Acta Crystallographica Section C

Crystal Structure Communications

Volume 69, Part 11 (November 2013)


Special issue on Pharmaceuticals, drug discovery and natural products

Guest Editor: Professor Christopher S. Frampton (Pharmorphix, Cambridge, England)

[Buy print version] A printed copy of this issue is available for purchase


[Issue Author Index][Volume Author Index]
[Cover illustration] Cover illustration: The structure of carbamazepine tri­fluoro­acetic acid monosol­vate overlaid on its difference Fourier map [see Eberlin, Eddleston & Frampton (2013). Acta Cryst. C69, 1260-1266]. The paper forms part of the special issue on Pharmaceuticals, drug discovery and natural products.

editorial


 

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Acta Cryst. (2013). C69, 1205-1206  [ doi:10.1107/S0108270113027960 ]

An introduction to the special issue on pharmaceuticals, drug discovery and natural products

C. S. Frampton

Synopsis: An overview of current topics of interest in the field of solid-state pharmaceuticals and an introduction to papers featured in this special issue.

Online 31 October 2013


pharmaceuticals, drug discovery and natural products


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Acta Cryst. (2013). C69, 1207-1211  [ doi:10.1107/S010827011302492X ]

Structural assignment of a bis-cyclo­pentenyl-[beta]-cyano­hydrin formed via alkene metathesis from either a triene or a tetra­ene precursor

K. G. Andrews, C. S. Frampton and A. C. Spivey

Synopsis: Density functional theory (DFT) NMR prediction, 1H-1H Total Correlated Spectroscopy (TOCSY) NMR and single-crystal X-ray crystallography were used to confirm the formation of a bis-cyclo­pentenyl-[beta]-cyano­hydrin in preference to a 2,3,6,7-de­hydro­deca­lin-[beta]-cyano­hydrin as the kinetic product upon subjecting tri- and tetra­ene substrates to Ru-catalyzed alkene metathesis.

Formula: C11H13NO

Online 9 October 2013


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Acta Cryst. (2013). C69, 1212-1216  [ doi:10.1107/S0108270113018842 ]

Absolute configuration of naturally occurring glabridin

C. Simmler, F. R. Fronczek, G. F. Pauli and B. D. Santarsiero

Synopsis: Glabridin is a species-specific biomarker from the roots Glycyrrhiza glabra L. (European licorice, Fabaceae). Stereochemical analysis, including circular dichroism, NMR data and an X-ray diffraction data set with Bijvoet differences, confirms that glabridin, purified from its natural source, is found only in a C3 R configuration.

Formula: C20H20O4

Online 9 October 2013


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Acta Cryst. (2013). C69, 1217-1220  [ doi:10.1107/S0108270113025936 ]

A new polymorph of N-(6-methyl­pyridin-2-yl)mesityl­ene­sulfon­amide

F. Pan and U. Englert

Synopsis: A new polymorph of the pharmaceutically active sulfa­pyridine derivative N-(6-methyl­pyridin-2-yl)mesityl­ene­sulfon­amide was obtained as a phase-pure product from methanol. The mol­ecules adopt the conformation which is predicted for an individual mol­ecule by force field calculations.

Formula: C15H18N2O2S

Online 19 October 2013


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Acta Cryst. (2013). C69, 1221-1224  [ doi:10.1107/S0108270113025948 ]

Bis[4-amino-N-(pyrimidin-2-yl)benzene­sulfonamido]­diamminecopper(II): aqua or ammine ligands?

F. Pan, I. Kalf and U. Englert

Synopsis: High-resolution diffraction data support our interpretation that the title compound is coordinated by two ammine rather than by an ammine and an aqua ligand.

Formula: [Cu(C10H9N4O2S)2(NH3)2] and [Cu(C10H9N4O2S)2(NH3)2]

Online 19 October 2013


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Acta Cryst. (2013). C69, 1225-1228  [ doi:10.1107/S010827011302595X ]

Preparation and structural analysis of (±)-threo-ritalinic acid

S. Wyss, I. A. Werner, W. B. Schweizer, S. M. Ametamey and S. Milicevic Sephton

Synopsis: The preparation, single-crystal X-ray structure and solution-state NMR analysis of (±)-threo-ritalinic acid, obtained from the hydrolysis of the methyl ester (±)-threo-methyl phenidate, are reported.

Formula: C13H17NO2

Online 19 October 2013


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Acta Cryst. (2013). C69, 1229-1233  [ doi:10.1107/S0108270113026863 ]

Structures of cefradine dihydrate and cefaclor dihydrate from DFT-D calculations

J. van de Streek, J. Rantanen and A. D. Bond

Synopsis: The isostructural crystal structures of cefradine dihydrate and cefaclor dihydrate, based on experimental data where available and supplemented with dispersion-corrected density functional theory calculations, are presented. The crystal structures are typical examples of isolated-site hydrates.

Formula: C16H19N3O4S·2H2O and C15H14ClN3O4S·2H2O

Online 19 October 2013


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Acta Cryst. (2013). C69, 1234-1237  [ doi:10.1107/S0108270113025961 ]

Enantio­tropically related polymorphs of gaboxadol hydro­chloride

H. Lopez de Diego, V. Koradia and A. D. Bond

Synopsis: Gaboxadol hydrochloride (also known as THIP hydrochloride) undergoes a reversible single-crystal-to-single-crystal transformation at 221 K. Crystal structures have been determined at 298 and 220 K.

Formula: C6H9N2O2+·Cl- at two different temperatures

Online 19 October 2013


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Acta Cryst. (2013). C69, 1238-1242  [ doi:10.1107/S0108270113025924 ]

Crystal structure and packing energy calculations of (+)-6-amino­penicillanic acid

S. Saouane, G. Buth and F. P. A. Fabbiani

Synopsis: (+)-6-Amino­penicillanic acid, a precursor of a variety of semi-synthetic penicillins, represents an ordered zwitterion and the crystals are nonmerohedrally twinned. The complementary analysis of the crystal packing by the PIXEL method brings to light the nature and ranking of the energetically most stabilizing inter­molecular inter­action energies.

Formula: C8H12N2O3S

Online 24 October 2013


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Acta Cryst. (2013). C69, 1243-1250  [ doi:10.1107/S0108270113028126 ]

Structural and docking studies of potent e­thio­namide boosters

N. J. Tatum, B. Villemagne, N. Willand, B. Deprez, J. W. Liebeschuetz, A. R. Baulard and E. Pohl

Synopsis: This report illustrates the crystal structures of three new inhibitors targeting the mycobacterial regulator EthR which has previously been identified as a novel target for tuberculosis drug boosters. In addition, we describe how the results of our structure determination were used to develop a docking protocol using GOLD for future in silico screening.

Formula: C14H14N4O2S, C19H19F3N4O3S and C19H22F3N3O4S

Online 24 October 2013


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Acta Cryst. (2013). C69, 1251-1259  [ doi:10.1107/S0108270113028643 ]

The principles underlying the use of powder diffraction data in solving pharmaceutical crystal structures

K. Shankland, M. J. Spillman, E. A. Kabova, D. S. Edgeley and N. Shankland

Synopsis: Solving pharmaceutical crystal structures from powder diffraction data is discussed in terms of both the various methodologies that have been applied and the complexity of the structures that have been solved.

Online 31 October 2013


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Acta Cryst. (2013). C69, 1260-1266  [ doi:10.1107/S010827011302859X ]

Methane­sulfonic acid salt forms of carbamazepine and 10,11-di­hydro­carbamazepine

A. R. Eberlin, M. D. Eddleston and C. S. Frampton

Synopsis: Methane­sulfonic acid salt forms of carbamazepine and 10,11-di­hydro­carbamazepine have been prepared and characterized by a number of analytical techniques, including single-crystal X-ray diffraction at 100 K. The structural data for these complexes were analysed in relation to data derived from other carbamazepine complexes and a redetermination of the apparently anomalous tri­fluoro­acetic acid solvate structure was undertaken.

Formula: C15H13N2O+·CH3O3S-, C15H15N2O+·CH3SO3- and C15H12N2O·CF3COOH

Online 31 October 2013


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Acta Cryst. (2013). C69, 1267-1272  [ doi:10.1107/S0108270113029545 ]

A 1:2 cocrystal of genistein with isonicotinamide: crystal structure and Hirshfeld surface analysis

M. Sowa, K. Slepokura and E. Matczak-Jon

Synopsis: The mol­ecules in the title cocrystal are present in their neutral forms, and assemble a mol­ecular layer by means of hydrogen bonding. Differences in the environments of the isonicotinamide molecules were assessed by Hirshfeld surface analysis.

Formula: C15H10O5·2C6H6N2O

Online 31 October 2013


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Acta Cryst. (2013). C69, 1273-1278  [ doi:10.1107/S0108270113029363 ]

A complementary experimental and computational study of loxapine succinate and its monohydrate

R. M. Bhardwaj, B. F. Johnston, I. D. H. Oswald and A. J. Florence

Synopsis: The structure determination of loxapine succinate and its monohydrate is presented. Fixed cell geometry optimization using density functional theory in CASTEP was used as a complementary tool to locate the H-atom positions in the crystal structure determined from X-ray powder diffraction data.

Formula: C18H19ClN3O+·C4H5O4- and 2C18H19ClN3O+·C4H4O42-·C4H6O4·2H2O

Online 31 October 2013


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Acta Cryst. (2013). C69, 1279-1288  [ doi:10.1107/S0108270113029533 ]

Utilizing proton transfer to produce mol­ecular salts in bromanilic acid substituted-pyridine mol­ecular complexes - predictable synthons?

L. H. Thomas, M. S. Adam, A. O'Neill and C. C. Wilson

Synopsis: Proton transfer systematically producing mol­ecular salts is used in a study of nine mol­ecular complexes of bromanilic acid with methyl­pyridines, which show predictable synthons related to the stoichiometry and a common N-H...O charge-assisted hydrogen bond.

Online 31 October 2013


inorganic compounds


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Acta Cryst. (2013). C69, 1289-1291  [ doi:10.1107/S0108270113027145 ]

MYb(BH4)4 (M = K, Na) from laboratory X-ray powder data

W. Wegner, T. Jaron and W. Grochala

Synopsis: The title compounds were prepared via a mechano­chemical reaction in the solid state. They crystallize in the NaSc(BH4)4 structure type composed of isolated [Yb(BH4)4]- anions, with Yb coordinated tetra­hedrally by BH4 groups, surrounded by M+ cations (M = Na, K) which form distorted trigonal prisms.

Formula: KYb(BH4)4 and NaYb(BH4)4

Online 19 October 2013


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Acta Cryst. (2013). C69, 1292-1300  [ doi:10.1107/S0108270113028138 ]

Crystal structures of hydrates of simple inorganic salts. I. Water-rich magnesium halide hydrates MgCl2·8H2O, MgCl2·12H2O, MgBr2·6H2O, MgBr2·9H2O, MgI2·8H2O and MgI2·9H2O

E. Hennings, H. Schmidt and W. Voigt

Synopsis: Crystals of MgCl2·8H2O, MgCl2·12H2O, MgBr2·6H2O, MgBr2·9H2O, MgI2·8H2O and MgI2·9H2O were grown from their aqueous solutions at temperatures below 298 K according to the solid-liquid phase diagrams. All structures are built up from Mg(H2O)6 octa­hedra. Dimensions and angles in the hexa­aqua cation complexes are very similar and variation is not systematic.

Formula: MgCl2·8H2O, MgCl2·12H2O, MgBr2·6H2O, MgBr2·9H2O, MgI2·8H2O and MgI2·9H2O

Online 31 October 2013


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Acta Cryst. (2013). C69, 1301-1303  [ doi:10.1107/S010827011302862X ]

The double molybdate Na9Sc(MoO4)6 refined from powder XRD data

A. A. Savina, V. A. Morozov, O. M. Basovich, E. G. Khaikina and B. I. Lazoryak

Synopsis: Rietveld refinement of Na9Sc(MoO4)6 shows that its structure is made up of clusters formed from an ScO6 octa­hedron and three Na1O6 octa­hedra sharing total edges. The clusters are connected by sharing vertices with bridging MoO4 tetra­hedra, forming a three-dimensional framework.

Formula: Na9Sc(MoO4)6

Online 31 October 2013


metal-organic compounds


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Acta Cryst. (2013). C69, 1304-1306  [ doi:10.1107/S0108270113026267 ]

The organic-inorganic hybrid material 1-cyclo­hexyl­piperazine-1,4-diium tetra­chlorido­zincate

S. Soudani, E. Aubert, C. Jelsch and C. Ben Nasr

Synopsis: In the title organic-inorganic hybrid material, the tetra­chlorido­zincate anions and 1-cyclo­hexyl­piperazine-1,4-diium dications are inter­connected via N-H...Cl and C-H...Cl hydrogen bonds to form layers parallel to the (001) plane. The cyclo­hexyl groups are located between these layers to form an infinite three-dimensional network.

Formula: (C10H22N2)[ZnCl4]

Online 5 October 2013


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Acta Cryst. (2013). C69, 1307-1310  [ doi:10.1107/S010827011302475X ]

A one-dimensional coordination polymer created via in situ ligand synthesis involving C-N bond formation

H. Cai, Y. Guo and J.-G. Li

Synopsis: A novel cadmium complex consists of one-dimensional ladders constructed from [Cd2(COO)2] dimeric subunits. A combination of hydrogen bonding and [pi]-[pi] stacking inter­actions extend the one-dimensional ladders into a three-dimensional supra­molecular architecture.

Formula: [Cd(C12H9N3O4)]

Online 5 October 2013


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Acta Cryst. (2013). C69, 1311-1313  [ doi:10.1107/S0108270113025377 ]

A two-dimensional network con­taining an -Mn-O-C-O-Mn- chain: poly[diaqua[1,2-bis(pyridin-4-yl)ethylene][[mu]3-3-carboxy-5-(carboxylatomethoxy)benzoato]manganese(II)]

Y.-Q. Lei and G.-H. Wang

Synopsis: The title compound is a two-dimensional network containing an -Mn-O-C-O-Mn- chain. Each layer presents a herringbone pattern and interacts with neighbouring layers through intermolecular hydrogen bonds.

Formula: [Mn(C10H6O7)(C12H10N2)(H2O)2]

Online 5 October 2013


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Acta Cryst. (2013). C69, 1314-1316  [ doi:10.1107/S0108270113025614 ]

The purine-carboxylate-containing coordination polymer poly[[[mu]4-1-(2-carboxyl­ato­ethyl)-6-oxo-6,9-di­hydro-1H-purin-9-ido]zinc(II)]

W.-J. Ma and G.-T. Li

Synopsis: A three-dimensional metallohelicate is constructed from one-dimensional metal-organic helices of purine-containing 3-(6-oxo-6,9-di­hydro-1H-purin-1-yl)propionate ligands and zinc(II) ions.

Formula: [Zn(C8H6N4O3)]

Online 5 October 2013


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Acta Cryst. (2013). C69, 1317-1321  [ doi:10.1107/S0108270113025973 ]

3,4-Dihy­droxy-1,6-bis­(4-meth­oxy­phen­yl)hexa-2,4-diene-1,6-dione, its 4-methyl­phenyl analogue, and a potassium salt of 2-hy­droxy-4-(4-meth­oxy­phen­yl)-4-oxobut-2-enoic acid

L. Nye, M. M. Turnbull and J. L. Wikaira

Synopsis: 3,4-Dihy­droxy-1,6-bis­(4-meth­oxy­phenyl)hexa-2,4-diene-1,6-dione exhibits the di-enol-dione tautomeric form and is compared with its 4-methyl­phenyl analogue. In a potassium salt of 2-hy­droxy-4-(4-meth­oxy­phenyl)-4-oxobut-2-enoic acid, the organic species are linked by a strong hydrogen bond between the carb­oxy­lic acid and carboxyl­ate groups.

Formula: C20H18O6, C20H18O4 and [K(C11H9O5)(C11H10O5)]

Online 9 October 2013


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Acta Cryst. (2013). C69, 1322-1327  [ doi:10.1107/S0108270113026450 ]

Two sodium(I) coordination polymers constructed by the V-shaped ligands 2,2'-[iso­propyl­idene­bis(1,4-phenyl­ene­oxy)]di­acetic acid and 2,2'-[sulfonyl­bis­(1,4-phenyl­ene­oxy)]di­acetic acid

Q.-Y. Huang, C.-L. Liu and Z.-P. Zhou

Synopsis: Two novel inorganic-organic coordination polymers, based on NaI cations with semi-rigid V-shaped di­carboxyl­ate ligands, have been prepared and structurally characterized.

Formula: [Na2(C19H19O6)2] and [Na4(C16H14O8)2(H2O)8]

Online 9 October 2013


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Acta Cryst. (2013). C69, 1328-1331  [ doi:10.1107/S0108270113027182 ]

A fivefold inter­penetrating diamondoid framework constructed by flexible dipyridyl and di­carboxyl­ate ligands

J.-F. Wang, W.-J. Guo and F.-Z. Deng

Synopsis: In a novel three-dimensional CdII complex prepared by hydro­thermal assembly of Cd(NO3)2·4H2O, 1,4-bis­[2-(pyridin-4-yl)ethenyl]benzene and 2,2'-(1,4-phenyl­ene)di­acetic acid, each CdII centre is located in a distorted penta­gonal bipyramidal coordination environment. The three-dimensional net can be regarded as a diamondoid network by treating the CdII atoms as nodes and the benzene and di­acetic acid ligands as linkers.

Formula: [Cd(C10H8O4)(C20H16N2)(H2O)]

Online 9 October 2013


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Acta Cryst. (2013). C69, 1332-1335  [ doi:10.1107/S010827011302711X ]

Synthesis, crystal structure and fluorescence spectrum of a cadmium(II) sulfaquinoxaline complex

X.-H. Zhao, Y.-Y. Zhao, J. Zhang, J.-G. Pan and X. Li

Synopsis: A one-dimensional polymeric structure of CdII with sulfaquinoxaline is further stabilized by inter­molecular hydrogen bonding. The fluorescence spectrum reveals that the complex emits strong blue fluorescence. The thermal analysis shows that the framework is stable up to 663 K.

Formula: [Cd(C14H11N4O2S)2(H2O)]

Online 9 October 2013


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Acta Cryst. (2013). C69, 1336-1339  [ doi:10.1107/S0108270113027194 ]

Enantio­tropic phase transition in a binuclear tin complex with an O,N,O'-tridentate ligand

A. Schwarzer, L. E. H. Paul and U. Böhme

Synopsis: A dinuclear tin(IV) complex of 2-[(2-oxido­benzyl­idene)amino]­ethanolate is disordered above 178 K. The crystal structure at 93 K contains two ordered mol­ecules. The phase transition corresponds to an order-disorder transition of a vinyl group bound to the SnIV atom.

Formula: [Sn2(C2H3)3(C9H9NO2)2Cl] at 93 and 273 K

Online 12 October 2013


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Acta Cryst. (2013). C69, 1340-1343  [ doi:10.1107/S0108270113026292 ]

A novel one-dimensional tubular cadmium(II) coordination polymer based on 5-(carboxyl­atometh­oxy)benzene-1,3-di­carboxyl­ate containing 4-amino­pyridinium ions

P. Wang, Y. Zhao, Y. Chen and X.-Y. Kou

Synopsis: A novel anionic tubular CdII coordination polymer based on the 5-(carboxyl­atometh­oxy)benzene-1,3-di­carboxyl­ate ligand and containing 4-amino­pyridinium cations had been synthesized under hydro­thermal conditions. In the solid state, the 4-amino­pyridinium cation props up the structure through hydrogen bonds to the O-atom acceptors of ligands and solvent water mol­ecules.

Formula: (C5H7N2)[Cd(C10H5O7)(H2O)2]·2H2O

Online 12 October 2013


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Acta Cryst. (2013). C69, 1344-1347  [ doi:10.1107/S0108270113026620 ]

The layered structure of poly[[hexa­aqua­([mu]4-benzene-1,2,4,5-tetra­car­box­yl­ato)dicopper(II)] tetra­hydrate]

P. Cancino, E. Spodine, V. Paredes-García, D. Venegas-Yazigi and A. Vega

Synopsis: The layered polymeric structure of a benzene-1,2,4,5-tetra­carboxyl­ate-Cu complex forms parallelogram-shaped channels.

Formula: [Cu2(C10H2O8)(H2O)6]·4H2O

Online 12 October 2013


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Acta Cryst. (2013). C69, 1348-1350  [ doi:10.1107/S0108270113027212 ]

Different ZnII cation coordination geometries in di-[mu]-acetato-bis­{2-chloro-6-[(pyridine-2-yl­methyl­imino)­methyl]phenol}dizinc(II) chloro­form monosolvate

Y.-I. Kim, J. Y. Lee, Y.-K. Song and S. K. Kang

Synopsis: In a dinuclear zinc(II) complex of acetate and 6-chloro-2-{(E)-[(pyridin-2-yl)methyl­imino]­methyl}phenolate, the ZnII cations differ in their five-coordinate geometries, with one adopting a distorted trigonal bipyramidal geometry and the other a square-pyramidal geometry.

Formula: [Zn2(C13H10ClN2O)2(C2H3O2)2]·CHCl3

Online 12 October 2013


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Acta Cryst. (2013). C69, 1351-1356  [ doi:10.1107/S0108270113027108 ]

Multiple anion...[pi] inter­actions in tris­(1,10-phenanthroline-[kappa]2N,N')iron(II) bis­[1,1,3,3-tetra­cyano-2-(2-hydroxy­ethyl)propenide] mono­hydrate

Z. Setifi, K. V. Domasevitch, F. Setifi, P. Mach, S. W. Ng, V. Petrícek and M. Dusek

Synopsis: Double nitrile...[pi] interactions are relevant for the crystal packing of charge-diffuse conjugated tetracyanopropenide anions when combined with common heteroaromatic tris-chelate octahedral complexes, [Fe(phen)3]2-.

Formula: [Fe(C12H8N2)3](C9H5N4O2)2·H2O

Online 12 October 2013


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Acta Cryst. (2013). C69, 1357-1361  [ doi:10.1107/S0108270113027091 ]

Low-dimensional compounds containing cyanide groups. XXVI. (Dicyanamido-[kappa]N1)bis­(5,5'-dimethyl-2,2'-bi­pyridine-[kappa]2N,N')copper(II) complexes with tetra­fluoro­borate and perchlorate anions

I. Potocnák, M. Burcák and M. Dusek

Synopsis: The Cu atoms in the title complexes are five-coordinated in distorted trigonal bipyramidal environments by four N atoms of two 5,5'-dimethyl-2,2'-bi­pyridine ligands and one N atom of a dicyanamide anion, which is coordinated in a monodentate manner in the equatorial plane. The structures are stabilized by C-H...N and C-H...X hydrogen bonds (X = F and O) and [pi]-[pi] inter­actions between pyridine rings.

Formula: [Cu(C2N3)(C12H12N2)2]BF4 and [Cu(C2N3)(C12H12N2)2]ClO4

Online 12 October 2013


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Acta Cryst. (2013). C69, 1362-1366  [ doi:10.1107/S0108270113027996 ]

A well-resolved cyclic water tetra­mer in a dinuclear CuII coordination complex based on 1,2-bis­(pyridin-3-yl­oxy)ethane and capped by pyridine-2,6-di­carb­oxy­lic acid

J.-Y. Ge, P. Wang, J.-P. Ma, Q.-K. Liu and Y.-B. Dong

Synopsis: Two five-coordinated aqua­copper(II) centres chelated to pyridine-2,6-di­carboxyl­ate terminal ligands are bridged by a 1,2-bis­(pyridin-3-yl­oxy)ethane spacer. The structure includes a well-resolved cyclic water tetra­mer, which acts as a subunit to form a larger aggregate.

Formula: [Cu2(C7H3NO4)2(C12H12N2O2)(H2O)2]·4H2O

Online 24 October 2013


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Acta Cryst. (2013). C69, 1367-1372  [ doi:10.1107/S010827011302845X ]

Bis(4-methyl­anilinium) and bis­(4-iodo­anilinium) penta­molybdates from laboratory X-ray powder data and total energy minimization

M. Oszajca, L. Smrcok and W. Lasocha

Synopsis: The crystal structures of bis­(4-methyl­anilinium) and bis­(4-iodo­anilinium) penta­molybdates were determined using laboratory X-ray data and refined by total energy minimization methods. The obtained structures present alternating organic cation and inorganic polyanion layers bound by weak bonding (apart from ionic inter­actions).

Formula: (C7H10N)2[Mo5O16] and (C6H7IN)2[Mo5O16]

Online 31 October 2013


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Acta Cryst. (2013). C69, 1373-1377  [ doi:10.1107/S0108270113027984 ]

A novel one-dimensional copper(II) coordination polymer and a trinuclear nickel(II) complex with a one-dimensional hydrogen-bonded structure

X.-H. Chen, S.-Y. Chen, C.-L. Xie and Q.-J. Wu

Synopsis: A novel infinite one-dimensional coordination polymer involving N'-(2-hy­droxy­benzyl­idene)-2-(naphthalen-2-yl­oxy)aceto­hydrazide, and a trinuclear nickel complex of 2-hy­droxy-N'-(2-oxo-2-phen­oxy­ethyl)benzo­hydrazide with a one-dimensional network structure constructed by hydrogen-bonding inter­actions, are reported.

Formula: [Cu(C19H14N2O3)]·C3H7NO·H2O and C15H11N2O4)2(C3H4N2)2(H2O)2]·4C3H7NO

Online 31 October 2013


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Acta Cryst. (2013). C69, 1378-1382  [ doi:10.1107/S0108270113027881 ]

A dense hydrogen-bonding network and an unusually large packing index in tri­aqua­tris­(2,4-dioxo-1,2,3,4-tetra­hydro­pyrimidine-5-carboxyl­ato)neodymium(III) trihydrate

A. M. Atria, M. T. Garland and R. Baggio

Synopsis: In a mononuclear NdIII complex, three chelating 2,4-dioxo-1,2,3,4-tetra­hydro­pyrimidine-5-carboxyl­ate ligands and three aqua ligands build up a distorted monocapped square anti­prism around the cation. A complex hydrogen-bonding network results in a densely packed structure (packing index = 77.7%)

Formula: [Nd(C5H3N2O3)3(H2O)3]·3H2O

Online 31 October 2013


organic compounds


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Acta Cryst. (2013). C69, 1383-1389  [ doi:10.1107/S0108270113025869 ]

A series of N-(2-phenyl­ethyl)nitro­aniline derivatives as precursors for slow and sustained nitric oxide release agents

C. B. Wade, D. K. Mohanty, P. J. Squattrito, N. J. Amato and K. Kirschbaum

Synopsis: A series of N-(2-phenyl­ethyl)nitro­aniline derivatives is presented, demonstrating that modest changes in the functional groups cause significant differences in mol­ecular conformation, inter­molecular inter­actions and packing.

Formula: C14H13N3O4, C22H22N4O4, C15H13N3O2 and C15H16N2O4S

Online 5 October 2013


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Acta Cryst. (2013). C69, 1390-1396  [ doi:10.1107/S010827011302581X ]

Supra­molecular architectures of N-acetyl-L-proline monohydrate and N-benzyl-L-proline

P. Rajalakshmi, N. Srinivasan, R. V. Krishnakumar, I. A. Razak and M. M. Rosli

Synopsis: Proline (Pro) exists in its neutral form in N-acetyl-L-proline monohydrate and is zwitterionic in N-benzyl-L-proline. The presence of a water molecule in the neutral form and the difference in the ionization states between the two forms have effected significant changes in the respective intermolecular schemes.

Formula: C7H11NO3·H2O and C12H15NO2

Online 5 October 2013


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Acta Cryst. (2013). C69, 1397-1401  [ doi:10.1107/S0108270113025341 ]

N-[2-(Pyridin-2-yl)ethyl]-derivatives of methane-, benzene- and toluenesulfonamide: prospective ligands for metal coordination

D. L. Jacobs, B. C. Chan and A. R. O'Connor

Synopsis: Three N-[2-(pyridin-2-yl)ethyl]-substituted sulfonamides are almost structurally identical, the most dramatic different being seen for the N-C-C-C torsion angle with the introduction of a methyl group in the para position of the sulfonamide moiety. These compounds are prospective ligands for the formation of new metal complexes.

Formula: C8H12N2O2S, C13H14N2O2S and C14H16N2O2S

Online 5 October 2013


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Acta Cryst. (2013). C69, 1402-1407  [ doi:10.1107/S0108270113028874 ]

Three new pseudopolymorphs of 6-amino­uracil

V. Gerhardt and M. Bolte

Synopsis: The structures of two 6-amino­uracil di­methyl­acetamide monosolvates and a 1-methyl­pyrrolidin-2-one monosolvate display N-H...O hydrogen-bonding patterns that link the uracil mol­ecules to their respective solvent mol­ecules. The formation of R_{2}^{2}(8) N-H...O hydrogen-bond motifs between 6-amino­uracil mol­ecules can only be found in two-dimensional frameworks, whereas R_{3}^{3}(14) N-H...O patterns are present when zigzag chains of 6-amino­uracil mol­ecules are formed.

Formula: C4H5N3O2·C4H9NO, C4H5N3O2·C4H9NO and C4H5N3O2·C5H9NO

Online 31 October 2013


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Acta Cryst. (2013). C69, 1408-1410  [ doi:10.1107/S0108270113028631 ]

The glycogen phospho­rylase inhibitor 2-(3-benzyl­amino-2-oxo-1,2-di­hydro­pyridin-1-yl)-N-(3,4-di­chloro­benz­yl)acetamide

I. Popova, P. C. Healy, W. A. Loughlin, N. D. Karis and I. D. Jenkins

Synopsis: The crystal structure of a potent glycogen phospho­rylase a (GPa) inhibitor (IC50 of 6.3 µM) consists of four distinct conjugated [pi] systems separated by rotatable bonds around the Csp3 atoms. The mol­ecules are linked into dimers disposed about a crystallographic centre of symmetry through a cyclic N-H...O hydrogen-bonding motif.

Formula: C21H19Cl2N3O2

Online 31 October 2013


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Acta Cryst. (2013). C69, 1411-1413  [ doi:10.1107/S0108270113028461 ]

Absolute configuration determination of the anti-head-to-head photo­cyclo­dimer of anthracene-2-carb­oxy­lic acid through cocrystallization with L-prolinol

Y. Kawanami, H. Tanaka, J. Mizoguchi, N. Kanehisa, G. Fukuhara, M. Nishijima, T. Mori and Y. Inoue

Synopsis: The absolute configuration of the enantio­pure anti-head-to-head cyclo­dimer of anthracene-2-carb­oxy­lic acid was determined. The dimer inter­acts with L-prolinol through a nine-membered hydrogen-bonded ring [R_{2}^{2}(9)], while a di­chloro­methane mol­ecule is incorporated to fill the void space.

Formula: C5H12NO+·C30H19O4-·CH2Cl2

Online 31 October 2013


addenda and errata


 

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Acta Cryst. (2013). C69, 1414  [ doi:10.1107/S010827011302756X ]

A hydrogen-bonded ribbon in 6-amino-3-methyl-5-nitroso-2-(pyrrol­idin-1-yl)pyrimidin-4(3H)-one monohydrate and hydrogen-bonded sheets in 6-amino-2-dimethyl­amino-3-methyl-5-nitroso­pyrimidin-4(3H)-one monohydrate. Corrigendum

F. Orozco, B. Insuasty, J. Cobo and C. Glidewell

Synopsis: Corrigendum to Acta Cryst. (2009), C65, o549-o552.

Formula: C9H13N5O2·H2O and C7H11N5O2·H2O

Online 31 October 2013


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