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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

November 2017 issue

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Cover illustration: Four mol­ecular salts made from hexa­methyl­ene­tetra­minium and 2-chloro-4-nitro­benzoate have been synthesized and are reported, namely ammonium hexa­methyl­ene­tetra­minium bis­(2-chloro-4-nitro­benzoate), NH4+·C6H13N4+·2C7H3ClNO4-, (I), hexa­methyl­ene­tetra­minium hydrogen bis­(2-chloro-4-nitro­benzoate), 0.5C6H13N4+·C7H3.50ClNO4-, (II), hexa­methyl­ene­tetra­minium 2-chloro-4-nitro­benzoate, C6H13N4+·C7H3ClNO4-, (IIIa) and (IIIb). All four mol­ecular salts show N+-H...O- hydrogen bonding. Salt (I), illustrated here, crystallized out with an NH4+ counter-ion which came from decomposition of 50% of the hexa­methyl­ene­tetra­minium cation in solution. (II) shows an unusual asymmetric unit, with both a hexa­methyl­ene­tetra­minium cation and a partially deproton­ated 2-chloro-4-nitro­benzoate anion. Salts (IIIa) and (IIIb) are polymorphs of each other but have different packing arrangements. This work shows that hexamethylenetetramine only protonates once, even in the presence of excess acid. See: Lemmerer & Motlaung [Acta Cryst. (2017). E73, 1630-1635].

research communications


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A novel three-dimensional bimetallic CdII–NaI metal–organic framework has been synthesized and the X-ray structure has been reported.

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The title compound is a polyoxygenated ep­oxy steroid that crystallizes in the P212121 space group.

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An intra­molecular amine-N—H⋯N(imine) hydrogen bond is found in the disubstituted amino­urea residue; the conformations about the imine and ethyl­ene double bonds are E. The packing features amide-N—H⋯O(carbon­yl) hydrogen bonds, leading to centrosymmetric aggregates, as well as C—H⋯O and C—H⋯π inter­actions, which significantly influence the packing.

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The binuclear mol­ecules of the title complex show weak inter­molecular C—H⋯Pd inter­actions, whereas the amine N—H functional groups are not involved in hydrogen bonding.

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The aceto­nitrile solvate and the ethanol hemisolvate of bis­(acetato-κO){5,6-dimethyl-2-(pyridin-2-yl)-1-[(pyridin-2-yl)meth­yl]-1H-benzimidazole-κ2N2,N3}copper(II) have been structurally characterized. Both compounds exhibit π–π inter­actions.

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In the title compound, the C=C—C—C torsion angles in the phenyl­methyl­idene units are 166.6 (3) and −48.0 (4)°. In the crystal, mol­ecules form a three-dimensional network by means of weak C—H⋯O hydrogen bonds. The most important contributions to the crystal structure are the H⋯H inter­actions (68.8%).

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A new 4-thia­zolidinone derivative has been obtained from the cyclization reaction of 4-methyl-3-thio­semicarbazone and dimethyl acetyl­enedi­carboxyl­ate (DMAD).

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Four mol­ecular salts made from hexa­methyl­ene­tetra­minium and 2-chloro-4-nitro­benzoate have been synthesized and are reported. All four mol­ecular salts show N+—H⋯O hydrogen bonding. This work shows that hmta only protonates once, even in the presence of excess acid.

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The title compounds feature various types of weak inter­molecular inter­actions but their decomposed Hirshfeld fingerprint plots show significant differences.

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The NS4 donor set in Zn[S2CN(i-Pr)CH2CH2OH]2(4,4′-bipyrid­yl).0.5(4,4′-bipyrid­yl), which features monodentate and non-coordinating 4,4′-bipyridyl mol­ecules, is based on a trigonal bipyramid; the cadmium(II) analogue is isostructural.

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A solvent-free microwave-assisted synthesis of the title compound is presented together with its crystal structure which is characterized by the herringbone motif in the packing.

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The title crystal features two Ru3(CO)11 fragments linked by a Ph2P(CH2)6PPh2 bridge, the latter with an all-trans conformation. The mol­ecular packing features C—H⋯O, as well as C≡O⋯π(arene) inter­actions.

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The structure of akuammicine, an alkaloid isolated from the Madagascar periwinkle, was confirmed and its absolute configuration determined.

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In the title compound, both independent mol­ecules possess a very similar proximal conformation, this referring to the juxtaposition of the 4-hy­droxy­phenyl substituent with respect to the syn-related methyl group.

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The title structure consists of a (Z)-N-benzyl­idene-1-phenyl­methanamine oxide and a hydrogen peroxide mol­ecule linked through both O—H groups into a one-dimensional chain structure.

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The crystal structure of this hybrid organic–inorganic material exhibits chains of lead chloride capped by 4-(di­methyl­amino)­pyridinium and di­methyl­ammoium by hydrogen bonding. This creates a one-dimensional zipper-like structure down the a axis.

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The title zwitterion exists in the iminium/phenoxide form. The mol­ecule is twisted around the N—C(benzene) bond with the C=N—C—C torsion angle being 39.42 (8)°. In the crystal, a zigzag supra­molecular chain is sustained by charge-assisted hy­droxy-O—H⋯O(phenoxide) hydrogen bonding.

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The structure of C12H19Br0.30Cl0.70HgN2·C12H19Br0.24Cl0.76HgN2 contains two mol­ecules in the asymmetric unit with each containing a mixed Cl/Br halide site. The two mol­ecules are linked into dimers by a combination of Hg⋯Hg [Hg⋯Hg = 3.6153 (3) Å] and C—H⋯Cl and C—H⋯π inter­actions.

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The title Schiff base mol­ecule displays a trans configurations with respect to the C=N double bond. Inter­molecular N—H⋯O and C —H⋯O hydrogen bonds connect centrosymmetrically related mol­ecules into dimers, forming rings of R_{3}^{3}(11) and R_{2}^{2}(10) graph-set motif stacked along the a axis into a columnar arrangement.

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The title compounds were obtained by deprotonation of 1,2,4-tri­hydroxy­anthra­quinone (purpurin) using sodium hydride followed by reaction with either 1-bromo­propane or 1-bromo­butane. The compounds were characterized by 1H and 13C NMR and the structures determined using single-crystal X-ray diffraction.

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In the crystal of the ternary co-crystalline adduct, the components inter­act through two inter­molecular O—H⋯N hydrogen bonds. The supra­molecular adducts are inter­linked through of halogen bonds and weak non-conventional hydrogen bonds.

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The CoII atom in the title compound is seven-coordinate, being bound to two pyridine N atoms, one amine N atom and four O atoms to form a distorted penta­gonal–bipyramidal environment. Each dipyridyl-type ligand links the CoII atoms into polymeric zigzag chains, which are connected via inter­molecular π–π stacking inter­actions and N/C—H⋯O hydrogen bonds.

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The reaction of cobalt(II) nitrate with bis­(pyridin-3-ylmeth­yl)sulfane ligand, afforded a one-dimensional looped polymeric chain. The CoII cation displays a distorted octa­hedral geometry coordinated by four pyridine N atoms from four individual ligands and two O atoms from two monodentate nitrate anions. Two symmetry-related ligands are connected by two symmetry-related CoII cations, forming a 20-membered cyclic dimer. These cyclic dimers are connected to each other by sharing CoII atoms, forming a looped chain. In the crystal, adjacent looped chains are connected by inter­molecular π–π stacking inter­actions and C—H⋯π and C—H⋯O hydrogen bonds, resulting in the formation of a three-dimensional supra­molecular architecture.

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In the mol­ecule, the CoII cation is N,O,O′,O′′-chelated by a 2,2′-[N-(phenyl­phospho­rylmeth­yl)aza­nedi­yl]di­acetate dianion and coordinated by two 1H-benzo[d][1,2,3]triazole mol­ecules in a slight distorted octa­hedral coordination.

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The title compound crystallizes as an unsymmetrical dinuclear cation bridged by the phen­oxy O atoms with one Cu atom coordinated by a water mol­ecule and the other by a perchlorate anion, thus making both Cu atoms five-coordinate, and with a further perchlorate anion present for charge balance.

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The title compound is a salt containing a protonated endo-3-amino­tropane cage and a novel anionic copper(II) complex, [CuCl3(NO3)(H2O)]2−.

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In the title compound, the 1,2,3-triazoyl ring is flanked by nitro­benzene and benzyl substituents with the dihedral angle of 70.60 (9)° between rings indicating a twisted L-shape for the mol­ecular conformation.

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The synthesis and structural determination of bis­(4,4′-di­ammonio­diphen­yl)sulfone tetra­(nitrate) monohydrate is reported. The crystal structure features N—H⋯O, O—H⋯O and C—H⋯O hydrogen-bonds and π–π inter­actions.

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The 3,5-isomer of the title compound contains two almost planar mol­ecules in the asymmetric unit, whereas the 3,4-isomer contains a single substanti­ally twisted mol­ecule. Both crystal structures feature short S⋯N and S⋯O inter­actions.

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1-(2-Acetyl-11-meth­oxy-5,6-di­hydro­[1,3]dioxolo[4,5-g]pyrrolo­[2,1-a]isoquinolin-1-yl)propan-2-one, the product of a domino reaction between cotarnine chloride and acetyl­acetylene catalysed by copper(I) iodide, was studied by X-ray diffraction.

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The title compound was isolated as a by-product from a reaction incorporating 2,4,6-tri­methyl­benzoic acid under basic conditions.

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The title complex is coordinated by two acetyl­acetonate, one 1H-imidazole, one nitrate and one water ligand. The mol­ecular plane of the imidazole ligand is almost parallel to that of the nitrate anion.

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The title cyano acid forms a honeycomb-like sheet structure, six mol­ecules circumscribing anthracene, with carb­oxy hydrogen-bonded dimers linked by half of the possible R_{2}^{2}(10) CN⋯Br rings.

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The asymmetric unit contains two independent mol­ecules, which exhibit coplanar, mostly sp2-hybridized meth­oxy and di­methyl­amino substituents on their respective aromatic rings, consistent with π-donation into the aromatic systems. The B—H groups exhibit an intra­molecular close contact with a C—H group of the pyridine ring, which may be evidence of electrostatic attraction between the hydridic B—H and the electropositive aromatic C—H.

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In the title compound, the hydro­philic glucose residues lie in the regions zab plane, from which the pyridyl rings project; pyridyl ring stacking parallel to the a axis links adjacent layers.

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The di­cyano­aurate anions bridge the FeII cations to form polymeric chains propagating along the b axis.

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The structure of this new halide-bridged polymer comprises polyanionic zigzag chains of formula [(BiCl5)2−]n running along the c-axis direction. The 1,2,3-benzotriazolium cations are linked between these polymer chains, via the water mol­ecules, giving rise to left- and right-handed helical chains.

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The crystal structure of tetra­iso­butyl­thiuram di­sulfide reveals a −85.81 (1)° C—S—C—S torsion angle and multiple intra- and inter­molecular S⋯C—H close contacts.

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The structure of methyl 5,6-dimeth­oxy-3a,10-dimethyl-1-phenyl-3,3a,8,8a-tetra­hydro-3,8-(epimino­methano)­cyclo­penta­[a]indene-2-carboxyl­ate, the product of unusual thermolysis of aza­cyclic allene under microvawe conditions, was studied by synchrotron X-ray diffraction.

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The solid solutions Na3Zn0.912Cd0.088B5O10 and Na3Zn0.845Mg0.155B5O10 adopt the ortho­rhom­bic form of the parent compound Na3ZnB5O10 where parts of the zinc cations are replaced by cadmium and magnesium cations, respectively.

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The divalent CoII atom is six-coordinated by three N atoms from two symmetrical 5-(pyridin-4-yl)-1H,2′H-3,3′-bi[1,2,4-triazole] (H2pyttz) ligands and three O atoms from three symmetrical 3-carb­oxy­benzoate (Hbdic) ligands, leading to a distorted {CoN3O3} octa­hedral coordination environment. Two CoII cations are linked by four bridging carboxyl­ate groups to generate a dinuclear [Co2(CO2)4] unit.

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The structure of the title copper(I) coordination polymer is reported. One CuI atom is surrounded by three μ3-iodide anions and one S atom, while the other is coordinated by three μ3-iodide ions an O atom. In the crystal, there are inter­molecular C—H⋯I hydrogen bonds and C—H⋯π inter­actions between ligands. The packing generates a two-dimensional brick-wall structure.

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The crystal structure of the title compound consists of discrete octa­hedral complexes that are linked by inter­molecular N—H⋯S hydrogen bonds into a three-dimensional network that contains channels in which the hydrogen-bonded methanol mol­ecules are located.

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In the title compound, the two indole ring systems are approximately perpendicular to one another, subtending a dihedral angle of 86.0 (5)°. In the crystal, pairs of N—H⋯O hydrogen bonds link the mol­ecules into the inversion dimers, which are further linked by N—H⋯O hydrogen bonds into supra­molecular chains propagated along the b-axis direction.

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The structure of title co-crystal consists of a 2,3,5,6-tetra­kis­(pyridin-2-yl)pyrazine coformer and hydrogen peroxide solvent mol­ecules in a ratio of 1:4.75.

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The crystal structure of the dinuclear copper(II) complex with dianionic Schiff base derived from 5-bromo­salicylic aldehyde and cyste­amine prepared by direct synthesis is reported.

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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