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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

November 2015 issue

Highlighted illustration

Cover illustration: Trimeric perfluoro-o-phenylene mercury is a macrocyclic Lewis acidthat can be used for the preparation of charge-transfer complexes with unusual optical properties. In combination with the unstable dienophilic compound tetracyanoethylene, this macrocycle reacted to the adduct [Hg3(C6F4)3]·C6N4. In the crystal structure, the macrocycle exhibits point group symmetry 2 and the tetracyanoethylene molecule point group symmetry \overline{1}. The latter is nearly perpendicular to the mean plane of the macrocycle at a dihedral angle of 88.20 (5)°. Intermolecular interactions between the moieties are weak with Hg...N distances to the nitrile N atoms from the three mercuryatoms of the macrocycle ranging from 2.990 (4) to 3.030 (4) Å Thermogravimetrical analysis revealed that upon complexation tetracyanoethylene is stable to higher temperatures compared to the free state. See: Castañeda, Timofeeva & Khrustalev [Acta Cryst. (2015). E71, 1375-1378].

research communications



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The title compound was produced unexpectedly from (±)-1,2-diphenyl-1,2-propane­diol by a sequential non-acid Pinacol rearrangement followed by acetal formation during recrystallization in 1-butanol. The tri-substituted dioxolane ring has a twist conformation and in the crystal, mol­ecules are linked by C—H⋯O hydrogen bonds, forming chains along [001].

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A 5:1 mixture of 4-hy­droxy­pyridine with benzene 1,3,5-tri­carb­oxy­lic acid in methanol yields the title hydrogen-bonded framework compound. This compound crystallizes in the ortho­rhom­bic space group Pna21 and is a polymorph of the same stoichiometric species, reported in Cc.

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The reaction of AgBF4 with the unsymmetrical ligand N-(pyridin-4-ylmeth­yl)pyridine-3-amine afforded a helical coordination polymer. The AgI atom adopts a slightly distorted linear coordination geometry. The symmetry-related right- and left-handed helical chains are arranged alternately via Ag⋯Ag and Ag⋯F inter­actions and π–π stacking inter­actions, resulting in the formation of a two-dimensional supra­molecular network.

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Crystal structures of three co-crystals of bis­(4-alk­oxy­benzoic acid) and 4,4′-bipyridyl have been determined at 93 K. The asymmetric unit of each compound comprises two crystallographically independent acid mol­ecules and one base mol­ecule, which are held together by O—H⋯N hydrogen bonds, forming a linear hydrogen-bonded 2:1 unit.

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The dinuclear complex [{Fe(CO)3}2(μ-L)] [L = 3,3-dimethyl-4-(propan-2-yl­idene)thietane-2,2-bis­(thiol­ate)] consists of two Fe(CO)3 moieties bridged by a di­thiol­ate ligand. This is the first crystal structure reported in which the 3,3-dimethyl-4-(propan-2-yl­idene)thietane-2,2-bis­(thiol­ate) ligand bridges two metal atoms.

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The title compound is an example of a 12-metallacrown-4 self-assembled supra­molecular coordination complex with ring MnIII ions. A YIII ion and Na+ ion are captured on opposite sides of the metallacrown cavity, and the YIII ion is tethered to the metallacrown with four tri­methyl­acetate anions.

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Using a predesigned tripodal Schiff-base ligand, a monomeric octa­hedral MnIV complex has been synthesized and its structure determined at 100 K.

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Mol­ecules of the title compound are linked via N—H⋯O(carbon­yl), N—H⋯O(hy­droxy) and O—H⋯O(carbon­yl) bonds into a 5-connected framework.

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Treatment of an irida­benzene with either bromine or iodine generates high-oxidation-state IrIII irida­benzenes that contain an open coordination site.

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In the title compound 1-thio­phen-2-yl­methyl­ene­amino­pyrimidine derivative, the pyrimidine and thienyl rings are inclined to one another by 42.72 (5)°. In the crystal, mol­ecules are linked by N–H⋯Nnitrile and N–H⋯O=C hydrogen bonds, forming chains parallel to the b axis.

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In the title compound compound, the phenyl and pyrimidine rings are inclined to one another at 31.72 (6)°. The residues are associated into ribbons parallel to [110] by three classical hydrogen bonds. Adjacent ribbons are connected by translation parallel to the c axis by a `weak' hydrogen bond to form a layer structure parallel to (1-10), while a further contact connects the residues in the third dimension.

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The crystal structures of two phospho­rus oxonitride polymorphs (cristobalite- and coesite-type) were redetermined by means of single-crystal X-ray diffraction data.

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The title compound, is the first tri-substituted cyclo­hex­yloxy triazine to be described. In the crystal, the triazine rings form (C3i-PU) Piedfort units and the mol­ecules are linked by C—H⋯O hydrogen bonds, forming ribbons propagating along [1-10].

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In the title compound, the 2-amino-1,3-di­bromo-6-oxo-5,6-di­hydro­pyrido[1,2-a]quinoxalin-11-ium cations are non-planar and are linked through centrosymmetric hydrogen-bonded cyclic Br2(H2O)2 anion–water units by N—H⋯Br, N—H⋯O and O—H⋯Br hydrogen bonds, forming one-dimensional ribbons, with the planes of the cations lying parallel to (100).

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The title compound, [Cr(urea)6](Cr2O7)Br·H2O, is isotypic with the corresponding chloride salt and consists of discrete [Cr(urea)6]3+ cations, staggered Cr2O74− and Br anions and water solvent mol­ecules that are held together by an intricate three-dimensional network of hydrogen-bonding inter­actions.

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Crystal structures of three co-crystals of 1,2-bis­(pyridin-4-yl)ethane with 4-alk­oxy­benzoic acids have been determined. The asymmetric unit of each compound comprises two crystallographically independent acid mol­ecules and one base mol­ecule, which are held together by O—H⋯N hydrogen bonds, forming linear hydrogen-bonded 2:1 units.

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The crystal structure of the novel organic–inorganic hybrid compound is based on a β-type Anderson polyoxidomolybdate anion containing a central FeIII ion. In the crystal, inter­molecular N—H⋯O and O—H⋯O hydrogen bonds link the components into a three-dimensional network structure.

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The title compound was prepared by the reaction of [butane-2,3-dione bis­(4-methyl­thio­semicarbazonato)]zinc(II) with pyridine. The ZnII atom is five-coordinate in a pseudo-square-pyramidal geometry.

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The anionic network of the new hybrid compound (C7H10NO)[BiI4]·2H2O is built up by edge-sharing [BiI6] octa­hedra leading to a one-dimensional structural topology. Hydrogen bonds ensure the crystal cohesion by connecting the alternating organic–inorganic layers and building a three-dimensional framework.

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The components of the ternary cocrystalline adduct are linked by inter­molecular O—H⋯N hydrogen bonds This is the first example of a 1:2 adduct containing two 4-nitro­phenol mol­ecules and one aza­adamantane structure.

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This report describes the crystal structure of highly substituted tri­fluoro­azepane as an important building block of therapeutic inter­est. Data were collected with synchrotron radiation on a very small crystal.

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In the isostructural ortho-tolyl N-pyridinylcarbamate and ortho-bromo­phenyl N-pyridinylcarbamate monohydrates, the primary aggregation involves cyclic hydrogen bonding as (amide–water–pyridine)2 comprising amideN—H⋯O—Hwater⋯Npyridine inter­actions about inversion centres [as R_{4}^{4}(14) rings]. The remaining H2O O—H donor and carbonyl O=C form a strong hydrogen bond. The participation of strong hydrogen-bonding donors and acceptors is maximized in short inter­actions, resulting in two-dimensional sheets.

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(N-Methyl-N-phenyl­carbamoyl)(N-methyl-N-phenyl­amino)sulfide and the corresponding disulfane are stable derivatives of (chloro­carbon­yl)sulfenyl chloride and (chloro­carbon­yl)disulfanyl chloride, respectively.

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The crystal structure and thermal properties of a mixed-stack donor–acceptor complex of trimeric perfluoro-o-phenyl­ene mercury with tetra­cyano­ethyl­ene in an 1:1 ratio were studied by X-ray diffraction and TGA methods.

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The title compounds are two closely related oxalate-bridged dinuclear copper complexes. The histamine ligand is in a gauche conformation and coordinates to copper ions in a bidentate chelating fashion. The dinuclear complexes are linked to form three-dimensional networks via different types of hydrogen-bond and weak inter­actions.

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The title salt, (C6H14N2)2[Bi2Cl10]·2H2O, bears a close resemblance to its homologous anti­monate structure. The crystal structure is formed by an alternating packing of organic and inorganic layers along [001] and contains isolated (Bi2Cl10)4− bi­octa­hedra.

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In the crystal structures of 4-meth­oxy-N-(4-methyl­phen­yl)benzene­sulfonamide and N-(4-fluoro­phen­yl)-4-meth­oxy­benzene­sulfonamide, the supra­molecular architecture of the former is controlled by C—H⋯πar­yl inter­actions, forming a two-dimensional architecture, while in the latter, a pair of C—H⋯O inter­molecular inter­actions lead to the formation of a three-dimensional architecture.

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The anhydrous morpholinium salts of phen­oxy­acetic acid, (4-fluoro­phen­oxy)acetic acid and the isomeric (3,5-di­chloro­phen­oxy)acetic acid and (2,4-di­chloro­phen­oxy)acetic acid, provide three similar examples of one-dimensional hydrogen-bonded chain polymers and one of a cyclic hydrogen-bonded hetero­tetra­mer.

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The title compound contains one independent mol­ecule which exhibits an overall ruffled conformation, with an average Ni—N bond length of 1.917 (13) Å. The mol­ecules form a closely spaced lattice structure in which neighbouring porphyrins are oriented in inversion-related dimers.


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In the crystal structure of the title compound, the mol­ecular components, viz. 4-(di­methyl­amino)­pyridinium cations, tris­[oxalatochromate(III)] anions and lattice water mol­ecules, are linked through O—H⋯O and N—H⋯O hydrogen bonds into a three-dimensional network. Additional π–π inter­actions between pyridinium rings stabilize this arrangement.

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The title compound exists in a trans conformation with respect to the methene C=C and the acyclic N=C bonds, with the 1,2,4-triazole-5(4H)-thione ring almost normal to the indole and benzene rings. In the crystal, mol­ecules are linked by pairs of N—H⋯S hydrogen bonds, forming inversion dimers with an R_{2}^{2}(8) ring motif.

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In the crystal, the acid H atom is twisted roughly 180° from the typical carb­oxy conformation and mol­ecules are linked by pairs of O—H⋯N hydrogen bonds, involving the indole N atom, forming inversion dimers. Together with a weak C—H⋯O hydrogen bond, involving the carbonyl O atom, chains of inversion dimers are formed along [100].

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The structure of hexa­amminecobalt(II) bis­[tetra­carbonyl­cobaltate(-I)] contains discrete octa­hedral [Co(NH3)6]2+ cations and [Co(CO)4] anions held together by N—H⋯O hydrogen bonds.

data reports

inorganic compounds


metal-organic compounds












organic compounds






















































addenda and errata


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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