the mol­ecules into a three-dimensional network structure. A π–π inter­action with a centroid-centroid distance of 3.675 (1) Å between the constituent rings of the oxo­quinoline unit may further stabilize the structure.

Crystal structure of a two-dimensional coordination polymer of formula [Zn(NDC)(DEF)] (H₂NDC is naphthalene-2,6-di­carb­oxy­lic acid and DEF is N,N-di­ethyl­formamide)

The zinc metal organic framework poly[bis­(N,N-di­ethyl­formamide)(μ₄-naphthalene-2,6-di­carboxyl­ato)(μ₂-naphthalene-2,6-di­carboxyl­ato)dizinc(II)], built from windmill-type secondary building units and forming zigzag shaped two-dimensional stacked layers, has been solvothermally synthesized from naphthalene-2,6-di­carb­oxy­lic acid and zinc(II) acetate as the metal source in N,N-di­ethyl­formamide containing small amounts of formic acid.

Crystal structure and Hirshfeld surface analysis of 2-(4-nitro­phen­yl)-2-oxo­ethyl picolinate

2-(4-Nitro­phen­yl)-2-oxoethyl picolinate was synthesized under mild conditions. The chemical and mol­ecular structure was confirmed by single-crystal X-ray diffraction studies. The mol­ecules are related by inversion into centrosymmetric dimers via weak C—H⋯O inter­molecular inter­actions, and further strengthened by weak π–π inter­actions. A qu­anti­fication of the inter­molecular contacts in the crystal were estimated using Hirshfeld surface analysis and two-dimensional fingerprint plots.

Crystal structures of two dimeric nickel di­phenyl­acetate com­plexes

The mol­ecular and crystal structures of μ-aqua-κ²O:O-di-μ-di­phenyl­acetato-κ⁴O:O′-bis­[(di­phenyl­acetato-κO)bis­(pyridine-κN)nickel(II)] and μ-aqua-κ²O:O-di-μ-di­phenyl­acetato-κ⁴O:O′-bis­[(2,2′-bi­pyridine-κ²N,N′)(di­phenyl­acetato-κO)nickel(II)]–aceto­nitrile–di­phenyl­acetic acid (1/2.5/1) are reported. Hirshfeld surface analysis of both com­pounds have been carried out.

Crystal structure, Hirshfeld surface analysis and PIXEL calculations of a 1:1 epimeric mixture of 3-[(4-nitro­benzyl­idene)amino]-2(R,S)-(4-nitro­phenyl)-5(S)-(propan-2-yl)imidazolidin-4-one

A 1:1 epimeric mixture of 2(R,S)-(4-nitro­phen­yl)-3-[(4-nitro­benzyl­idene)amino]-5(S)-(propan-2-yl)imidazolidin-4-one was derived from an initial reaction of 2(S)-amino-3-methyl-1-oxo­butane­hydrazine at its hydrazine moiety to provide a 4-nitro­benzyl­idine derivative, followed by a cyclization reaction with another mol­ecule of 4-nitro­benzaldehyde to form the chiral five-membered imidazolidin-4-one ring.

Crystal structures of 2-(2-bromo-5-fluoro­phen­yl)-8-eth­oxy-3-nitro-2H-thio­chromene and 2-(2-bromo-5-fluoro­phen­yl)-7-meth­oxy-3-nitro-2H-thio­chromene

The synthesis and structure of 2-(2-bromo-5-fluoro­phen­yl)-8-eth­oxy-3-nitro-2H-thio­chromene (A) and 2-(2-bromo-5-fluoro­phen­yl)-7-meth­oxy-3-nitro-2H-thio­chromene (B) are described. In each crystal, the mol­ecules are linked by hydrogen bonds and π–π stacking inter­actions.

The `super acid' BF₃H₂O stabilized by 1,4-dioxane: new preparative aspects and the crystal structure of BF₃H₂O·C₄H₈O₂

The crystal structure of BF₃H₂O·C₄H₈O₂ – the dioxane adduct of the 'super acid' BF₃H₂O – is reported along with new preparative aspects and results of ¹H, ¹¹B and ¹³C and ¹⁹F spectroscopic investigations. The pronounced thermal stability of the solid adduct (m.p. 128–130 °C) in com­parison to the liquid com­ponents is attributed to the chain structure established by O—H⋯O hydrogen bonds of exceptional strength taking into account the mol­ecular (non-ionic) character of the structural moieties.

Crystal structure and Hirshfeld surface analysis of 2-(4-nitro­phen­yl)-2-oxo­ethyl 2-chloro­benzoate

The title compound, 2-(4-nitro­phen­yl)-2-oxoethyl 2-chloro­benzoate, is relatively planar with the two aromatic rings being inclined to each other by 3.56 (11)°.

Crystal structure of catena-poly[[[(2-eth­oxy­pyrazine-κN)copper(I)]-di-μ₂-cyanido] [copper(I)-μ₂-cyanido]]

The title compound, {[Cu(EtOpz)(CN)₂][CuCN]}_n, where EtOpz is 2-eth­oxy­pyrazine, is a two-dimensional polymeric copper complex with different coordination environments of the two Cu^I ions. One Cu atom is coordinated to the 2-eth­oxy­pyrazine mol­ecule and two bridging cyanide ligands, equally disordered over two sites. The second Cu atom is coordinated by two disordered over two sites bridging cyanide groups. Two copper–cyanide chains are connected through Cu⋯Cu contact.

Crystal structures of two coordination isomers of copper(II) 4-sulfo­benzoic acid hexa­hydrate and two mixed silver/potassium 4-sulfo­benzoic acid salts

A reaction of copper(II) carbonate and potassium 4-sulfo­benzoic acid in water acidified with hydro­chloric acid yielded two crystalline products, tetra­aqua­bis­(4-carb­oxy­benzene­sulfonato)­copper(II) dihydrate and hexa­aqua­copper(II) 4-carb­oxy­benzene­sulfonate. A reaction of silver nitrate and potassium 4-sulfo­benzoic acid in water also resulted in two distinct products, an anhydrous silver potassium 4-carb­oxy­benzene­sulfonate salt and a hydrated mixed silver potassium 4-carb­oxy­benzene­sulfonate salt dihydrate.

Synthesis and crystal structure of (E)-1,2-bis­[2-(methyl­sulfan­yl)phen­yl]diazene

In the crystal structure of the title compound, two half-mol­ecules are found in the asymmetric unit. The completed mol­ecules differ only slightly in bond lengths and torsion angles.