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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

July 2020 issue

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Cover illustration: Neutron powder diffraction has been used to redetermine the structure of hemihydrate phenol. This very simple alcohol is an ideal system to analyse the interplay/competition of different supramolecular forces (hydrogen bonding, [pi]-[pi] stacking and C-H...[pi] interactions) in determining the outcome of the solid-state packing. The hemihydrate form described in the paper gives rise to inversion dimers bridged by water molecules, which then propagate in supramolecular chains along the c-axis direction. The chains are held together in the bc plane via C-H...[pi] interactions. The different interactions governing the crystal structure impact the thermal expansion properties of the material. See: Fortes [Acta Cryst. (2020). E76, 1062-1069].

research communications


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The title hexa­thia­pyrazino­phanes are regioisomers, having a central tetra-2,3,5,6-methyl­ene­pyrazine unit with two –S—CH2—CH2—S—CH2—CH2—S– chains linking the methyl­ene C atoms at positions 2 and 6 and 3 and 5 in the m-bis regioisomer, but linking the methyl­ene C atoms at positions 2 and 5 and 3 and 6 in the p-bis regioisomer.

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The reaction of the hexa­thia­pyrazino­phane ligand, 2,5,8,11,14,17-hexa­thia-[9.9](2,6,3,5)-pyrazino­phane, with copper(II) dibromide lead to the formation of a binuclear complex. Reaction with copper(I) iodide also gave a binuclear complex, which is bridged by a Cu2I2 unit to form a two-dimensional coordination polymer.

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The title hydrazine carbodi­thio­ate chloro­form hemi-solvate features approximately planar mol­ecules with splayed phenyl groups. Supra­molecular tapes are formed in the crystal through a combination of N—H⋯S, hydroxyl-O—H⋯O(hydrox­yl) and hydroxyl-O—H⋯π(phen­yl) inter­actions.

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The complete mol­ecule of the hexa­metallic title complex, namely, tetra­bromido­tetra-μ-hydroxido-hexa­kis­[μ-2-methyl-3-(pyrrolidin-1-yl)propan-2-olato]hexa­zinc(II) acetone disolvate, is generated by a crystallographic centre of symmetry. Two of the unique zinc atoms adopt distorted ZnO2NBr tetra­hedral coordination geometries and the other adopts a ZnO3N tetra­hedral arrangement. Both unique alkoxide ligands are N,O-chelating and both hydroxide ions are μ2 bridging.

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The title compound represents the di­fluoro­phosphate salt of Nitron, an analytical reagent used for gravimetrical analysis of nitrate ions. An analysis of the bond–length distribution and average bond lengths in PO2F2 tetra­hedra is given.

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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. The dimers are linked by the offset face-to-face π–π stacking inter­actions.

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Three new platinum(II) complexes bearing an isopropyl eugenoxyacetate and pyridine derivatives have been synthesized and further characterized by single-crystal X-ray diffraction.

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The synthesis and crystal structure of a diisopropyl-substituted p-tolunesulfonamide is discussed. This structure features C—H⋯O hydrogen bonds (both intra- and inter­molecular) and inter­molecular C—H⋯π inter­actions.

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Three [CoO6] octa­hedra, one [CoO4] tetra­hedron and three PO4 tetra­hedra are linked into a three-dimensional framework structure exhibiting channels parallel to [100] in which the eleven-coordinate strontium cations are located.

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The mol­ecular structure of the title compound comprises two parts, xanthene and iso­indole, sharing a central quaternary carbon atom. Both the xanthene and iso­indole moieties are nearly planar and are almost perpendicular.

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The asymmetric unit of the title compound comprises three independent mol­ecules of similar geometry. The crystal structure is stabilized by inter­molecular C—H⋯N and C—H⋯Cl hydrogen bonds in addition to C—Cl⋯π inter­actions.

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The title compound, {[Cu(succ)(tmeda)]·4H2O}n, consists of one-dimensional polymeric chains in which the central metal atom is coordinated in a distorted square-planar geometry by one oxygen atom each from two succ ligands and two TMEDA ligand nitro­gen atoms.

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The addition of tert-butyl hydro­peroxide (tBuOOH) to two MnII complexes, differing by a small synthetic alteration from an ethyl to a propyl linker in the ligand scaffold, results in the formation of the high-valent bis-oxo complexes {[MnIV(N4(6-Me-DPEN))]2(μ-O)2}2+ (1) and {[MnIV(N4(6-Me-DPPN))]2(μ-O)2}2+ (2).

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The crystal structure is reported of a single crystal containing potassium salts of two different tert-butyl­cyanamide anions that co-crystallized with one equivalent of 1,3-di-tert-butyl urea.

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The title compound is constructed about a tri-substituted 1,2,3-triazole ring, with the substituent at the C atom flanked by the C and N atoms being a substituted amide group, and with the adjacent C and N atoms bearing phenyl and benzyl groups, respectively. In the crystal, pairwise amide-N—H⋯O(carbon­yl) hydrogen bonds give rise to a centrosymmetric dimer.

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In each of the title newly synthesized and closely related N-{[4-(3-aryl-4-sydnonyl­idene­amino)-5-sulfanyl­idene-1H-1,2,4-triazol-3-yl]meth­yl}benzamides, which crystallized as ethanol monosolvates, the independent components are linked by hydrogen bonds to form centrosymmetric four-mol­ecule aggregates.

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The existing crystal structure of phenol hemihydrate is shown to be incorrect and a new model, refined from high-resolution neutron powder diffraction data, is reported.

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The title compound comprises two mol­ecules in the asymmetric unit. Inter­molecular C—H⋯O and N—H⋯O hydrogen bonds lead to a three-dimensional network structure.

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The title compound, C15H15NO, shows an intra­molecular O—H⋯N hydrogen bond and the aromatic rings are tilted by 45.73 (2)°.

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The title compound, containing a tetra-substituted pyrrolidine ring, has an N-bound (equatorial) 4-nitro­phen­yl)ethyl­carboxyl­ate group with an adjacent C-bound 4-meth­oxy­phenyl (bis­ectional) and then two acet­yloxy subtituents in equatorial and axial positions, respectively. The five-membered ring is twisted about the bond bearing the acet­yloxy subtituents.

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The title compound represents the first example of a diphosphane-bridged heterobimetallic Fe—Pt dimetalla­cyclo­pentenone complex resulting from a bimetallic activation of metal-coordinated carbonyl ligand with an inter­nal alkyne, namely 1,4-bis­(p-tolyl­thio)­but-2-yne. The bridging μ2-C(= O)C(CH2SC6H4Me-4)=CCH2SC6H4Me-4 unit (stemming from a carbon–carbon coupling reaction between CO and the triple bond of the alkyne di­thio­ether) forms a five-membered dimetalla­cyclo­pentenone ring, in which the C=C bond is π-coordinated to the Fe center.

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Charge-assisted C—H⋯π hydrogen bonds along with π–π inter­actions stabilize the crystalline state. Inter­molecular inter­actions are qu­anti­fied by Hirshfeld surface analysis.

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The crystal structure 5-[(benzo­yloxy)meth­yl]-5,6-dihy­droxy-4-oxo­cyclo­hex-2-en-1-yl benzoate a natural product from Pipers griffithii leaves known as zeylenone has been determined.

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The title compound, 2-(2-(meth­oxy­carbon­yl)-3,6-bis­(meth­oxy­meth­oxy)phen­yl)acetic acid, was synthesized as an inter­mediate for a possible total synthesis of the isocoumarin 3-methyl-3,5,8-trihy­droxy-3,4-di­hydro­isocoumarin.

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Bromination of 6,8-dimeth­oxy-3-methyl-1H-isochromen-1-one resulted in the formation of the 5-bromo derivative, 5-bromo-6,8-dimeth­oxy-3-methyl-1H-isochromen-1-one. The two mol­ecules differ essentially in the orientation of the meth­oxy group on position 6 of the isocoumarin ring system.

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During systematic investigations of the biological action enhancement of well known compounds, a new metal complex, (ethane-1,2-di­amine)­bis­(3,5-di­nitro­benzoato)zinc(II), was synthesized and the structure of its ortho­rhom­bic form has determined. The zinc ion has a distorted tetra­hedral environment formed by two monodentate 3,5-di­nitro­benzoato anions and chelating ethyl­enedi­amine mol­ecule.

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The isostructural crystal structures of Cu4FeGe2S7 and Cu4CoGe2S7 were solved and refined. All the metal cations form MS4 tetra­hedra and share corners to create a three-dimensional, non-centrosymmetric structure.

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In the title compound, the benzene rings make a dihedral angle of 62.73 (9)° with each other. In the crystal, mol­ecules are linked by a pair of C—Cl⋯π inter­actions, forming an inversion dimer. A short HL⋯·HL contact links the dimers, forming a ribbon propagating along the c-axis.

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Bis(benzo­thia­zol-2-yl)tri­thio­carbonate, C15H8N2S5, crystallizes in two visually distinguishable polymorphs, each containing a different conformer of the title compound and featuring different kinds of intra- and inter­molecular S⋯S, S⋯N and π–π inter­actions.

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Reduction of (C5H4SiMe3)3YbIII in THF using excess Cs metal forms the oligomeric complex [(THF)Cs(μ-η55-Cp′)3YbII]n. The complex has hexa­gonal layers of Cs3Yb3 with THF ligands and Me3Si groups in between the layers.

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Exceptionally large crystals of posnjakite, Cu4SO4(OH)6(H2O), formed during corrosion of a Swagelock(tm) Snubber copper gasket within the MX1 beamline at the ANSTO-Melbourne, Australian Synchrotron. The crystal structure was solved using synchrotron radiation and revealed a structure based upon [Cu4(OH)6(H2O)O] sheets, which contain Jahn–Teller-distorted Cu octa­hedra.

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The structural comparison of two Mn carbonyl complexes comprising a terpyridine derivative engaged in bidentate or tridentate coordination of the central MnI atom is reported.

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Mosher's Acid (systematic name: 3,3,3-tri­fluoro-2-meth­oxy-2-phenyl­propanoic acid) is a carb­oxy­lic acid that when resolved can be employed as a chiral derivatizing agent. The two independent mol­ecules in the asymmetric unit form a non-centrosymmetric homochiral dimer via inter­molecularly hydrogen-bonded head-to-tail dimers with graph-set notation R_{2}^{2}(8).

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In the title Schiff base compound, C13H9IN2O3, the hy­droxy group forms a intra­molecular hydrogen bond to the imine N atom and generates an S(6) ring motif. The 4-iodo­benzene ring is inclined to the phenol ring by 39.1 (2)°. The configuration about the C=N bonds is E. The crystal structure features C—H⋯O hydrogen-bonding inter­actions.

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In the title 1:1 solvate, 2,2′-di­thiodi­benzoic acid (DTBA):di­methyl­formamide (DMF), the DTBA mol­ecule is twisted [C—S—S—C = −88.57 (6)°]. Four-mol­ecule aggregates are formed in the crystal via DTBA-O—H⋯O(DMF) and DTBA-O—H⋯O(DTBA) hydrogen bonding. These are connected in three-dimensions by benzene-C—H⋯O(DTBA), DTBA-C=O⋯π(benzene) and benzene-C—H⋯π(benzene) inter­actions.

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The structures of two hy­droxy-thio­phenone derivatives related to the anti­biotic thiol­actomycin are presented. The main structural feature of both compounds is C(6) hydrogen-bonded chains formed between the OH and C=O groups.

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2-Ferrocenyl­carbonyl­benzoic acid (C18H14FeO3) was synthesized from the Friedel–Crafts acyl­ation of ferrocene with phthalic anhydride, and the product was reduced to 3-ferrocenylphthalide (C18H14FeO2) using Zn(Cu) in aqueous sodium hydroxide. Both compounds were characterized using IR, NMR, and single-crystal X-ray analysis.

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The asymmetric unit of the title salt consists of an olanzapinium cation, an independent 2,5 di­hydroxy­benzoate anion and a solvent isopropyl alcohol mol­ecule. The central seven-membered heterocycle is in a boat conformation, while the piperazine ring displays a distorted chair conformation. The dihedral angle between the benzene and thiene rings flanking the diazepine ring is 52.58 (19)°. In the crystal, the anions and cations are connected by N—H⋯O and O—H⋯O hydrogen bonds, forming a three-dimensional network.

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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