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Journal logoSTRUCTURAL
CHEMISTRY
ISSN: 2053-2296

December 2013 issue

Special issue on Interplay of crystallography, spectroscopy and theoretical methods for solving chemical problems

Guest Editors: Larry Falvello (Universidad de Zaragoza, Spain) and Alberto Albinati (Universita degli Studi di Milano, Italy)

Highlighted illustration

Cover illustration: Powder diffraction: what's in a name? See Von Dreele [Acta Cryst. (2013). C69, 1433-1436]. The paper forms part of the special issue on Interplay of crystallography, spectroscopy and theoretical methods for solving chemical problems.

editorial


crystallography, spectroscopy and theory


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The co-deposition method was used for preparation of the mixed-valence supra­molecular compound {[CuI4(O2CCF3)4]2–{μ2-OC(CH3)2}2–[CuII2(O2CCF3)4]}, which consists of copper(I) and copper(II) tri­fluoro­acetate units held together by acetone bridges and inter­molecular Cu⋯O inter­actions.

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Three RuII–hydride species have been synthesized and fully characterized, including X-ray single-crystal structures. Quantum chemical calculations predict very accurately the observed crystallographic data.

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The preparation and structure elucidation of a new tin-rich heterometallic complex [Sn4(hfpt)2–Cu(hfac)2–Sn4(hfpt)2], which consists of a planar [Cu(hfac)2] fragment sandwiched between two tetra­nuclear [Sn4(hfpt)2] units, are reported.

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The development of powder diffraction is briefly described; the extent of this development from studies of metals to protein crystal structures shows that powder diffraction is at the cutting edge of crystallography. A new name `polycrystallography' is proposed for these endeavours.

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NMR diffusion methods continue to attract increasing attention from practising chemists. This short article summarizes some of the more recent developments and highlights the areas in which these methods are finding application.

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The complex (dtbpe-κ2P)NiI2 is close to square planar in the solid state but is neither diamagnetic nor red in colour. Its structure and magnetism have been investigated by a combination of experiment and density functional theory. Comparisons have been made with analogous compounds bearing different halides and different phosphine ligands. Observed trends in structure and colour have been reproduced theoretically and rationalized.

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The analysis of the structures of metastable linkage isomers, generated photochemically, using single-crystal photocrystallographic techniques, is described. The factors that favour the formation of the metastable states are discussed.

inorganic compounds


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Clathrates with the type-I structure are reported in the quaternary Rb–Eu–In–Ge system. Possible cation ordering is suggested.

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The structure of fac-triamminetri­chlorido­rhodium consists of isolated octa­hedra and that of the fac-triammine­trinitratorhodium trigonal complex consists of octa­hedral columns with partially filled rhodium positions.

metal-organic compounds


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The ReI centres of the tri­carbonyl­rhenium(I) complexes of 5-[2-(2,4,6-tri­methyl­phenyl)diazen-1-yl]quinolin-8-olate and 5,7-bis­[2-(2-methyl­phenyl)diazen-1-yl]quinolin-8-olate are facially surrounded by the ligands in a slightly distorted octa­hedral environment. Both structures exhibit inter­molecular C—H⋯O inter­actions.

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The hydrated sodium salt of 4-chloro-3-nitro­benzoic acid and the hydrated sodium and potassium salts of 2-amino-4-nitro­benzoic acid are stabilized by intra- and inter­molecular hydrogen bonding and strong π–π ring inter­actions. Na centres are linked through centrosymmetric four-membered duplex water bridges and through 18-membered duplex head-to-tail ligand bridges. Similar centrosymmetric bridges are found in the potassium salt.

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The coordination polymer [Cu(ptt)]n (ptt is 1-phenyl-1H-1,2,3,4-tetra­zole-5-thiol­ate) has been prepared under solvothermal conditions. Its structure features two-dimensional layers which lie parallel to the (100) plane.

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The crystal structure and NMR data of the title compound are reported. It crystallizes in the space group P\overline{1} with Z′ = 2, the mol­ecules forming infinite chains via hydrogen bonds. The chains inter­act through dispersive aliphatic contacts.

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A metal–organic framework (MOF) is reported in which an AgI cation is coordinated by two N atoms from two different 3,5-diethyl-1,2,4-triazolate ligands in a linear configuration. Each AgI cation is then connected to two adjacent AgI cations via a μ3-N1:N2:N4-triazolate ligand.

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In two complexes, CuI atoms connect the symmetric 2,7-bis­(1H-imidazol-1-yl)-9,9-dimethyl-9H-fluorene and 2,7-bis­(1H-imidazol-1-yl)-9,9-dipropyl-9H-fluorene ligands into one-dimensional chains. In the former, a {[CuICl2]} unit adheres to the one-dimensional chain through a weak Cu⋯Cu inter­action, while in the latter, a {[CuI2Cl4]2−} unit links two different chains into a one-dimensional rope-ladder-type chain.

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The calcium and strontium terahydrate salts of (glycinato)oxidobis(peroxido)vanadate(V) crystallized at pH ca 7.4 with similar lattice parameters. The glycinate anion acts as a bidentate N,O-chelating ligand, and the V atom has a penta­gonal bipyramidal geometry, with two η2-peroxide groups and the glycinate N atom in the equatorial plane, and one terminal oxo and a glycinate O atom at the axial positions.

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In two dinuclear copper complexes, the two CuII ions are bridged by four syn,syn11:μ carboxyl­ate groups, showing a paddle-wheel cage type structure with a square-pyramidal geometry. The three-dimensional supra­molecular metal–organic frameworks of one complex consist of three different R_{2}^{2}(20) and an R_{4}^{4}(36) ring motif, while the other complex simply packs as mol­ecular species.

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Three-dimensional coordination polymers made up of lanthanides, oxydi­acetate and sulfate show novel structures in which the sulfate anion tends to reach saturation as a ligand.

organic compounds


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A polymorphic form of the title indole alkaloid was extracted from Aristotelia chilensis. Its crystal structure is described and compared with a previously reported polymorph.

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The structure of a nitroxide radical determined from laboratory X-ray powder diffraction data is reported for the first time. The attractive forces between the mol­ecules in the crystal structure are mainly of dispersive nature.

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Two tosyl­ate salts of lapatinib, an anti­cancer drug, crystallize in centrosymmetric and noncentrosymmetric space groups. The crystal packing in both structures is influenced by a combination of N—H⋯O hydrogen bonds and C—H⋯O inter­actions

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A tetra­hydro­pyrimidin-4(3H)-one, prepared by mild oxidation of the corresponding hexa­hydro analogue, forms hydrogen-bonded R_{2}^{2}(8) dimers.

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The structures of 4-oxo-N-phenyl-4H-chromene-2-carboxamide and of a new polymorph of 7-meth­oxy-4-oxo-N-p-tolyl-4H-chromene-2-carboxamide and its hemihydrate. The structures have an anti-rotamer conformation about the C—N bond; however, the amide O atom can be either trans- or cis-related to the O atom of the pyran ring.

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The imidazolidin-2-one ring displays a half-chair conformation. N—H⋯O hydrogen bonds connect the mol­ecules to form R_{2}^{2}(8) rings and thence ribbons parallel to the a and b axes. The crystal was merohedrally twinned.

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Two salts obtained from the proton-transfer reactions of benzene-1,2,4,5-tetra­carb­oxy­lic acid (pyromellitic acid, PMA) with 2,2′-bi­imidazole and 4,4′-dimethyl-2,2′-bipyridine form one-dimensional O—H⋯O hydrogen-bonded chain structures extended into two-dimensional supra­molecular layers and sheets via O—H⋯O and N—H⋯O hydrogen bonding.

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In 1,8-dibenzoyl-2,7-di­hydroxy­naphthalene, centrosymmetric dimeric aggregates arise from two intra- and inter­molecular O—H⋯O=C hydrogen bonds, forming head-to-tail square-shaped cyclic ⋯O⋯H⋯O⋯H⋯ hydrogen bonds. These dimeric aggregates are connected into layers in the bc plane by inter­molecular (naphthalene)C—H⋯O=C inter­actions.

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2,2′-Disulfanyl­idene-5,5′-biimidazolidinyl­idene mol­ecules aggregate through N—H⋯S hydrogen-bonding inter­actions with cyclic motifs [graph set R_{2}^{2}(8)], giving two-dimensional ribbon structures which are close to being parallel. Two independent water mol­ecules associate to form centrosymmetric cyclic hydrogen-bonded (H2O)4 tetra­mer units [graph set R_{4}^{4}(8)].

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The crystal packing motifs in two polymorphic modifications (monoclinic and ortho­rhom­bic) of the title salt are different, but the conformations of the anions are generally similar.

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The title compounds are oxidation products of the parent compound 10-ethynyl-10H-pheno­thia­zine and differ with respect to transannular S⋯N inter­actions, the intra­molecular S⋯N contact being shorter in the dioxide.

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Two physalin compounds have been isolated from Congolese Physalis angulata L. plants and their structure and pharmacological activity has been determined. In both structures, physalin dimers are formed by inter­molecular hydrogen bonding.

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The title 1,4-naphtho­quinone is a chlorinated derivative of vitamin K3, which is a synthetic compound also known as menadione. Mol­ecules are planar, lie on a crystallographic mirror plane (Z′ = 0.5) and are connected to each other by C—H⋯O hydrogen bonds, forming two-dimensional layers parallel to the ac plane.

Special and virtual issues

Acta Crystallographica Section C is planning special issues on

The Structural Chemistry of Homogeneous and Heterogeneous Catalysts

NMR Crystallography

Full details are available on the special issues page.

The latest virtual issue, featuring Coordination polymers and with an introduction by Len Barbour, was published in July 2014.

What are the 'most read' articles from the recent special issues?

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