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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

August 2017 issue

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Cover illustration: The drug Premarin, isolated from pregnant mares' urine, is used for hormone replacement therapy. Three important components of Premarin are the estrogenic steroids Equilinin, Equilin and 17[beta]-estrone. This report describes the molecular and crystal structure of Equilinin, compares it to the known structures of Equilin and 17[beta]-estrone, and relates the differences in conformation to differences in oestrogenic activity. See: Frampton & MacNicol [Acta Cryst. (2017). E73, 1223-1226].

research communications


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The title compound, [Cu(dppaS2)(PPh3)2], is a neutral mononuclear copper(I) complex bearing an N,N-bis­(di­phenyl­phospho­rothio­yl)amidate (dppaS2) ligand and two tri­phenyl­phosphane ligands. The structure of this complex was obtained by X-ray diffraction and supported by DFT calculations.

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The characteristic feature in the crystal structure of the title salt is the formation of a columnar chain structure in the cation comprising mixed-valent ⋯Br—PtIV—Br⋯PtII⋯ entities.

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The structure of a trinuclear manganese Schiff base complex with an Mn3O core is reported with the stoichiometry, C45H42Cl3Mn3N6O7, ClO4, C4H10O, CH2Cl2.

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The title compound, tetra­hydro­seselin (THS), a hydrogenated product of the angular pyran­ocoumarin seselin, possesses photo-biological activity against different kinds of inflammatory skin diseases such as atopic dermatitis and pigment disorders like vitiligo and psoriasis.

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The Tb3+ ion is nine-coordinated in a distorted tricapped trigonal-prismatic geometry by the three N atoms of the tridentate 1-(pyridin-2-yl­methyl­idene)-2-(pyridin-2-yl)hydrazine ligand, four carboxyl­ate O atoms of two chelating acetate groups and two O atoms of the coordinated water mol­ecules. In the crystal, the complex cations are linked by pairs of O—H⋯O hydrogen bonds into dimers. These dimers, nitrate anions and non-coordinating water mol­ecules are joined by O—H⋯O and N—H⋯O hydrogen bonds into a three-dimensional structure.

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The syntheses and crystal structures of two 2,3-di­ethyl­naphtho­quinoxaline-6-11-dione derivatives are described. Mol­ecules of C20H16N2O4 (II) are near planar and form stacks down the c axis through π–π ring inter­actions. In the substituted derivative, C30H34N4O2 (IV), the polycyclic cores have a significant twist and only minor inter­molecular C—H⋯O hydrogen-bonding inter­actions are present.

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The synthesis and crystal structure of 7-hy­droxy-3-(2-meth­oxy­phen­yl)-2-tri­fluoro­meth­yl-4H-chromen-4-one, C17H11F3O4, are reported. This isoflavone is used as a starting material in the preparation an array of potent and competitive FPR antagonists.

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The syntheses and crystal structures of two novel adamantane-substituted N-Mannich bases are reported herein. In the crystals of both compounds, there are C—H⋯F hydrogen bonds present, forming inversion dimers in one and chains in the other.

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The synthesis, characterization and structural analysis of triphenylphosphoniummethylenetrifluoroborate are presented.

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1-(2-Hy­droxy­benz­yl)-2-(2-hy­droxy­phen­yl)-1H-benzimidazol-3-ium chloride, C20H17N2O2+·Cl, is prepared by reaction of salicyl­aldehyde with o-phenyl­enedi­amine in the presence of tri­methyl­silyl chloride acting as a source of HCl. As a result of steric hindrance, the cation in the crystal is far from planar: the benzimidazole ring system makes dihedral angles of 55.49 (9) and 81.36 (8)° with the planes of the phenolic groups. The crystal packing is dominated by the O—H⋯Cl and N—H⋯Cl hydrogen bonds. The title compound exhibits two transitions in the UV region, which are revealed in the solid state and solution spectra as an absorption maximum at 280 nm and a shoulder at 320 nm. According to the results of TD–DFT calculation, both transitions have a π–π* nature and the mol­ecular orbitals involved in these transitions are mostly localized on the benzimidazole ring system and on the phenyl ring attached to it at the 2-position.

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The synthesis and crystal structure of palladium(II) complex, cis-[{ArN=C(Me)-(Et)C=NAr}PdCl2] (Ar = 2,6-iPr2C6H3), containing unsymmetrical α-di­imine ligand, is reported.

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The title isonicotinohydrazide derivative is planar, with an r.m.s. deviation for the fitted non-H atoms of 0.062 Å, and an intra­molecular O—H⋯N hydrogen bond with an S(6) ring motif. In the crystal, mol­ecules are linked by N—H⋯N and C—H⋯N hydrogen bonds forming chains propagating along the a-axis direction.

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The new chromone–thia­zole hybrid presented here is a candidate as a selective ligand for adenosine receptors. Its structure shows packing polymorphism: the two polymorphs (one with space group P21/n and one with P21/c) show slightly different conformations and the major change induced by crystallization regards the intra­molecular contacts defining the supra­molecular structure.


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The synthesis and structural determination of a nickel(II) complex where the two nickel cations in the asymmetric unit each are coordinated by two tridentate, potentially redox non-innocent bis-imino­pyridyl ligands are reported.

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The ethynyl­pyrimidine moiety displays an almost planar geometry. In the crystal, mol­ecules are linked by O—H⋯N and C—Hpyrimidine⋯O hydrogen bonds, forming a three-dimensional supra­molecular architecture.

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tert-Butyl (5-chloro­penta-2,4-diyn-1-yl)carbamate and tert-butyl (5-iodo­penta-2,4-diyn-1-yl)carbamate are new members of the isostructural family of compounds with the general formula BocNHCH2CCCCX (X = H, Cl, Br, I). In the crystals of all these di­acetyl­enes, mol­ecules are linked via a bifurcated N—H⋯O hydrogen bond and C—X⋯O halogen bond involving the same carbonyl group.

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The title compound was prepared from an equimolar mixuture of o-phenyl­enedi­amine and pyrene-1-carboxaldehyde. We report herein on its crystal structure and a density functional theory (DFT) study.

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The structure of 2-tert-butyl-2,3-di­hydro-1H-benzo[c]pyrrol-1-one is compared with those of the related compounds (3R*,1′S*,3′R*)-3-(1′-tert-butyl­amino-1′H,3′H-benzo[c]furan-3′-yl)-2-tert-butyl-2,3-di­hydro-1H-benzo[c]pyrrol-1-one and 2-isopropyl-2,3-di­hydro-1H-benzo[c]pyrrol-1-one, with special attention paid to the planarity of the substituted pyrrole rings in these structures.

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The crystal structure of the sulfoxide of 2,3-diphenyl-2,3-di­hydro-4H-1,3-benzo­thia­zin-4-one, which belongs to a bioactive family of compounds, exhibits a screw-boat pucker for the thia­zine ring. C—H⋯O hydrogen-bond and van der Waals inter­actions stabilize the crystal lattice.

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Crystal structures of the title hydrogen-bonded compounds have been determined at 98 K. In each crystal, the acid and base mol­ecules are linked by short O—H⋯N/N—H⋯O hydrogen bonds, forming a linear hydrogen-bonded 2:1 or 1:2 unit of the acid and the base.

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In the title compound, C—H⋯O hydrogen bonds and aromatic π–π stacking combine to generate a three-dimensional network. A Hirshfeld surface analysis is presented.

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[Mo(tfd)2(ox)]2− as tetra-n-butyl­ammonium salt [co-crystal with oxalic acid and chloro­form; tfd is S2C2(CF3)2 and ox is C2O4] and [(tfd)2Mo(μ-ox)Mo(tfd)2]2− as tetra-n-butyl­ammonium salt.

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A synthetic approach to the new zinc complex based on amino­methyl­ene derivative of 1-phenyl-3-methyl-4-[(quinolyl-3-yl)imino­meth­yl]-1H-pyrazol-5(4H)-one and its structural characterization by synchrotron single-crystal X-ray diffraction are reported.

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The ortho-amino groups of the title compound, C5H6ClN3, twist out of the plane of the mol­ecule to minimize intra­molecular inter­action between them. The amino groups and the pyridine N atom engage in inter­molecular hydrogen bonding. The mol­ecules pack into spiral hydrogen-bonded columns with offset face-to-face π-stacking.

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In the title compound, the epoxide O atom and the 4-meth­oxy­phenyl group lie on opposite sides of the pyrrolidyl ring, whereas the ethyl ester is approximately planar. Linear supra­molecular chains sustained by methine-C—H⋯O(carbon­yl) inter­actions are evident in the mol­ecular packing.

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The structure of the estrone related steroid, Equilenin 1, has been determined at 100 K. It is of great inter­est to investigate what the structural and conformational consequences are on the C and D rings of the steroid framework of 1 by having fully unsaturated A and B rings.

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The title compounds are constructed from a benzo­furan ring and an ortho-substituted phenyl ring connected by a carbonyl-connecting bridge. The structural conformation of the compounds are under substantial influence of steric repulsion. In the crystals, the mol­ecules are connected by C—H⋯O hydrogen bonds and π–π inter­actions [with extra C—H⋯π inter­action for compound (II)].

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Mol­ecules (I) and (II) are nearly planar, while mol­ecule (III) is not planar. In compounds (I) and (II), mol­ecules are linked into chain by C—H⋯π inter­actions. In compound (III), mol­ecules are linked by a pair of C—H⋯O hydrogen bonds, forming inversion dimers. Weak C—Br⋯π inter­actions are present in (III).

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In the title NiII complex, the divalent Ni ion occupies a crystallographically imposed centre of symmetry and is coordinated by two O atoms from the carboxyl­ate groups of two 2,4,6-tri­methyl­benzoate ligands, two N atoms from the pyridyl groups of two isonicotinamide ligands and two water mol­ecules in a slightly distorted octa­hedral geometry. Hirshfeld surface analysis indicates that the most important contributions for the crystal packing are from H⋯H (59.8%), O⋯H/H⋯O (20.2%) and C⋯H/H⋯C (13.7%) inter­actions.

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X-ray structure analysis of hy­droxy–cineole, derived from the biotransformation of cineole, was undertaken to unambiguously determine the location and stereochemistry of the hydroxyl functionality. In the solid state, weak intra­molecular O—H⋯O hydrogen bonding is present, causing the mol­ecules to arrange in spiral chains.

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The ZnII atoms in {Zn[S2CN(R)CH2CH2OH]2(pyridine)·pyridine}, for R = Me (I) and Et (II), are coordinated non-symmetrically by two di­thio­carbamate ligands and by a pyridine ligand, resulting in an NS4 donor set that defines a distorted geometry in each case; the non-coordinating pyridine mol­ecules are connected with the Zn-containing mol­ecules via O—H⋯N(pyridine) hydrogen bonds. The mol­ecular packing features significant (hy­droxy)O—H⋯O(hy­droxy) hydrogen bonding, in each case leading to supra­molecular chains with zigzag (I) or helical (II) arrangements.

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The title compound consists of a cyclo­triphosphazene core and six 4-meth­oxy­carbonyl­phen­oxy groups. The phospho­rus atoms are attached to two substituents located up and down with respect to the plane of the phosphazene ring, the central P3N3 ring having a twisted-boat conformation.

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The crystal structure determination based on 90 K data of the title imine ligand revealed non-merohedral twinning with three twin domains. In our experience, this is an indication of an ordering phase transition. Consequently, the structure was redetermined with higher temperature data, and a reversible phase transition was discovered.

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Reaction of BI3 with carbodi­phospho­rane, C(PPh3)2, gives a mixture of the dicationic compounds, [Ph3PCH2PPh3]I2·2CH2Cl2 and [Ph3PCH2PPh3](BI4)2. Solvents are the source of the protons at the ylidic C atom.

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The title compound, epalerstat acetone monosolvate, is isotypic with the previously reported tetra­hydro­furan solvate.

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The P=O bond in the crystal structure of (3,5-dimethyl-1H-pyrrol-2-yl)di­phenyl­phosphine oxide is not elongated despite its involvement in N—H⋯O=P hydrogen bonding.

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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