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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

November 2019 issue

Highlighted illustration

Cover illustration: The title hydrated molecular salt, tetra-n-butylammonium 2,6-dioxo-1,2,3,6-tetrahydropyrimidine-4-carboxylate monohydrate, crystallizes with N-H...O and O-H...O hydrogen-bonded double-stranded antiparallel ribbons consisting of the hydrophilic orotate monoanions and water molecules, separated by the bulky hydrophobic cations. An accurate structure analysis conducted at T = 100 K is compared to a lower-resolution less accurate determination using data measured at T = 295 K. The structure at room temperature suffers not only from a complex disorder of one terminal ethyl group of the cation, but also produces weak diffraction, to the extent that from intensity statistics we estimate the effective resolution of the data to be about 1.0 Å. The data at T = 100 K are much stronger and give what in present times is regarded as an accurate result, which includes the observation of positive difference density at the centers of most of the bonds not involving H atoms. The results of both analyses were evaluated using a knowledge-based approach, and it was found that the less accurate room-temperature structure analysis provides geometric data that are similar to those derived from the accurate low-temperature analysis, with both sets of results consistent with previously analysed structures. See: Ara, Basdouri, Falvello, Graia, Guerra & Tomás [Acta Cryst. (2019). E75, 1632-1637].

research communications


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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.

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In the title compound, the ZnII 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.

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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\overline{1}). Both structures display extensive networks of O—H⋯O hydrogen bonds.

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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.

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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]).

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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.

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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.

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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.

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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.

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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.

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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.

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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.

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SrGa4As4 was synthesized under high-pressure/high-temperature conditions. The crystal structure com­prises a network of GaIIIAs4 tetra­hedra and ethane-like GaII2As6 groups with Ga—Ga bonds.

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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.

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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—HBnz⋯OThz (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—HMethy⋯SThz (Methy = methyl­ene) hydrogen bonds, enclosing R_{4}^{4}(22) ring motifs.

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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.

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

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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—HMthy⋯OCarbx (Mthy = methyl and Carbx = carboxyl­ate) hydrogen bonds. The ribbons are connected into layers parallel to the bc plane by inversion-related C—HBnz⋯π(ring) inter­actions.

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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 R_{2}^{2}(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.

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In the crystal structure of the title com­pound, the NiII 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].

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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.

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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.

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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.

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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.

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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.

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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)°.

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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)°.

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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.

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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.

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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.

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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.

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

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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—HOxqn⋯OEthx and C—HPh­yl⋯OCarbx (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.

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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.

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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.

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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.

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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.

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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.

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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.

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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)°.

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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 CuI 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.

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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.

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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.

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.

Emerging Sources Citation Index

Acta E is included in the Emerging Sources Citation Index.

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