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December 2018 issue
research communications
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The first benzohydrazide complex of a lanthanide is reported. The SmIII ion is nine-coordinated in a distorted tricapped trigonal–prismatic geometry by three oxygen atoms and three nitrogen atoms from three benzhydrazide (bzz) ligands, one oxygen atom from the isophthalate (itp2−) ligand, and two oxygen atoms from coordinated water molecules. The crystal structure features extensive hydrogen bonding as well as C—H⋯π and π–π interactions.
CCDC reference: 1876239
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The closely related title compounds are comprised of three types of rings: thiazolidinone, nitrophenyl and cyclohexyl. In both structures, the rings are close to mutually perpendicular, with interplanar dihedral angles greater than 80° in each case.
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One O atom of the succinate anion and three O atoms and two N atoms from a tetrakis(2-hydroxyethyl)ethylenediamine ligand coordinate to the NiII cation to form the complex which has a distorted octahedral geometry.
CCDC reference: 1564209
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The title compounds were prepared via chemo- and regioselective [3 + 2]-cycloadditions. The thiophene ring in each crystal structure has an envelope conformation. The largest differences between the two molecular structures is in the bond lengths about the quaternary C atom of the thiophene ring. In the spirocyclic structure, the C—C bonds to the spiro C atom in the cyclobutane ring are around 1.60 Å and weak intermolecular C—H⋯X (X = S, O) interactions link the molecules into extended ribbons. In the other structure, weak C—H⋯π interactions link the molecules into sheets.
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The crystal structures of three N′-(arylidene)4-nitrobenzenesulfonohydrazides, namely, (E)-4-nitro-N′-(2-chlorobenzylidene)benzenesulfonohydrazide (I), (E)-4-nitro-N′-(2-methylbenzylidene) benzenesulfonohydrazide (II) and (E)-4-nitro-N′-(4-methylbenzylidene)benzenesulfonohydrazide (III), have been studied to investigate the effect of the nature and site of substitutions on the structural parameters and the supramolecular features in these compounds. Hirshfeld surface analysis was also carried out to examine the contributions of the various atom–atom interactions in the crystal packing of the three compounds.
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The structures are reported of six racemic tris(bipyridyl)iron salts with a range of 2-substituted-1,1,3,3-tetracyanopropenide anions, mostly also containing either perchlorate or tetrafluoridoborate as co-anions. In three of the compounds the polynitrile anions are fully ordered, and in three others they are disordered, while the co-anion is also ordered in three compounds, but disordered in two others. Supramolecular assemblies range from no continuous aggregation up to a three-dimensional hydrogen-bonded framework structure.
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The structures of the hydrogen-bonded 1:1 co-crystal of chloranilic acid with ethyleneurea and the 1:2 co-crystal of chloranilic acid with hydantoin have been determined at 180 K. In the crystals of both compounds, the base molecules are in the lactam form and no acid–base interaction involving H-atom transfer is observed. The acid and base molecules are linked by short O—H⋯O and N—H⋯O hydrogen bonds.
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The title compound crystallizes in monoclinic (space group P21/c) and triclinic (space group Pī) forms from N,N-dimethylformamide and isopropyl alcohol solutions, respectively. The planar structures of the molecules in both crystals are essentially the same as each other, with maximum deviations of 0.0969 (11) and 0.209 (4) Å for the monoclinic and triclinic forms, respectively, from the mean planes of all non-H atoms.
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Three ammonium salts of 2-amino-4-nitrobenzoate are described. Based on N—H⋯O and O—H⋯O hydrogen-bonding involving the different constituents, supramolecular chains, tubes and double-layers are found in their crystals.
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Two polymorphic crystal forms of 6-methyl-N-phenyl-2,3-dihydro-1,4-oxathiine-5-carboxamide) were isolated from a truncated, (12 solvent), polymorph screen on pure lyophillized material. Crystals of form 1 were obtained from all solvents included in the screen with the exception of methanol. As isolated from acetonitrile the crystals are triclinic, space group P with Z′ = 2. Crystals of form 2, which were isolated from methanol only are monoclinic, space group I2/a with Z′ = 1.
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In the title compound, the benzodiazolone moieties are planar to within 0.017 (1) and 0.026 (1) Å, and oriented at a dihedral angle of 57.35 (3)°. In the crystal, two sets of intermolecular C—H⋯O hydrogen bonds generate layers parallel to the bc plane.
CCDC reference: 1875883
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In the binuclear complex, [Cu2(OH)2(C12H7N2(PO3C2H5))2(H2O)2]·7H2O, the two Cu2+ cations each have a square-pyramidal geometry and are bridged by two hydroxide groups. The phenanthroline ligand in this complex acts as a counter-ion due to a negatively charged monoethylphosphoryl group. In the crystal, O—H⋯O hydrogen bonds link the cations, P(O)(O−)(OEt) group and water molecules of crystallization into a three-dimensional supramolecular architecture.
CCDC reference: 1877346
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The new compound (BEDT-TTF)4[Cu(NCS)4] based on the organic donor BEDT-TTF [bis(ethylenedithio)tetrathiafulvalene] has been obtained during a galvanostatic electrocrystallization process with Cu(NCS). It exhibits a pseudo-κ arrangement, never observed up to now in the BEDT-TTF family with thiocyanatocuprate(II) anions.
CCDC reference: 1876009
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The crystal structures of the title compounds have been studied to clarify the characteristics of the NO2− ligand as a C—H⋯O hydrogen-bond acceptor, in relation to the solid-state photochemical linkage isomerization.
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The asymmetric unit of the title co-crystal comprises two twisted molecules of 2,2′-thiodibenzoic acid and four molecules of triphenylphosphane oxide. The three-dimensional molecular packing is stabilized by hydroxy-O—H⋯O(oxide) hydrogen bonds and TPPO-C—H⋯O(oxide, carbonyl) and TDBA-C—H⋯(oxide, carbonyl) interactions.
CCDC reference: 1876525
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Four binary charge-transfer complexes were made using pyromellitic acid dianhydride (pmda), all of which show alternating donor and acceptor stacks, which have weak C—H⋯O hydrogen bonds connecting the donor and acceptor molecules.
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The crystal structure of a second phase, which results from packing polymorphism, is described for a previously reported MnIII complex.
CCDC reference: 1877342
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1-Phenyl-1H-pyrazole-3,4-dicarboxylic acid and 1-(4-methoxyphenyl)-1H-pyrazole-3,4-dicarbohydrazide form complex hydrogen-bonded framework structures each containing multiple hydrogen-bond types, but dimethyl 1-phenyl-1H-pyrazole-3,4-dicarboxylate and dimethyl 1-(4-methylphenyl)-1H-pyrazole-3,4-dicarboxylate form simple cyclic dimers containing only C—H⋯O hydrogen bonds.
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The complex [{La(Ph3CCOO)2(Me3AlOMe)}2] has an La2(μ-OCO)4 core, contains the carboxylate ligands in μ2-κ1O:κ1O′ bridging and μ2-κ2O,O′:κ1O semi-bridging coordination modes, and displays La—C interactions with the π-system of a phenyl ring.
CCDC reference: 1877930
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In the polymeric potassium complex [{iPrN= CHN(iPr)N(NiPr)2K}2(μ-DME)]n, the amidinoguanidinate ligand adopts an unusual mixed σ-/π-coordination mode.
CCDC reference: 1862025
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The title molecule is substantially twisted, with a dihedral angle of 43.70 (2)° between the 2-(methylsulfanyl)thiophene and 4-methoxyphenyl rings. In the crystal, molecules are linked through C—H⋯O interactions, forming a bifurcated layer stacking along the b-axis direction enclosing (10) ring motifs.
CCDC reference: 1871776
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Three compounds consisting of pyridinium or morpholinium hydrogen oxalates each display different hydrogen oxalate hydrogen-bonding motifs, resulting in chains for 4-(dimethylamino)pyridinium hydrogen oxalate 0.22-hydrate, dimers for 4-tert-butylpyridinium hydrogen oxalate and chains for morpholinium hydrogen oxalate.
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The crystal structures of (E)-4-chloro-N′-(4-chlorobenzylidene)benzenesulfonohydrazide and (E)-4-chloro-N′-(4-nitrobenzylidene)benzenesulfonohydrazide have been studied to investigate the effect of substituents on the structural parameters. The two-dimensional fingerprint plots of these two p-substituted compounds indicate that in the 4-chloro-substituted compound, the largest contribution to the Hirshfeld surface comes from the H⋯H contacts (26.6%), in contrast to the 34.8% contribution of the O⋯H/H⋯O contacts in the 4-nitro-substituted compound.
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The title compound is built up from a planar quinoxalinone ring system linked through a methylene bridge to a 1,2,3-triazole ring, which is inclined by 67.09 (4)° to the quinoxalinone ring plane.
CCDC reference: 1878133
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Straight ⋯I—PtIV—I⋯PtII⋯ chains are observed in the mixed-valent title salt. Extensive hydrogen bonding involving the amino groups, hydrogen sulfate counter-anions and water molecules of crystallization stabilizes the crystal packing.
CCDC reference: 1878955
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New Schiff bases containing piperidine and arylsulfonohydrazide moieties have been synthesized, characterized and their crystal structures determined to study the effect of substituents on the structural parameters. Their crystal structures are stabilized by N—H⋯O, C—H⋯O and O—H⋯O interactions. Two-dimensional fingerprint plots show that the largest contributions come from H⋯H interactions.
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The nine-membered ring system of the title compound is essentially planar. In the crystal, molecules are linked via C—HTrz⋯NTrz and C—HPyrm⋯NTrz (Trz = triazole and Pyrm = pyrimidine) hydrogen bonds together with weaker C—HPyrm⋯NPyrm hydrogen bonds to form layers parallel to (02). The layers are further connected by π–π-stacking interactions between the nine-membered ring system, forming oblique stacks along the a-axis direction.
CCDC reference: 1879279
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The binuclear title molecule exhibits point group symmetry 2, with the PdII atom in a square-planar coordination environment defined by two N atoms from ethylenediamine and two O atoms from methylenediphosphonate ligands.
CCDC reference: 1879750
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In the title compound, the benzodiazole unit is planar while the benzyl and propynyl substituents are rotated significantly out of this plane.
CCDC reference: 1879758
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Crystal structure of 4-[(3-methoxy-2-oxidobenzylidene)azaniumyl]benzoic acid methanol monosolvate
In the crystal, the Schiff base molecule exists in the zwitterionic form and an intramolecular N—H⋯O hydrogen bond stabilizes the molecular structure.
CCDC reference: 1879300
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The mefloquinium cation in the title salt is L-shaped as the piperidin-1-ium group is nearly orthogonal to the quinolinyl residue. Supramolecular chains arise in the crystal as a result of charge-assisted O—H⋯O and N—H⋯O hydrogen-bonding.
CCDC reference: 1879700
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The asymmetric unit of the title compound consist of two independent molecules. In the crystal, N–H⋯O and C—H⋯O hydrogen bonds form zigzag chains along the b-axis direction. Additional C—H⋯O hydrogen bonds link the chains into layers parallel to (10). These are connected by slipped π-stacking and C—H⋯π(ring) interactions.
CCDC reference: 1879920
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In the pentanuclear title complex, [SmZn2(C22H18N2O4)2(NCS)2(C3H7NO)2][Zn2(C22H18N2O4)(NCS)3]·C3H7NO·0.32H2O, a dinuclear unit and a trinuclear unit co-exist. In the crystal, the trinuclear cationic units and dinuclear anionic units are assembled into infinite layers.
CCDC reference: 1878960
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The compound, prepared by the NaBH4 reduction of 4,8,9,10-tetrakis(4-fluorophenyl)-1,3-diazaadamantan-6-one in chloroform and ethanol as solvent, crystallizes in the monoclinic space group P21/n with four molecules in the unit cell.
CCDC reference: 1854381
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The molecule of (1) presents a >C(CH3)2 group that bridges two nearly planar salicylaldehyde groups, each comprising a planar phenyl ring bonded with a hydroxyl and an aldehyde group. Similarly, molecule (2) presents the same bridging group, but it connects two nearly planar appendants, each comprising a phenyl ring bonded with a hydroxyl and two aldehyde groups. Compound (2) exhibits a strong visible luminescence when excited with ultraviolet radiation.
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The compound tris(1,1′-dibutyl-4,4′-bipyridine-1,1′-diium) bis(dimethyl sulfoxide)di-μ3-iodido-tetra-μ2-iodido-octaiodidotetralead(II) dimethyl sulfoxide tetrasolvate belongs a class of organic–inorganic hybrid materials with novel functionalities. In this compound, C—H⋯O and C—H⋯I hydrogen-bonding interactions, π–π interactions, other short contacts and Pb octahedral chains are present, extending the crystal structure into a three-dimensional supramolecular network.
CCDC reference: 1880239
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We report herein the synthesis, crystallographic analysis and a study of the non-covalent interactions observed in the new 4′-substituted terpyridine-based derivative bis[4′-(isoquinolin-2-ium-4-yl)-4,2′:6′,4′′-terpyridine-1,1′′-diium] tris-[tetrachloridozincate(II)]. The compound is similar in its formulation to the recently reported 2,2′:6′,2′′ terpyridinium analogue, although rather different and much simpler in its structural features, mainly in the number and type of non-covalent interactions present, as well as in the supramolecular structure they define.
CCDC reference: 1879345
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The molecule has mirror symmetry with the all non-H atoms, except tert-butyl groups, located on the mirror plane. An intramolecular O—H⋯N hydrogen bond forms an S(6) ring motif. In the crystal, the molecules are connected by C—H⋯π interactions
CCDC reference: 1873612
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The title molecular salts are stilbazole, or 4-styrylpyridine, derivatives in which the cation has a methyl group attached to the pyridine ring N atom and a diethyl amine group attached to the benzene ring. In salt (I), the cadmium atom of the [CdI4]2− dianion is located on a twofold rotation axis and the compound crystallizes with one cation in the asymmetric unit. In salt(II), the anion consists of a 4-methoxybenzenesulfonate ion, and it crystallizes as a monohydrate.
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In the title bimetallic metal–organic framework, {Fe(Brpz)2[Cu(CN)2]2}n, where Brpz is 2-bromopyrazine, the FeII cation is located on an inversion centre and has a slightly elongated octahedral FeN6 coordination environment. The CuI center has a fourfold CuC3N coordination environment with an almost perfect trigonal–pyramidal geometry. Copper(I) centers related by a twofold rotation axis are bridged by two carbon atoms from a pair of μ-CN groups, resulting in Cu2(CN)2 units that build up the coordination framework.
CCDC reference: 1880717
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In the crystal structure of the title compound, the MnII cations are octahedrally coordinated by two terminally N-bonded thiocyanate anions and four 4-benzoylpyridine coligands into discrete complexes, which are further linked into chains by intermolecular C—H⋯O hydrogen bonding.
CCDC reference: 1879856
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The dihydrate and hydrate forms of the DNA-binding bis-benzimidazole radioprotector methylproamine are reported. These are the first single-crystal structures of bis-benzimidazoles related to Hoechst 33342 to be reported.
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The crystal structure of the title compound has been studied to show that the macrocyclic cyclam ligand is very suitable as the co-ligand for the nitro–nitrito photo-isomerization of the CoIII complex.
CCDC reference: 1881114
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In the title imidazo[1,2-a]pyridine derivatives, N-tert-butyl-2-(4-methoxyphenyl)-5-methylimidazo[1,2-a]pyridin-3-amine, (I), and N-tert-butyl-2-[4-(dimethylamino)phenyl]imidazo[1,2-a]pyridin-3-amine, (II), the 4-methoxyphenyl ring in (I) and the 4-(dimethylamino)phenyl ring in (II) are inclined to the mean planes of the respective imidazole rings by 26.69 (9) and 31.35 (10)°.
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The title heterocyclic 1,3,4-oxadiazole derivatives differ from each other in the groups attached to the carbon atoms: a methoxyphenyl ring and a benzonitrile group in (I) and a chlorophenyl ring and an acetamide group in (II).
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The paper reports the crystal structure of novel salt of 4-aminobenzoic acid (Vitamin B10) with pyrazinoic acid.