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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

March 2020 issue

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Cover illustration: Tetra­aza­macro­cycles are useful in a variety of applications, in particular in the elimination of toxic metals. The N-substituted tetraazamacrocyle discussed in this contribution (1,4,8,11-tetra­methyl-1,4,8,11-tetra­azonia­cyclo­tetra­decane) is a tetracation resulting from the reaction of 1,4,8,11-tetra­methyl-1,4,8,11-tetra­aza­cyclo­tetra­decane (TMC, C14H32N4) with sodium perchlorate/chromium trioxide in HCl. The structure determination by synchrotron radiation indicated that this tetra-protonated amine displays a distorted trans-IV conformation, one of the five possible conformations of the macrocyclic cation. The structure is characterized by an intricate and extensive network of N-H...Cl and C-H...Cl hydrogen bonds, which link the two Cl- anions to the C14H36N44+ cation, while C-H...O hydrogen bonds inter­connect neighboring cations with the perchlorate anions. See: Moon & Choi [Acta Cryst. (2020). E71, 324-327].

research communications


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The key inter­actions in the extended structure of the title solvate are O—H⋯O hydrogen bonds, which generate [010] chains.

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The crystal structure of the title heterocyclic amine was determined in the presence of water. The compound co-crystallizes with three water mol­ecules in the asymmetric unit, which leads to the formation of hydrogen bonding in the crystal.

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The title compound belongs to the class of neutral pyridine aroylhydrazone complexes. In the crystal, π–π stacking leads to dimerization of the complex mol­ecules, which, in turn, are connected by weak C⋯O and C⋯C inter­actions, thus giving rise to a supra­molecular layered architecture.

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The replacement of ZnII with MnII ions in the hybrid structure, which also changed the space group from ortho­rhom­bic Pbca with Z = 8 to monoclinic P21/c with Z = 4, quenched the fluorescence emission of the hybrid material.

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The title compound, [Ni(tren)(H2O)2][Ni(H2O)6](SO4)2, consists of two octa­hedral nickel complexes within the same unit cell. It co-precipitates with the starting material, [Ni(H2O)6](SO4). The crystals of the title compound are purple, different from the [Ni(H2O)6](SO4) crystals, which are turquoise.

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High steric constraints lead to inter­locking tri­methyl­silyl and tertbutyl (or isoprop­yl) substituents in the structures of three silyl-protected phenol and anilene reagents. The two di-tert-butyl compounds are distorted from planarity to mild boat conformations but the diiso­propyl­anilene remains rigorously planar.

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In the title salt, [C14H36N4]4+·2ClO4·2Cl, the macrocyclic cations lie about an inversion center. In the crystal, N–H⋯Cl, C–H⋯Cl and C–H⋯O hydrogen bonds connect the cations and anions, forming a three-dimensional network.

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The thallium(I) atom in the polymeric title compound is bonded to four O atoms, with the lone pair electrons stereochemically active.

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On reaction of the new pyrazine dicarboxamide ligand, N2,N3-bis­(quinolin-8-yl)pyrazine-2,3-dicarboxamide, with Cu(ClO4)2 in aceto­nitrile a binuclear copper complex was formed. Both copper atoms are CuN5 coordinate, and while one copper atom has a perfect square-pyramidal coordination sphere the other has a distorted shape.

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Three huntite-type aluminoborates of stoichiometry REAl3(BO3)4 (RE = Tb, Dy and Ho) were synthesized by slow cooling within a K2Mo3O10 flux with spontaneous crystallization. The synthesized borates are isostructural to the huntite [CaMg(CO3)4] structure and crystallized within the trigonal R32 space group.

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Two different mol­ecules with point group symmetry 2 are present in the crystal structure of the title compound. Each independent mol­ecule forms chains parallel to the b axis with its symmetry-related counterparts through C—H⋯π(ring) inter­actions.

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The first metal–organic framework (MOF) formed from lithium(I) and γ-cyclo­dextrin is reported. The structure is characterized by an unusually low metal/ligand ratio.

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In the title polymer, the eightfold-coordinated SrII atoms are linked by bridging (H2BTEC)2– anions to generate a two-dimensional network Thermal analysis (TG–SDTA–MS) has been undertaken.

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1,3-Disubstituted chalcones have been converted into 3,5-disubstituted 4,5-di­hydro­pyrazole-1-carbo­thio­amides by reaction with thio­semicarbazide. Two isomorphous chalcone precursors form hydrogen-bonded sheets, while in two isomorphous reduced pyrazole products, hydrogen-bonded chains of rings are formed: in a third product, the mol­ecules are linked into complex sheets.

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In the crystal, edge-sharing [CuO5] trigonal bipyramids form dimers that are linked to PO4 tetra­hedra via a common edge. The obtained [Cu2P2O12] units are inter­connected through vertices to form sheets that are sandwiched between undulating layers resulting from the junction of PO4 tetra­hedra and [InO6] octa­hedra. The two types of layers are alternately stacked along [101] and are joined into a three-dimensional framework through vertex- and edge-sharing, leaving channels parallel to the stacking direction in which the Na+ ions are located.

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The title mol­ecule is only a few degrees out of planarity except for the 2-hy­droxy­ethyl substituent. In the crystal, O—H⋯N hydrogen bonds form stepped chains along the c-axis direction, which are formed into layers parallel to the bc plane by weak C—H⋯O and C—H⋯π (ring) inter­actions. Completion of the overall layer structure occurs through weak C—H⋯O, C—H⋯π (ring) and head-to-tail slipped π-stacking inter­actions.

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The dihedral angles between the mean plane of the piperidine ring, which adopts a chair conformation, and the phenyl rings are 89.72 (8) and 48.32 (8)°. In the crystal, mol­ecules are linked into chains along the b-axis direction by C—H⋯O hydrogen bonds.

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In the title CuII complex, a newly synthesized dye, the metal atom is coordinated by two N atoms and two O atoms from two bidentate (E)-1-[(2,4,6-tri­bromo­phen­yl)diazen­yl]naphthalen-2-olate ligands.

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The title conjugated carbazole chalcone compound, synthesized using a Claisen–Schmidt condensation reaction, adopts an s-cis conformation with respect to the ethyl­enic double bonds (C=O and C=C).

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The structures of four phospho­rescent monoiridium and chloro-, cyanato- or oxamidato-bridged diiridium complexes with a potential for OLED applications are described.

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The title compound is a pure diastereoisomer built up from a central five-membered di­hydro­isoxazole ring substituted in the 3 and 5 positions by a p-chloro­phenyl group and a cyclo­hex-2-enone ring. The cyclo­hex-2-one and the isoxazoline rings both exhibit an envelope conformation. The crystal packing features C—H⋯O, C—H⋯N and C—H⋯π inter­actions.

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The crystal structures of two new tetra­kis-substituted pyrazine compounds, 1,1′,1′′,1′′′-(pyrazine-2,3,5,6-tetra­yl)tetra­kis­(N,N-di­methyl­methanamine) and N,N′,N′′,N′′′-[pyrazine-2,3,5,6tetra­yltetra­kis­(methyl­ene)]tetra­kis­(N-methyl­aniline), and a degredation product, N,N′-[(6-phenyl-6,7-di­hydro-5H-pyrrolo­[3,4-b]pyrazine-2,3-di­yl)bis­(methyl­ene)]bis­(N-methyl­aniline), are described and have been analysed by Hirshfeld surface analysis.

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In the cadmium(II) and zinc(II) complexes of the tetra­kis-substituted pyrazine ligand, N,N′,N′′,N′′′-[pyrazine-2,3,5,6-tetra­yltetra­kis­(methyl­ene)]tetra­kis­(N-methyl­aniline), the ligand coordinates in a mono-tridentate fashion, and both metal atoms have fivefold coordination spheres with distorted shapes.

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In the solid state the title compound shows full-mol­ecule disorder (occupancy ratio 0.65: 0.35), generated by a twofold rotation about the shorter axis of the mol­ecule.

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A new title heterometallic Cu/Ca complex, [Cu(C8H8NO2)2Ca(NCS)2(H2O)], with a Schiff base ligand derived from o-vanillin and ammonia has been synthesized by a facile one-pot reaction under ambient conditions. In the crystal, O—H⋯S hydrogen bonds between the coordinating water mol­ecules and thio­cyanate groups form a supra­molecular chain with a zigzag-shaped calcium skeleton.

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In the crystal, the cations and anions of the title salt are linked via N—H⋯Br hydrogen bonds. In the 1H NMR spectra of this compound, the NH iminium protons were observed at δ 10.35 p.p.m., which confirms the strong charge-assisted hydrogen bonding (CAHB) in the =HN+—HBr synthon.

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The mol­ecules of the two title polymorphs mainly differ in the orientation of the carb­oxy­lic OH group that results in different packing features.

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Two new co-crystals of tetra­iodo­ethyl­ene with two aza­phenanthrenes were successfully synthesized. In the crystals, C—I⋯π and C—I⋯N halogen bonds link the mol­ecules. A study of their luminescence properties indicates that co-crystals 1 and 2 exhibit distinctly different luminescence in the solid state at room temperature.

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In the title compound, the dihedral angle between the fused pyrazole and pyridine rings is 3.81 (9)°. The benzene ring forms dihedral angles of 35.08 (10) and 36.26 (9)° with the pyrazole and pyridine rings, respectively. In the crystal, weak C—H⋯O hydrogen bonds connect mol­ecules along [100].

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The title coordination polymers show different degrees of deprotonation of the disiloxane-di­carboxyl­ate bridging ligands: both contain tetra­gonally distorted trans-NiN4O2 octa­hedra.

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The crystal structure of a pyrrolidine-substituted p-toluene­sulfonamide is described. The crystal structure features both intra- and inter­molecular C—H⋯O hydrogen bonds, as well as inter­molecular C—H⋯π and π–π inter­actions, leading to the formation of sheets parallel to the ac plane.

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In the crystal structure of the title compound, the MnII cations are sixfold coordinated by four N atoms of a cyclen ligand and two terminal S atoms of an [S4]2− anion into discrete complexes that are connected via inter­molecular N—H⋯S hydrogen bonding into a three-dimensional network.

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The crystal structure of 4-allyl-2-meth­oxy-6-nitro­phenol, which crystallizes in the centrosymmetric space group P\overline{1} with three independent mol­ecules in the asymmetric unit, is reported along with the Hirshfeld surface analysis.

addenda and errata


Research communications

Research communications are designed to help authors bring out the science behind their structure determinations. Authors are encouraged to report more than one structure in the same communication and also to include the results of investigations with other techniques. The Research communications format makes Acta E the natural home for structure determinations with interesting science to report.

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