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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

February 2018 issue

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Cover illustration: Crystal engineering, the conception and synthesis of molecular solid-state structures, is fundamentally based upon the discernment and subsequent exploitation of intermolecular interactions, to obtain new solid forms with tailored properties. One of the many possible applications is the stabilization of explosive materials by co-crystallization. In the present paper, the authors have synthesized four new charge-transfer co-crystals of the shock- and heat-sensitive trinitrobenzene (TNB) with various polycyclic aromatic hydrocarbons and studied the weak interactions stabilizing their crystal structures. See: Hill, Levendis & Lemmerer [Acta Cryst. (2018). E74, 113-118].

research communications


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In the compound [Lu(C7H7)3(C4H8O)2], the Lu ion is coordinated by three benzyl and two tetra­hydro­furan ligands. Two of the benzyl groups are bonded in a classical η1-fashion through the methyl­ene via the ipso-carbon atom of the benzyl ligand in addition to bonding through the methyl­ene C atom, resulting in a modified trigonal–bipyramidal coordination geometry about the Lu center.

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A new organic perchlorate, C7H10N+·ClO4, was synthesized by slow evaporation at room temperature and its crystal structure was determined. This compound was characterized by powder XRD, IR, and UV–Vis spectroscopy. The DFT optimized structure at the B3LYP/6–311++G (d,p) level was compared with the experimentally determined mol­ecular structure in the solid state. Hirshfeld surface and fingerprint plots are presented and discussed.

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The title crystals are isomorphous, and form centrically stacked planar sheets formed by CN⋯I and NC⋯I short contacts.

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The treatment of non-fully substituted 4,4-di­fluoro-4-bora-3a,4a-di­aza-s-indacene (BODIPY) with cupric nitrate leads to the introduction of a nitro group at different positions of the BODIPY core, depending on the substitution pattern. This methodology complements the treatment of fully substituted BODIPY with cupric nitrate that was previously reported. In all three structures, the fused ring system is in a very flattened `V-shape' and the central six-membered ring adopts a flattened sofa conformation.

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KNaCuP2O7 is a member of the diphosphate family and crystallizes isotypically with α-Na2CuP2O7. The structure exhibits nearly eclipsed diphosphate units, distorted CuO5 square-pyramids, and distorted NaO7 and KO9 polyhedra as the main building units.

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Three binary and one ternary charge-transfer complexes have been made using 1,3,5-tri­nitro­benzene, all of which show alternating donor and acceptor stacks, which have weak C—H⋯O hydrogen bonds perpendicular to the stacking axis. The final complex is a crystal engineering attempt to modify the packing of the stacks by inserting a third mol­ecule into the structure; this third mol­ecule features strong hydrogen bonds between the carb­oxy­lic acid group of the donor mol­ecule and the pyridine acceptor mol­ecule.

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The mol­ecule of the title Schiff base, has an E conformation with respect to the C=N bond, and a dihedral angle of 14.54 (11)° between the benzene ring and the mean plane of the N—N—C(N)=S hydrazinecarbo­thio­amide unit.

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The di­hydro­pyrimidine ring adopts a twist-boat conformation while the quinone ring is slightly non-planar. In the crystal, mol­ecules are linked by weak C—H⋯O and C—H⋯S hydrogen bonds and C—H⋯π inter­actions. In addition, a short inter­molecular S⋯N contact occurs.

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The monoclinic unit contains a rare acyclic keto tautomer of the amino sugar involved in the extensive hydrogen-bonding patterns. The acyclic conformation is a minor species in the compound's solution.

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The asymmetric unit of the title compound contains two independent mol­ecules with very similar conformations. Each mol­ecule is built up from a ferrocene unit substituted in the 1 and 1′ positions by a protected sulfur di­phenyl­phosphine and by a di­methyl­hydrazine fragment.

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The N atom of morpholine was coupled to the 2-carbon atom of pyrazine in a PdII/phosphatri­aza­adamantyl butane saltone-catalysed reaction and crystallized from the eluent (EtOAc–hexa­ne) after chromatography. In the crystal, the mol­ecules form sheets parallel to the b axis, which are supported by non-classical hydrogen-bonding inter­actions between C—H functionalities and the O atom of morpholine and the 4-N atom of pyrazine, respectively.

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The crystal structures of the title compounds consists of discrete octa­hedral (Co) or tetra­hedral (Zn) complexes that are linked by inter­molecular hydrogen-bonding inter­actions into three-dimensional networks.

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Here we report the chemical synthesis and crystal structure of a new hybrid chloro-cadmium coordination polymer based on 4-amino-4H-1,2,4 triazole solved by single-crystal X-ray diffraction. With an unusual architecture, the crystal structure exhibits two distorted octa­hedral coordinations of CdII joined by edge sharing. The first is composed by four chlorine and two N atoms from the triazole ligands. The second is formed by five Cl atoms and by one N atom from the triazole ligand.

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The title thio­semicarbazone compound features tetra­hedrally coordinated ZnII atoms within N2S2 donor sets because of the presence of chelating thio­semicarbazone anions. Supra­molecular chains are found in the crystal owing to the formation of thio­amide-N—H⋯S(thione) hydrogen bonds and eight-membered thio­amide {⋯HNCS}2 synthons.

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The title coordination polymer was obtained by combining an aqueous solution of copper(II) dichloride with the ligand {tert-butyl­meth­yl[4-(6-{[4-(pyridin-2-yl-)1H-1,2,3-triazol-1-yl]meth­yl}-1,3-benzo­thia­zol-2-yl)phen­yl]carbamate in aceto­nitrile.

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A new polymorph of [Sn(C6H5)3Cl(C2H6OS)] has been characterized, which crystallizes in space group P21 with Z′ = 2, while the previously reported phase was in space group P212121 with Z′ = 1.

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2,3,8,9,14,15-Hexamethyl- and 2,3,8,9,14,15-hexa­phenyl-5,6,11,12,17,18-hexa­zatri­naphthyl­ene (HATNMe6 and HATNPh6) are derivatives of hexa­aza­tri­naphthyl­ene (HATN). In the crystal structures of the two compounds, pronounced π–π stacking dominates the packing.

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The title Schiff base compound crystallizes in the zwitterionic form. The resulting iminium and hydroxyl groups are linked by a charge-assisted intra­molecular N+—H⋯O hydrogen bond, and the conformation about the C=N bond is E.

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In the title compound, two thio­sulfate ions coordinate to the zinc(II) ion through the terminal S atoms. The tetra­hedral coordination around the ZnII ion is completed by the ligation of two N atoms of two piperazinium ions. In the crystal, a network of N—H⋯O and O—H⋯O hydrogen bonds leads to the formation of a three-dimensional supra­molecular structure.

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A palladium(II) complex containing a bis­(selenium) ligand based on cyclo­diphosph(V)azane, cis-[(tBuNH)(Se)P(μ-NtBu)2P(Se)(NHtBu)] has been synthesized and structurally characterized. The crystal structure revels chelation of ligand through selenium donors with a natural bite-angle of 110.54 (1)°

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The mol­ecule in the title compound has the shape of the letter L. In the crystal, weak 4-tolyl-C—H⋯π(C6-ring of indole) and S—O⋯π(1,3-dioxole) contacts link the mol­ecules into a supra­molecular layer in the ab plane.

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The crystal structure of 2-(5-bromo­thio­phen-2-yl)aceto­nitrile, previously reported as a liquid, has short centrosymmetric Type I Br⋯Br halogen inter­actions.

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In the title compound, the imine C=N bond is essentially coplanar with the ketone C=O bond in an s-trans conformation. In the crystal, mol­ecules are connected into chains along the c axis through C—H⋯O hydrogen bonds, with two adjacent chains hinged by C—H⋯O hydrogen bonds.

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Crystal structure, packing, and FTIR characterization of 5,5′-di­hydroxy­methyl-3,3′-biisoxazole and 4,4′,5,5′-tetra­hydroxy­methyl-3,3′-biisoxazole are reported.

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The asymmetric unit of the title mol­ecular salt, consists of half a 4-amino­benzenaminium cation and a half a 5-carb­oxy­penta­noate anion. Each ion lies about an inversion centre, the other half being generated by inversion symmetry. In the crystal, charge-assisted O—H⋯O, N—H⋯O and N—H⋯N hydrogen bonds together lead to the formation of a three-dimensional supra­molecular framework.

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Two new organic–inorganic hybrid compounds have been synthesized from the same starting materials. Their crystal structures exhibits alternating inorganic and organic stacking sheets or layers in (II), with Cl ions and water mol­ecules occupying the space in between.

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Two new crystal structures of eight- and ten-membered cyclic bis­anisyl­phosphono­thioyl disulfanes have been determined and these are compared to the structures of their ferrocenyl analogues.

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In the complex cation, the CoII atom, located on an inverse centre, is coordinated by two isonicotinamide and four water mol­ecules in a distorted O4N2 octa­hedral geometry. The fumarate anion is located on another inverse centre and is linked to neighbouring complex cations via O—H⋯O and O—H⋯N hydrogen bonds and weak C—H⋯O hydrogen bonds. In the crystal, the complex cations are further linked by O—H⋯O, N—H⋯O an weak C—H⋯O hydrogen bonds, forming a three-dimensional supra­molecular architectecture.

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The title compound has monoclinic (P21/n) symmetry with a single Al atom in the asymmetric unit. The complex possesses catalytic activity in the ring-opening polymerization of ∊-caprolactone.

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The title compound crystallizes with half a mol­ecule in the asymmetric unit and shows Car—H⋯F inter­actions in the crystal packing.

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The title complex has two kinds of ligands, tri­fluoro­acetyl­acetonate and water. As a result of the presence of F atoms in the 1,1,1-tri­fluoro-4-oxo­pentan-2-olate ligand, the metal–metal distance is longer than in the case of the analogous yttrium complex containing an acetyl­acetonato ligand and also for the analogous lanthanum complex containing acetyl­acetonate.

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A novel heterometallic CuI–NiII coordination polymer with an infinite one-dimensional structure was prepared and structurally characterized via X-ray diffraction. This complex consists of a mononuclear nickel(II) unit of NiII(C6H10NS2)2 and a penta­nuclear copper(I) cluster unit of Cu5I5(CH3CH2CN).

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Two new salts – 2,6-di­amino-4-chloro­pyrimidin-1-ium 5-chloro­salicylate and bis­(2,6-di­amino-4-chloro­pyrimidin-1-ium) naphthalene-1,5-di­sulfonate – have been synthesized and characterized by single-crystal X-ray diffraction. The supra­molecular inter­actions such as hydrogen bonding, halogen bonding, C—Cl⋯π and π–π inter­actions are investigated for these crystal structures.

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In comparison with the known polymorph of KEu(SO4)2·H2O (monoclinic, P21/c), the new polymorph crystallizes in the trigonal crystal system (space group P3121).

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The CdII cation, located on a twofold rotation axis, is coordinated by two 2,4,6-tri­methyl­benzoate anions, two nicotinamide ligands and a water mol­ecule in a distorted penta­gonal–bipyramidal geometry.

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The mol­ecular and crystal structure of a new mononuclear neutral high-spin iron(III) complex with two different tridentate ligands has been studied by an X-ray diffraction analysis.

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The title mol­ecule is twisted, with the dihedral angles between the imine core (C3N) and thio­urea and methyl­pyridyl residues being 20.25 (8) and 7.60 (9)°, respectively. In the crystal, corrugated supra­molecular layers in the bc plane are mediated by amine-N—H⋯N(pyrid­yl) and thio­amide-N—H⋯S(thione) hydrogen bonds.

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The title mol­ecule has a approximately coplanar relationship between the methyl­idenehydrazinecarbodi­thio­ate (C2N2S2) core and substituted pyridyl ring but the former plane is nearly orthogonal to the thio­ester phenyl ring. Supra­molecular layers in the bc plane sustained by C—H⋯S and C—H⋯π inter­actions feature in the crystal.

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The title compound, trimeth­yl(tetra­hydro­furan-κO)aluminium(III), is an addition product of tri­methyl­aluminium and tetra­hydro­furan (THF). Instead of a dimeric structure, which is very common for these types of compounds, a monomeric mol­ecular structure is observed.

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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