issue contents

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

February 2017 issue

Highlighted illustration

Cover illustration: Different crystallization conditions for the same reaction mixture led to two distinct terbium-tripodal alcohol complexes, viz. Tb(H3LEt)2(NO3)2](NO3)·0.5C4H10O2 and [Tb(NO3)(H3LEt)2(H2O)](NO3)2 (H3LEt = 1,1,1-tris­(hy­droxy­meth­yl)propane, C6H14O3. See: Gregório, Giese, Nunes, Soares & Hughes [Acta Cryst. (2017). E73, 278-285].

research communications


link to html
The title compound was obtained from the condensation reaction of 3,5-di-tert-butyl-4-hy­droxy­benzaldehyde and 2,4-di­nitro­phenyl­hydrazine. The essential part (including all the non-hydrogen atoms except two methyl carbons) of the mol­ecule lies on a mirror plane, which bis­ects the t-butyl groups.

link to html
The title compound was synthesized as a derivative of hepta­zethrene bearing two methyl and two tert-butyl­phenyl substituents, respectively, at the 1,9- and 7,15-positions. Albeit remotely located, the substituents contort the hepta­zethrene plane. The phenyl substituents stand approximately perpendicular to the core plane and prevent direct inter­molecular contacts of the hepta­zethrene cores.

link to html
Two NiII compounds forming zigzag chain structures through O—H⋯N hydrogen bonds between di­carb­oxy­lic acids and NiII complexes were synthesized, and their structures were determined. They are co-crystals rather than salts.

link to html
The syntheses and crystal structures of 3-chloro-3-methyl-r-2,c-6-di­phenyl­piperidin-4-one and two of its derivatives are described. In each structure, the piperidine ring adopts a chair conformation. In the crystals, mol­ecules are linked into C(6) chains by weak N—H⋯O hydrogen bonds and C—H⋯π inter­actions are also observed.

link to html
The title compound, C19H15N3O3, features an intra­molecular O—H⋯N hydrogen bond and an E conformation for the Schiff base unit.

link to html
The title compound contains an oxolane ring, and six defined stereocentres and may serve as a useful synthon for the synthesis of calcitriol analogues. The configurations of the chiral C atoms of the side chain were unambiguously established in the refinement.

link to html
Macrocyclic 22,24,25-trimethyl-8,11,14-trioxa-25-aza­tetra­cyclo­[19.3.1.02,7.015,20]penta­cosa-2,4,6,15 (20),16,18-hexaen-23-one obtained by a Petrenko–Kritchenko condensation of 1,5-bis­(2-formyl­phen­oxy)-3-oxa­pentane, pentan-3-one and methyl­ammonium acetate has been studied by X-ray structural analysis.

link to html
The title compound is an LiBr-bridged TiIV alkoxide dimer, supported by a novel monoanionic [NNN] pincer-type ligand. The bis­[2-(1-imino-2,2-di­methyl­prop­yl)-4-methyl­phen­yl]amine ligand is the first reported ligand that bears hydrogen atoms on its ketimine side arms.

link to html
The title complex, [Ir(C27H29N5)(C10H8N2)Cl]2+·2CF3SO3, was synthesized via the reaction of 2,6-bis­(N-butyl­benzimidazol-2′-yl)pyridine (bubzimpy) and 2,2′-bi­pyridine (bipy) with sodium hexa­chloro­iridate(III) and precipitated by adding aqueous sodium tri­fluoro­methane­sulfonate solution. The compound was characterized using single-crystal X-ray diffraction, FT–IR, cyclic voltammetry/rotating disc electrode polarography, fluorescence spectrometry, high resolution mass spectrometry, CHN elemental analysis and 1H NMR.

link to html
The crystal structure of caesium di­hydrogen citrate has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques.

link to html
The asymmetric unit of the title Schiff base contains three independent but conformationally similar mol­ecules that are linked in the crystal through inter­molecular N—H⋯N hydrogen bonds and C—H⋯π inter­actions, forming chains lying parallel to the c-axis direction.

link to html
Two mixed-valence compounds have been isolated from copper-cyanide-meen systems, Cu4(CN)5meen2 and Cu2(CN)3meen2·H2O, where meen is N-methyl­ethylenedi­amine. The former crystallizes as a polymer, in which CuIImeen2 moieties are covalently linked via cyanide bridges to a three-dimensional CuI cyanide-bridged array, while the latter is a binuclear monomer.

link to html
The title compound, [Rb(2.2.2)-crypt]3RbSn9, contains Rb+ cations, partially coordinated by 2.2.2-cryptand mol­ecules, and deltahedral nine-atomic tin cluster anions. The free Rb+ cations and the [Sn9]4– anions form strands extending parallel to [001].

link to html
The absolute structure of (R,R,SFc,SFc)-[Fe2(C5H5)2(C38H36BrNP2)]·Br·CH2Cl2 has been determined by X-ray single-crystal diffraction.

link to html
Wavy layers of mol­ecules are formed in the crystal structure of 5-methyl­salicyl­aldehyde due to weak C—H⋯O inter­actions between methyl groups and the aromatic ring system. Mol­ecules form columns in which the methyl groups are oriented in opposite directions layer-by-layer along cell axis a. In the mol­ecule, the hydroxyl substituent is bound intra­molecularly to the aldehyde group at the ortho position.

link to html
The title compound has been crystallized in liquid ammonia as a reaction product of the reductive ammonolysis of the natural compound streptozocin. Elemental rubidium was used as reduction agent as it is soluble in liquid ammonia, forming a blue solution. Reductive bond cleavage in biogenic materials under kinetically controlled conditions offers a new approach to gain access to sustainably produced raw materials.

link to html
Two tetra­chlorido­zincate salts of 4-carb­oxy-1H-imidazol-3-ium were structurally characterized. The first crystallizes with a water mol­ecule of hydration and the second with a water of hydration and two equivalents of the zwitterion 4-carb­oxy-1H-imidazole per salt formula unit.

link to html
The mol­ecule of 5-nitro­isatin-3-phenyl­hydrazone deviates slightly from a planar geometry. In the crystal, mol­ecules are linked by hydrogen bonding into a two-dimensional polymer along (120), forming rings of graph-set motifs R_{2}^{2}(8), R_{2}^{2}(26), R_{4}^{4}(32) and S(6). In addition, mol­ecules are stacked along the [100] through C=O⋯Cg inter­actions, as suggested by the Hirshfeld surface, which also indicates that the most important contributions for the crystal structure cohesion are O⋯H (28.5%) and H⋯H (26.7%) inter­actions. An in silico evaluation of the title compound with the di­hydro­folate reductase enzyme was performed and N—H⋯O and CgCg inter­actions were found.

link to html
In the title compound, the 1,2,4-triazole ring is twisted with respect to the mean plane of quinoline moiety at 65.24 (4)°. In the crystal, mol­ecules are linked by weak C—H⋯O and C—H⋯N hydrogen bonds.

link to html
In the title 1-oxo-1,2-di­hydro­naphthalene derivatives, the cyclo­hexa-1,3-diene rings of the 1,2-di­hydro­naphthalene ring systems adopt half-chair, boat and half-chair conformations, respectively. In the crystal of the methyl­phenyl compound, the mol­ecules are linked via C—H⋯O, C—H⋯π and π–π inter­actions, forming a double-chain structure, while in the crystals of the other two compounds, mol­ecules are linked by π–π inter­actions, forming a chain structure.

link to html
The title compound crystallizes in the monoclinic space group P21, with four crystallographically independent mol­ecules, having a very similar conformation, in the asymmetric unit. The cluster of independent mol­ecules has approximate non-crystallographic C2 point symmetry.

link to html
The redetermined structure of NaK5Cl2(S2O6)2 shows a super-cell, which accommodates subtle changes in the orientation of the O atoms of the di­thio­nate groups compared to the previously reported structure.

link to html
The NiII cation is coordinated by three N atoms of three different 1,3,5-tris­(imidazol-1-ylmeth­yl)benzene ligands, one O atom of an ethane-1,2-diol mol­ecule, by a sulfate anion and a water mol­ecule, forming a distorted octa­hedral NiN3O3 coordination geometry. The tripodal 1,3,5-tris­(imidazol-1-ylmeth­yl)benzene ligands link the NiII cations to generate a metal–organic chain running along [100].

link to html
Copper is known for its variable coordination geometry adopted for different ligands. Here we report the crystal structure of a new imidazo[1,2-a]pyridin-1-ium tetra­chlorido­cuprate(II) salt with a distorted tetra­hedral geometry for the copper atom.

link to html
The title compound, Rb2O2·2NH3, has been obtained as a reaction product of rubidium metal dissolved in liquid ammonia and glucuronic acid. As a result of the low-temperature crystallization, a disolvate was formed. The peroxide bond length is 1.530 (11) Å

link to html
p-Arsanilic acid forms an isotypic set of three compounds with the alkali metals K, Rb and Cs, in which the primary layered coordination polymeric structures have similar asymmetric units comprising two independent and different metal cations and a bridging water mol­ecule which lie within crystallographic mirror planes parallel to (100). The layers are linked across [100] through amine N—H⋯O hydrogen bonds to arsonate and water O-atom acceptors, giving overall three-dimensional network structures.

link to html
The title compound exhibits a polymeric structure caused by long Cu⋯O inter­actions, which lead to the formation of chains parallel to [100]. In the crystal, the chains are arranged in a distorted hexa­gonal rod packing.

link to html
An octa­hedral fac-C3NS2 coordination geometry is found for the ReI atom in the title compound; the di­thio­carbamate ligand forms symmetric Re—S bonds. In the crystal, supra­molecular layers are formed via weak C—H⋯O inter­actions.

link to html
The crystal structure of the title compound comprises a segregated columnar structure of cations and anions extending parallel to the b axis

link to html
(E)-4-Hy­droxy-6-methyl-3-{1-[2-(4-nitro­phen­yl)hydrazinyl­idene]eth­yl}-2-H-pyran-2-one has been synthesized and characterized by single-crystal X-ray diffraction and by using FT–IR, 1H and 13C NMR and UV–Vis spectroscopic techniques.

link to html
The crystal structure of trirubidium citrate monohydrate has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques.

link to html
The crystal structure of dicesium hydrogen citrate has been solved using laboratory X-ray single-crystal diffraction data, refined using laboratory powder data, and optimized using density functional techniques.

link to html
Two independent copper(II) cations with coordination numbers of 4 and 6 are bridged by dianionic salicylate anions into chains extending parallel [001]. O—H⋯O hydrogen-bonding inter­actions involving both the coordinating and the lattice water mol­ecules result in the formation of a three-dimensional network.

link to html
A new arsenate K1 + 2xNi1 - xFe2(AsO4)3 (x = 1/8) was synthesized using a flux method and its crystal structure was determined from single-crystal X-ray diffraction data. It appears closely related to the α-CrPO4 structure type. The proposed structural model was validated by bond-valence-sum calculations, charge-distribution and Madelung energy analyses

link to html
A new centrosymmetric chloride-bridged CuII dimeric anion, in which one carboxyl group of the pyridine-2,4-di­carb­oxy­lic acid ligand remains protonated, is present in the title structure, together with a diprotonated piperazine as a charge-compensating agent.

link to html
The crystal structure of trirubidium citrate has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques.

link to html
The title nitro­pyrrole-based compounds are inter­mediates used in the synthesis of modified DNA minor-groove binders. They are ethyl 4-nitro-1H-pyrrole-2-carboxyl­ate, its derivative ethyl 4-nitro-1-(4-pentyn­yl)-1H-pyrrole-2-carboxyl­ate, N-[3-(di­methyl­amino)­prop­yl]-1-isopentyl-4-nitro-1H-pyrrole-2-carboxamide and 1-(3-azido­prop­yl)-4-(1-methyl-4-nitro-1H-pyrrole-2-carboxamido)-N-[2-(morpholin-4-yl)eth­yl]-1H-pyrrole-2-carboxamide.

link to html
A skew trapezoidal bipyramidal coordination geometry based on a C2S4 donor set is found in the structure of (C6H5)2Sn[S2CN(Me)CH2CH2OMe]2, with the SnIV atom lying on a mirror plane.

link to html
The hexa­nuclear copper pyrazolato complex has a trigonal prismatic shape and contains an encapsulated chloride ligand.


link to html
A direct synthesis of monomeric IrCl(1,5-cod)2 (1,5-cod = cyclo­octa-1,5-diene) from IrCl3·3H2O and its crystal structure are presented. The mol­ecule's shape is midway between square pyramidal and trigonal bipyramidal.

link to html
Two new mononuclear complexes of ten- and nine-coordinate terbium(III) were synthesized from Tb(NO3)3·5H2O and the tripodal alcohol 1,1,1-tris­(hy­droxy­meth­yl)propane (H3LEt) to be employed as potential building blocks for heterometallic 3d–4f block metal aggregates.

link to html
The crystal structure of penta­sodium hydrogen dicitrate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques.

link to html
There are two mol­ecules in the asymmetric unit of the title compound, one of them being disordered over the methyl group. The mol­ecules are linked by weak H⋯S inter­actions into chains with graph-set motifs C(4) along [100] and and R_{2}^{1}(10) rings. The Hirshfeld surface calculation suggests that the most important contribution for the crystal structure are the H⋯H inter­actions (64.20%).

link to html
The crystal structure of the title compound, dimethyl 2-((2Z,5Z)-5-(2-meth­oxy-2-oxo­ethyl­idene)-2-{(E)-[2-methyl-5-(prop-1-en-2-yl)cyclo­hex-2-enyl­idene]hydrazinyl­idene}-4-oxo­thia­zolidin-3-yl)fumarate displays a conformational disorder which inverts the configuration of the chiral C atom within the cyclo­hexyl­idene ring.

link to html
The two title compounds are pyrazine-2,3,5,6-tetra­carboxamide derivatives. In the first crystal, mol­ecules are linked by N—H⋯O and N—H⋯O hydrogen bonds, forming a two-dimensional network structure. In the second crystal, an N—H⋯N hydrogen bond links the mol­ecules into a chain structure, while a further weak N—H⋯N hydrogen bond links the chains, forming a two-dimensional network structure.

link to html
The two title compounds are (di­amino­pyrimidin-2-yl)thio­acetamide derivatives. In the first structure, the pyrimidine ring is inclined to the naphthalene ring system by 55.5 (1)°, while in the second, the pyrimidine ring is inclined to the benzene ring by 58.93 (8)°. In the crystals of both compounds, mol­ecules are linked by pairs of N—H⋯N hydrogen bonds, forming inversion dimers with R_{2}^{2}(8) ring motifs.

link to html
The mol­ecular structure of the title compounds may be visualized as two octa­hedral metal coordinated units, fused through μ-oxide bridges across symmetry centres, leading to edge-sharing dimers.

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.

Journal news

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

ESCI

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds