[ (IUCr) Acta Crystallographica Section E Volume 76, Part 10, October 2020

issue contents

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

October 2020 issue

Highlighted illustration

Cover illustration: Even in the absence of high-quality single crystals, three-dimensional structural information may still be accessible. Using home-laboratory powder X-ray diffraction, Rietveld refinement, and optimization by density-functional theory calculations, the structures of disodium hydrogen citrate monohydrate, Na2HC6H5O7(H2O), and diammonium sodium citrate, (NH4)2NaC6H5O7, have been solved and refined. See: Hong, Bhaskar, Golab & Kaduk [Acta Cryst. (2020). E76, 1572-1578].

research communications


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The title compounds, [Ir(C51H64N2)(C8H12)Cl]·CH2Cl2 and [Ir(C51H64N2)(C8H12)Cl], represent the first two examples of hexa­hydro­benzo­imidazole-based N-heterocyclic carbene (NHC) iridium complexes. The diastereomeric complexes differing only in their axial chirality, which could be separated via column chromatography, show noticeable differences in their 1H NMR spectra.


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The title compound crystallizes with a single mol­ecule in the asymmetric unit. The phenol ring makes a dihedral angle of 36.56 (3)° with the nitro­benzene ring. In the crystal, mol­ecules are linked by C—H⋯O inter­actions, forming chains along the b-axis direction.

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The title compound was synthesized by a new type of reaction using Mg(ReO4)2 as a new catalyst and a possible mechanism for this reaction is proposed. In the crystal, hydrogen bonds connect the mol­ecules into double layers, which are connected to each other by halogen bonds.

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The synthesis and characterization of a new titanocene dichloride complex with tert-butyl esters appended to the cyclo­penta­diene rings is reported.

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The crystal structures of the isostructural mixed-cation compounds dipotassium rubidium citrate monohydrate and potassium dirubidium citrate monohydrate have been solved and refined using laboratory X-ray powder diffraction data and optimized using density functional techniques.

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The crystal structures of disodium hydrogen citrate monohydrate and di­ammonium sodium citrate have been solved and refined using laboratory X-ray powder diffraction data and optimized using density functional techniques.

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A novel bis­(anil) compound was synthesized and structurally characterized. Theoretical calculations suggested that the new bis­(hy­droxy­imine) will exhibit histone de­acetyl­ase SIRT2, histone de­acetyl­ase class III and histone de­acetyl­ase SIRT1 activities, and will act as inhibitor to aspulvinone di­methyl­allyl­transferase, de­hydro-L-gulonate deca­rboxylase and gluta­thione thiol­esterase.

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The ferrocene-bridged compound 1,1′-bis­(pyridyl­triazoylmeth­yl)ferrocene acquires an anti conformation in its solid state but forms a discrete tetra­nuclear [2 + 2] complex with [Cu(CH3CN)4](PF6) in solution.


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In the crystal, the mol­ecules are linked by C—H⋯N and weak C—H⋯π hydrogen bonds and very weak π–π stacking inter­actions. Two-dimensional fingerprint plots show that the largest contributions to the crystal stability come from H⋯H and C⋯H/H⋯C inter­actions.

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In the crystal, mol­ecules are linked by C—H⋯π inter­actions, resulting in the formation of sheets along the a-axis direction. Within the sheets, very weak π–π stacking inter­actions occur. The Hirshfeld surface analysis and fingerprint plots reveal that the crystal structure is dominated by H⋯H (37.1%) and C⋯H (30.1%) contacts.

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The structure of three functionalized chalcones (1,3-di­aryl­prop-2-en-1-ones), containing combinations of nitro and di­methyl­amino functional groups, are presented.

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Two new substituted propane­dioate esters have been synthesized using a three-component solvent-free thermal reaction. The products, which are isomorphous, differ only in the presence of a bromo­phenyl group in one, where the mol­ecules are fully ordered, as compared with a chloro­phenyl group in the other, where the mol­ecules exhibit two types of disorder.

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The crystal structures of magnesium hydrogen citrate dihydrate and bis­(di­hydrogencitrato)magnesium have been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques.

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The synthesis and crystal structures of three new disubstituted [13]-macrodilactones, trans-4,8-dimethyl-1,10-dioxa­cyclo­tridec-5-ene-2,9-dione, cis-4-(4-bromo­phen­yl)-13-methyl-1,10-dioxa­cyclo­tridec-5-ene-2,9-dione, and trans-11-methyl-4-phenyl-1,10-dioxa­cyclo­tridec-5-ene-2,9-dione are reported and their conformations are put in the context of other [13]-macrodilactone structures reported previously, showing that the number, location, and relative disposition of groups attached at the termini of planar units of the [13]-macrodilactones subtly influence their aspect ratios.

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The title structure consists of isolated [SnCl6]2− octa­hedral anions separated by layers of organic 1-(prop-2-en-1-yl)-1H-imidazol-3-ium (C6H9N2)+ cations. The crystal packing features inter­molecular N—H⋯Cl and C—H⋯Cl hydrogen bonds and π–π stacking inter­actions.

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The title compound features a very short, but asymmetric, O—H⋯O hydrogen bond having an O⋯O distance of 2.452 (3) Å within the anion.

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Cubic K2Ni0.5Hf1.5(PO4)3 crystallizes in the langbeinite structure type. The principal building units are two independent [(Ni,Hf)O6] octa­hedra, [PO4] tetra­hedra and [KO9] and [KO12] polyhedra.

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Single-crystals of thallium(I) iodide oxide Tl3IO were obtained as by-product in a hydro­flux synthesis at 473 K for 10 h. The oxygen atoms center thallium octa­hedra. The [OTl6] octa­hedra share trans faces, forming a linear chain along [001]. Twelve thallium atoms surround each iodine atom in an [ITl12] anti-cubocta­hedron. Thallium and iodine atoms together form a hexa­gonal close-sphere packing, in which every fourth octa­hedral void is occupied by oxygen.

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In the title bicyclic trinuclear pyrazolate amino­alcohol complex, the central Cu atom lies on a center of symmetry and has a distorted tetra­hedral coordination geometry while the peripheral Cu atom is in a trigonal–bipyramidal coordination environment.

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The crystal of the melaminium salt C3H7N6+·NCCH2COO·H2O was produced by mixing melamine with cyano­acetic acid in aqueous solution. The melaminium cations are inter­connected by N—H⋯N hydrogen bonds, forming tapes. These tapes of melaminium cations develop a three-dimensional network through multiple donor–acceptor hydrogen-bonding inter­actions between the cyano­acetate anions and water mol­ecules.

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In the crystal, two mol­ecules of the title compound form an inversion dimer, through C—H⋯π inter­actions, which further inter­acts with adjacent dimers to form a one-dimensional column structure.

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Short syntheses to high Fsp3 index natural-product analogues such as imino­sugars are of paramount importance in the investigation of their biological activities and reducing the use of protecting groups is an advantageous synthetic strategy. In this case only an iso­propyl­idene group was employed towards the synthesis of seven-membered ring imino­sugars.

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The mol­ecular and crystal structure as well as the Hirshfeld surface were analysed for this benzo­thia­zine derivative with potential analgesic activity.

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The title compound shows a cis-arrangement of the thio­cyanate anions, while the coordination polyhedron around the iron(II) atom is close to a trigonal prism.

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Co12P7, synthesized at high pressure/temperature conditions, crystallizes isotypically with ordered Cr12P7 in space-group type P\overline{6}.

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The structure of poly[bis­(μ4-2-methyl­propano­ato-η2-O3-O′)-μ2-aqua­dipotassium] (potassium isobutyrate hemihydrate) is reported. The structure is composed of cation–oxygen bilayers, which are surrounded by hydro­phobic methyl­ethyl chains on both sides. Stacking of these sandwiches forms the structure. The potassium cations are situated in an irregular coordination polyhedron composed of seven O atoms.

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The crystal structure of the title compound shows a disorder of the methyl and meth­oxy­carbonyl groups of one alanine residue. Compared to previously reported peptide biphenyl hybrids, the backbone torsion angles are different.

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In the crystal structures of the monohydrate and methanol solvate title compounds, the host mol­ecule adopts similar geometries with an alternating orientation of the substituents above and below the plane of the central arene ring.

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The crystal structures of [Ca(C4H7O2)(H2O)3](C4H7O2)·2H2O, space group Pbca, (I), and [Sr(C4H7O2)(H2O)3](C4H7O2)·2H2O space group Cmce (II) are homeotypic; [(Ca,Sr)(C4H7O2)(H2O)3](C4H7O2)·2H2O, space group Pbca, (III), is an Sr-containing solid solution of (I) with Ca2+ and Sr2+ occupationally disordered in the ratio 0.794 (2):0.206 (2).

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The crystal structure of aqua­(citric acid)(hydrogen citrato)calcium monohydrate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. A DFT-optimized structure is also reported for calcium hydrogen citrate trihydrate.

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In the crystal, each cation is connected to two anions by N—H⋯ Br hydrogen bonds, forming an R_{4}^{2}(8) motif parallel to the (10\overline{1}) plane, while the N,N-di­methyl­formamide mol­ecules are linked to the cations by C—H⋯O contacts.

addenda and errata



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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