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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

August 2019 issue

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Cover illustration: Metallamacrocyclic complexes of transition metals have been studied extensively over the past years for their properties (magnetic, optical, catalytic etc.) and as building blocks to synthesize supramolecular assemblies and coordination polymers endowed with a porous structure. In this framework, the present paper describes the crystal structures of three isostructural heteropolynuclear 15-metallacrown-5 complexes based on an LnCu5 core (Ln = Gd, Dy, Ho) and glycinehydroxamato as ligand. These complexes are discrete entities, due to the presence of the carbonate counter-ion which is coordinated in the apical position by the Ln ion, thus hampering the formation of polymeric structures. Their molecular structure, obtained with high-quality data, has been used as a model to re-evaluate the formula of a previously reported EuCu5 complex with glycinehydroxamate. See: Pavlishchuk, Naumova, Zeller, Calderon Cazorla & Addison [Acta Cryst. (2019). E75, 1215-1223].

research communications


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An investigation into the crystallization, crystal structure and packing analysis of the biologically active drug mol­ecule riluzole and its derivative, the riluzolium chloride salt, has been carried out.

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Two N′-(1-(phenyl­ethyl­idene)-2-(thio­phen-3-yl)acetohydrazides containing –OH and –OCH3 at the para-position of the phenyl ring have been synthesized and their mol­ecular and crystal structures are reported.

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The mol­ecule is a zwitterion and features a strong multicentered intra­molecular hydrogen bonding involving the carboxyl, amino, and anomeric hydroxyl groups. It adopts the 2C5 β-pyran­ose conformation, which also the dominant form present in its solution.

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In each crystal of the title compounds the packing is driven by C—H⋯F inter­tactions, along with a variety of C—F⋯π, C—H⋯π, C—Br⋯N, C—H⋯N, and C—Br⋯π contacts. Hirshfeld surface analysis was conducted to aid in the visualization of these various influences on the packing.

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Reaction of [RuCl2(DMSO)4] with 1-benzyl-4-(pyridin-2-yl)-1H-1,2,3-triazole yields two of the four possible isomers of the title compound.

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In the crystal structure of the title compound, the ZnII cation is octa­hedrally coordinated by the N atoms of a chelating phenanthroline ligand and the N atoms of two symmetry-related di­hydro­bis­(pyrazol-1-yl)borate ligands into discrete complexes.

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The crystal structures of two new isocoumarin derivatives, 8-amino-6-methyl-3,4-diphenyl-1H-isochromen-1-one and 8-amino-3,4-diethyl-6-methyl-1H-isochromen-1-one, are described. The inter­molecular contacts in the crystals were analysed using Hirshfeld surface analysis and two-dimensional fingerprint plots.

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The crystal structure of 2-[(2-oxo-2H-chromen-4-yl)­oxy]acetic acid di­methyl­sulfoxide monosolvate is described and the inter­molecular contacts in the crystal analysed using Hirshfeld surface analysis and two-dimensional fingerprint plots.

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The title compound crystallizes in the monoclinic space group P21/c with three independent mol­ecules in the asymmetric unit. Two types of hydrogen-bonding inter­actions, C—H⋯O and N—H⋯O, are observed, as well as bifurcation of these inter­actions. The N—H⋯O inter­actions link mol­ecules to form infinite chains. The packing of mol­ecules in the unit cell shows a pattern of overlapping aromatic rings, forming column-like formations. π–π inter­actions are observed between the overlapping aromatic rings.

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The asymmetric unit of the title solvate comprises a half mol­ecule of each component as both species are disposed about a centre of inversion. In the crystal, two-dimensional arrays are formed by amide-N—H⋯N(pyrid­yl) hydrogen bonds, which are connected into a three-dimensional architecture by C—H⋯π(benzene and pyrid­yl) inter­actions with benzene acting as the acceptor and donor, respectively.

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The di­hydro­indole portion is planar and the nonyl substituent is in an `extended' conformation. In the crystal, the nonyl chains inter­calate aided by pairwise C—H⋯O hydrogen bonds and the di­hydro­indole­dione units are associated through additional C—H⋯O hydrogen bonds to form micellar blocks. The blocks are linked through π-stacking inter­actions between the six-membered rings of the di­hydro­indole units.

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The title AgI compound based on 3-(1,2,4-triazol-4-yl)adamantane-1-carboxyl­ate (tr-ad-COO) is a three-dimensional coordination framework with channels along the c-axis direction. Hydrogen bonding between water mol­ecules of crystallization and carboxyl­ate groups is realised in form of right- and left-handed helical motifs.

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Cyanide anions bridge FeII and AuI cations to form a one-dimensional polymeric compound with free di­cyano­aurate anions.

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In each of the title compounds, the packing is driven by C—H⋯F inter­tactions, along with a variety of C—H⋯O, C—O⋯π, and C—F⋯π contacts. Hirshfeld surface analyses were conducted to aid in the visualization of these various influences on the packing.

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The title hydrated salt, tris­[hexa­amminecobalt(III)] tetroxidorhenate(VII) tetra­kis­[hexa­fluorido­rhenate(IV)] hexa­hydrate, arose unexpectedly due to possible contamination of the K2ReF6 starting material with KReO4. It consists of octa­hedral [Co(NH3)6]3+ cation (Co1 site symmetry 1), tetra­hedral [ReVIIO4] anions (Re1 site symmetry 1) and octa­hedral [ReIVF6]2− anions (Re site symmetries, Re2: 1; Re3 and Re4: \overline{3}). A network of N—H⋯F hydrogen bonds consolidates the structure.

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As the piperidin-1-ium group is nearly orthogonal to the quinolinyl residue in each of the two independent cations of the title salt solvate, these cations are L-shaped. Supra­molecular chains arise in the crystal as a result of charge-assisted O—H⋯O and N—H⋯O hydrogen bonding.

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The title compound is built up by two dioxolo, two pyridine, one pyridazine and one pyran rings. The two dioxolo rings are in envelope conformations, while the pyran ring is in twisted-boat conformation. The pyradizine ring is oriented at dihedral angles of 9.23 (6) and 12.98 (9)° with respect to the pyridine rings, while the dihedral angle between the two pyridine rings is 13.45 (10)°. In the crystal, C—Hdioxolo⋯Odioxolo, O—Hwater⋯Opyran, O—Hwater⋯Ometh­oxy­meth­yl and O—Hwater⋯Npyridazine hydrogen bonds link the mol­ecules into a supra­molecular structure. A weak C—Hmeth­oxy­meth­yl⋯π inter­action is also observed.

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In the crystal of the title salt, the cations and anions are linked via N—H⋯Br hydrogen bonds. In the 1H NMR spectra of this compound, the NH iminium protons are observed at δ = 10.46 p.p.m., which confirms the strong charge-assisted hydrogen bonding (CAHB) in the =HN+—HBr synthon.

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The crystal structure of the title compound consists of discrete complexes with a five-coordinate Ni cation and intra­molecular hydrogen-bonded di­chloro­methane solvent mol­ecules that are linked into dimers via pairs of inter­molecular C—H⋯S hydrogen bonds.

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The self-assembly of CuII selenate and 1,2,4-triazol-4-yl-acetic acid (trgly-H) in aqueous solution under hydro­thermal conditions affords a two-dimensional coordination network ([Cu33-OH)(trgly)3(SeO4)]·2H2O) based on triangular coordination clusters [Cu33-OH)] as secondary building units (SBUs). The trinuclear motif is supported by three [N—N] triazole bridges and a facially coordinating tripodal SeO42− anion. This results in a less distorted square-pyramidal arrangement around the five-coordinate copper(II) centres in comparison to that of the analogous isomorphous Cu33-OH)(trgly)3(SO4)]·2H2O complex.

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In the crystal structure, the mol­ecules are linked into layers parallel to the (020) plane by C—H⋯O contacts and face-to-face π–π stacking inter­actions between symmetry-related aromatic rings along the a-axis direction.

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The mol­ecule of the title compound has a C-shape, with Cs mol­ecular symmetry. The dihedral angle between the planes of the di­thiol and phenyl rings is 8.35 (9)°. In the crystal, mol­ecules form helical chains along [001], the shortest inter­actions being π⋯S contacts within the helices.


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In the title compound, {Fe(Etpz)2[Cu(CN)2]2}n, where Etpz is 2-ethyl­pyrazine, the low-spin FeII atom lies on an inversion centre and has an elongated octa­hedral [FeN6] coordination environment, where the axial positions are occupied by two 2-ethyl­pyrazine ligands and the equatorial positions are occupied by two pairs of symmetry-related cyanido groups. Each Cu2(CN)2 unit is connected to six FeII centres via two bridging 2-ethyl­pyrazine mol­ecules and four cyanido groups, resulting in the formation of a polymeric three-dimensional bimetallic metal–organic framework, additionally stabilized by Cu⋯Cu contacts.

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An organic–inorganic hybrid salt with two [L]2[CdI4] mol­ecules in the asymmetric unit related by pseudosymmetry exhibits a layered structure. In the mixed chloride/nitrate salt, the one-dimensional hydrogen-bonding polymer built of anions and water mol­ecules runs parallel to a column of stacked L+ cations.

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The crystal structures of three new isomorphous 3d–4f 15-metallacrown-5 complexes, [LnCu5(GlyHA)5(CO3)(NO3)(H2O)5xH2O (LnIII = Gd (1, x = 3.5); Dy (2, x = 3.28) and Ho (3, x = 3.45)), were determined. Structural details of the previously reported isotypic EuIII analogue were re­inter­preted.

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The preparation and structural characterization of the diazo-diphenanthroline compound, (E)-6,6′-(diazene-1,2-di­yl)bis­(1,10-phenanthrolin-5-ol) are described. The fully conjugated bis-phenanthroline mol­ecule is expected to offer exciting new physical and chemical properties, and should form the basis of novel metal coordination complexes as a consequence of the dual N,N′-1,10-phenanthroline chelating moieties situated on the opposite ends of the mol­ecule.

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The crystal structure of the title mol­ecular solvate features O—H⋯O hydrogen bonds, Br⋯O and π–π inter­actions. Hirshfeld surface analysis and fingerprint plots helped to identify the major contributors to the inter­molecular inter­actions.

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In the title mol­ecule, di-methyl­hydroxy and 4-nitro­benzene groups cap a central di-substituted acetyl­ene residue. The extended structure features flattened, hexa­meric clusters sustained by hy­droxy-O—H⋯O(hy­droxy) hydrogen bonds.

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The reaction of 2-methyl­thio-5-amino-1,3,4-thia­diazole with copper(II) acetate monohydrate resulted in the formation of the title binuclear compound



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Six new 1-aroyl-4-(4-meth­oxy­phen­yl)piperazines have similar mol­ecular structures, but their supra­molecular assembly ranges from simple chains, via a chain of rings, to complex sheets.

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A molybdenum tris­(di­thiol­ene) complex acts as a ligand towards three Co(CO)2 units.

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The crystal structure of a palladium(II) coordination compound features the same ligand bound to the metal center in both a κ2 and κ3 fashion.

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The crystal of 6-(4-nitro­phen­yl)-7-phenyl-5-thia-7-aza­spiro­[2.6]nonan-8-one (1), has monoclinic (P21/n) symmetry while that of its isomer 6-(3-nitro­phen­yl)-7-phenyl-5-thia-7-aza­spiro­[2.6]nonan-8-one (2), has ortho­rhom­bic (Pca21) symmetry: compound 1 has two mol­ecules, A and B, in the asymmetric unit while 2 has one. In all three mol­ecules, the seven-membered thia­zepan ring exhibits a chair conformation. Except for the nitro groups, the three mol­ecules have similar conformations when overlayed in pairs.

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The title salt crystallizes with three independent ionic pairs in the asymmetric unit. In the crystal, (3,5-di­methyl­adamantan-1-yl)ammonium cations and methane­sulfonate anions associate via N—H⋯O hydrogen bonds into layers that extend parallel to (001) and comprise large supra­molecular hydrogen-bonded rings.

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The title compound is constructed by a 4-hy­droxy­benzyl ring, a 3,4-di­hydroxy­benzyl­idenyl ring and a hydrazide-connecting bridge. The overall conformation of the title compound are discussed and compared to the related structures. In the crystal, mol­ecules are connected by N—H⋯O, O—H⋯O and π–π inter­actions.

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The synthesis and crystal structures of four dimeric complexes composed of manganese(II) dibromide, a pyridine N-oxide and solvent mol­ecules are reported. The pyridine N--oxide, 2-methyl­pyridine N-oxide, 3-methyl­pyridine N-oxide, and 4-methyl­pyridine N-oxide complexes all form similar structures with slight differences owing to the substituent group effects.

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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Acta E is included in the Emerging Sources Citation Index.

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