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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

December 2017 issue

Highlighted illustration

Cover illustration: A new hybrid material, (C15H14N3)[NiCl4]Cl, comprising an almost planar terpyridinium trication, a tetrahedral tetrachloronickelate dianion and a free chloride anion shows promising luminescent properties. In the crystal packing, successive layers of terpyridinium chloride showing C/N-H...Cl interactions (layer A) and tetrachloronickelate (layer B) extend across the (100) plane. See: Zeghouan, Bendjeddou, Merazig & Daran [Acta Cryst. (2017). E73, 1937-1941].

research communications


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Resorcinarene-based tetra­phospho­nate cavitands are versatile mol­ecular receptors which combine a π-basic aromatic cavity with hydrogen-bond acceptor groups at their upper rim. Their complexation properties span from neutral mol­ecules to cationic species, and have been extensively studied both in solution and in the solid state. In this paper, we report the NMR solution studies and the crystal structure of a new supra­molecular complex between a tetra­phospho­nate cavitand and the nitrosyl cation NO+. The cation is disordered over two equivalent positions, and inter­acts with two adjacent P=O groups at the upper rim of the cavitand through a dipole–charge inter­action.

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A barium-μ2-oxygen motif develops along the a axis, connecting symmetry-related dinuclear BaII–CoII cationic fragments in a wave-like chain, forming a one-dimensional metal coordination polymer. Non-coordinating ClO4 anions are located in the space between the chains in this first example of a macrocyclic ligand forming a BaII-based one-dimensional coordination polymer, containing CoII ions surrounded by a N4O2 donor set.

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The asymmetric unit of the title compound consists of one and a half bis­chalcone mol­ecules. In the crystal, mol­ecules are linked into a three-dimensional network by C—H⋯F and C—H⋯O hydrogen bonds, some of the C—H⋯F links being unusually short (< 2.20 Å). Hirshfeld surface analyses are presented and discussed.

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In the title compound, the two indole ring systems are approximately perpendicular to one another, making a dihedral angle of 80.9 (5)°. In the crystal, pairs of N—H⋯O hydrogen bonds link the mol­ecules into inversion dimers and these are further linked by N—H⋯O and hydrogen bonds and short Cl—Cl contacts into supra­molecular chains.

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In the title compound, the toluene­sulfonamide ring and the combined ring system involving the pyridone and benzo­thia­zole rings subtend an inter­planar angle of 39.86 (4)°. The pyridone and benzo­thiazyl rings are linked by an intra­molecular N—Hamine⋯Nthia­zole hydrogen bond. The mol­ecules are linked by hydrogen bonds and an S⋯O contact to form layers parallel to the bc plane.

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The mol­ecular and crystal structure of a formal 20 electron zirconium(IV) complex bearing two cyclo­penta­dienyl and one sterically demanding penta­fulvene ligand is reported in which the penta­fulvene is bound in an η51 manner. The complex crystallizes together with toluene and n-hexane in a ratio of 1:0.125:0.125.

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The title diastereomeric salt, formed between 2-amino-1,2-di­phenyl­ethanol (ADE) and aspartic acid (ASP), crystallizes as a monohydrate. In the crystal, the ASP anions are linked via N—H⋯O hydrogen bonds to form a 21 helix along the b-axis direction.

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The simple synthesis and crystal structure of a new pyridinium bromide salt, 4-methyl-1-(3-phen­oxy prop­yl)pyridinium bromide, are reported. The C–H⋯Br inter­actions have an effect on the NMR signals of the ortho- and meta-pyridinium protons.

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The mol­ecules of the title compounds are effectively planar, apart from the methyl H atoms. In the crystals, C—H⋯O hydrogen bonds link the mol­ecules into chains in one compound and into sheets in the other.

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Crystal structures of hydrogen-bonded 1:2 dihydrate compounds of chloranilic acid with 2-carb­oxy­pyridine (I) and 2-carb­oxy­quinoline (II) have been determined at 180 and 200 K, respectively. The base mol­ecule in (I) is disordered over cationic and twitterionic states, while that in (II) is in a twitterionic form. In each crystal, the three components are linked by O—H⋯O and N—H⋯O hydrogen bonds, forming a layer structure.

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The title compounds were synthesized from the commercially available dye quinizarin. In both compounds, the anthra­quinone frameworks are close to planarity but there is a large difference in the conformation of the prop­yloxy group.

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The crystal structures of two (oxo­thia­zolidin-2-yl­idene)acetamides, namely (Z)-2-[2-(morpholin-4-yl)-2-oxo­ethyl­idene]thia­zolidin-4-one and (Z)-N-(4-meth­oxy­phen­yl)-2-(4-oxo­thia­zolidin-2-yl­idene)acetamide are described and compared with a related structure.

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BaMn2(AsO4)2 was isolated from a high-temperature halide flux. Its crystal structure is characterized by infinite sheets made up of AsO4 units and distorted MnO6 octa­hedra while barium cations inter­leave successive sheets. The layered framework comprises weakly inter­acting [Mn4O18]28− tetra­meric units. These units in the neighboring layer are separated from each other by 6.614 (2) Å (MnMn distance).

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The mol­ecular structure of the 2,5-di­aza­bicyclo­[2.2.1]heptane parent ring has been characterized for the first time. The asymmetric unit contains two crystallographically independent cages of 2,5-di­aza­bicyclo­[2.2.1]heptane, each cage being protonated at the two nitro­gen sites. The overall charge balance is maintained by four crystallogrphically independent bromide ions. In the crystal, the components of the structure are linked via a complex three-dimensional network of N—H⋯Br hydrogen bonds.

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The title mol­ecule is a tetra­substituted truxinic-type cyclo­butane derivative with a central ring that is almost planar despite of being placed in a general position. The mol­ecular structure of the dimer shows that the four benzene rings of the substituents are oriented in such a way that potential steric hindrance is minimized, whilst allowing some degree of inter­molecular π–π inter­actions for crystal stabilization.

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The reaction of HgII with the bridging ligand bis­(pyridin-3-ylmeth­yl)sulfane afforded a one-dimensional zigzag chain polymeric structure, with the charge balanced by two coordinated chloride anions. C—H⋯Cl hydrogen bonds and Hg—Cl⋯π inter­actions, together with C—H⋯π hydrogen bonds, stabilize the crystal structure.

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The synthesis and crystal structure of tridentate pyridine-2,6-di­carboxyl­ate CuII complex with a heterocyclic pyrazole ligand, a potential candidate for metal catalysts, are reported. The CuII atom is coordinated by three O atoms and two N atoms, provided by a tridentate pyridine-2,6-di­carboxyl­ate, one pyrazole and one water ligand, forming a slightly distorted square-pyramidal geometry.

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The title compounds are differing only by the position of the chlorine atom in the benzene ring. The mol­ecular structures are very similar, except for the relative position of the hy­droxy­phenyl rings.

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In the title compound, each CoII ion is coordinated by two pyridine N atoms from two individual dipyridyl ligands, two methanol O atoms and two chloride anions in an elongated octa­hedral geometry. Each dipyridyl ligand links two CoII ions, forming infinite zigzag chains.

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An aqueous 1:1 co-crystal salt formed from imidazole and picric acid was obtained in methanol solution. A three-dimensional hydrogen-bonded network is formed in the crystal by N—H⋯O, O—H⋯O and C—H⋯O hydrogen bonds and is further consolidated by π–π stacking inter­actions between pairs of imidazolium cations and picrate anions.

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Two mol­ecules comprise the asymmetric unit in the title thio­amide mol­ecule, each of which exists as the thioamide–thione tautomer. In the crystal, the mol­ecules assemble via an eight-membered thio­amide {⋯SCNH}2 synthon to form dimeric aggregates.

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This compound was previously shown to have anti­cancer activity in rodent test systems and recently found to have anti­fungal activity. The Pd centre is in a square-planar coordination environment with two chlorine atoms in cis positions and the remaining two coordination sites being coordinated by N and O atoms from deprotonated L-serine. Each of the Cs cations shows ninefold coordination with six chlorine and three O atoms resulting in a coordination environment that is similar to the well known Cs2SO4 structure.

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The planar deca­chloro­cyclo­penta­silane rings in the title compounds are coordinated by two chloride ions to generate inverse-sandwich complexes.

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In the title structures, each mol­ecules is connected to two other mol­ecules via four N—H⋯O hydrogen bonds, resulting in a chain with a sequence of R_{2}^{2}(8) rings.

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The title crystals are isomorphous, with tetra­meric Br⋯Br contacts as the principal packing inter­action. No CN⋯Br or NC⋯Br contacts are observed.

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The present work describes the synthesis and crystal structure of the new B-phenyl­oxaza­borocine, C26H23BN2O2. The title compound adopts a zwitterionic form with a significant intra­molecular N→B dative bond and inter­molecular C—H⋯O inter­actions connecting mol­ecules parallel to the b axis.

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Reaction of EuI2(THF)2 with K[HB(3,5-iPr2pz)] (= KTpiPr2, pz = pyrazol­yl) afforded the new europium(II) scorpionate complex (KTpiPr2)(3,5-iPr2pzH)2EuIII (1) in addition to the sterically crowded pyraza­bole derivative trans-{(3,5-iPr2pz)HB(μ-3,5-iPr2pz)}2 (2) which were both structurally characterized through X-ray diffraction.

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The title compound is a binuclear lanthanum(III) complex having each metal ion in deca­coordination with oxygen atoms from 1,4-chdc2− ligands, acetate groups and coordinated water mol­ecules to form a distorted bicapped square anti­prismatic geometry. The strong inter­molecular O–H⋯O and weak C–H⋯O inter­actions lead to the construction of a three-dimensional supra­molecular architecture.

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In the title compounds 1 and 2, the organic moieties adopt flattened conformations stabilized by an intra­molecular N—H⋯N hydrogen bonds formed by the protonated amino group and the N atom of the pyridyl substituent. In 1, the organic moieties are linked with two N—H⋯Cl-type hydrogen bonds, forming a C(4) graph-set. In its monohydrate, 2, the Cl anion and a water mol­ecule assemble the moieties into infinite bands showing hydrogen-bond patterns with graph sets C(6), R_{6}^{4}(12) and R_{4}^{2}(8). Both crystals display π–π stacked supra­molecular structures running along the b axis.

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The synthesis, and structural determination of 2,2′:6′,2′′-terpyridine-1,1′,1′′-triium tetra­chlorido­nickelate(II) chloride are reported. The crystal structure features N—H⋯Cl and C—H⋯Cl hydrogen bonds and Ni—Cl⋯π ring inter­actions.

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The whole mol­ecule of the title di­aryl­carbonate is generated by mirror symmetry, the mirror bis­ecting the central benzene ring, and the carbonate groups adopt an s-cis-s-cis conformation. In the crystal, there are only weak C—H⋯O hydrogen bonds and offset π–π inter­actions present.

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The effect of the nature of substitutions on the structural parameters and hydrogen-bonding inter­actions in N-acyl­hydrazone derivatives has been studied by synthesizing and determining the crystal structures of three ortho-substituted N-acyl­hydrazone derivatives, namely (E)-N-{2-[2-(2-chloro­benzyl­idene)hydrazin­yl]-2-oxoeth­yl}-4-methyl­benzene­sulfonamide (I), (E)-N-{2-[2-(2-methyl­benzyl­idene)hydrazin­yl]-2-oxoeth­yl}-4-methyl­benzene­sulfonamide (II) and (E)-N-{2-[2-(2-nitro­benzyl­idene)hydrazin­yl]-2-oxoeth­yl}-4-methyl­benzene­sulfonamide (III).

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Iridium(III) complexes based on 2,3′-bi­pyridine ligands are known to exhibit strong emission from blue to green that makes them of inter­est for organic light-emitting diodes and organic lighting uses. In the title compound, the IrIII ion adopts a distorted octa­hedral coordination environment defined by three C,N-chelating 2,6-di­fluoro-3-[5-(2-fluoro­phen­yl)pyridin-2-yl]pyridin-4-yl ligands in a meridional manner. In the crystal, inter­molecular C—H⋯F and C—H⋯π hydrogen bonds, as well as inter­molecular C—F⋯π inter­actions, are present, leading to a two-dimensional network.

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In the title compound, the two indole ring systems are approximately perpendicular to one another, making a dihedral angle of 89.7 (5)°. In the crystal, pairs of N—H⋯O hydrogen bonds link the mol­ecules into the inversion dimers, which are further linked into supra­molecular chains.

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The title compound is a new heterotrinuclear CoII–CaII–CoII dimer of L1. L1 undergoes a cobalt-driven preorganization, leading to the formation of an electron-rich area able to host a hard metal ion such as CaII. In the dimer, two neutral [Co(H–2L1)] moieties, held together by the CaII ion, are rotated by 90°. The trinuclear complexes form layers perpendicular to the c axis; the perchlorate anions are located between the layers and inter­act with the complexes, as well as the lattice water mol­ecules.

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The asymmetric unit of the title complex contains one half of the complex mol­ecule, one and a half ZnII cations, three benzoate (Bnz) and one pyridine-3-carbo­nitrile (CPy) mol­ecule; the Bnz anions act as bidentate ligands through the carboxyl­ate O atoms, while the Cpy anion acts as a monodentate N(pyridine)-bonding ligand. The complete centrosymmetric trinuclear complex thus comprises a linear array of three ZnII cations. In the crystal, the Bnz anions link to the Cpy N atoms via weak C—H⋯N hydrogen bonds, forming a two-dimensional network. The Hirshfeld surface analysis confirms the role of H-atom contacts in establishing the packing.

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The title compound, methyl 2-[5-(2-hy­droxy­phen­yl)-2H-tetra­zol-2-yl]acetate, is the major product from the reaction between 2-(2H-tetra­zol-5-yl)phenol and methyl 2-bromo­acetate in the presence of potassium carbonate, which gave three isomeric products.

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The crystal structure of the title compound has been determined at 100 K. In the crystal, O—H⋯O, C—H⋯On and C—H⋯F hydrogen bonds, and C—H⋯π and π–π inter­actions connect neighbouring mol­ecules.

Research communications

The first papers in this new format were published in July 2014. Research communications are longer papers with new text sections designed to help authors bring out the science behind their structure determinations. Figures are included in the published paper and, for the first time in Acta E, individual reports are not limited to single structure determinations. The Research communications format will make Acta E the natural home for structure determinations with interesting science to report.

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Acta E is now included in the Thomson Reuters Emerging Sources Citation Index.

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