world news N'-(2-Hydroxy-3-methoxybenzylidene)pyrazine-2-carbohydrazide monohydrate By scripts.iucr.org Published On :: 2020-01-10 In the title hydrated Schiff base, C13H12N4O3·H2O, the dihedral angle between the aromatic rings is 5.06 (11)° and an intramolecular O—H⋯N hydrogen bond closes an S(6) ring. In the crystal, Ow—H⋯O and Ow—H⋯N (w = water) hydrogen bonds link the components into centrosymmetric tetramers (two Schiff bases and two water molecules). Longer N—H⋯O hydrogen bonds link the tetramers into [010] chains. A weak C—H⋯O hydrogen bond and aromatic π–π stacking between the pyrazine and phenyl rings [centroid–centroid separations = 3.604 (2) and 3.715 (2) Å] are also observed. Full Article text
world news 2-[(5-Chloropyridin-2-ylimino)methyl]phenol By scripts.iucr.org Published On :: 2020-01-31 In the title compound, C12H9ClN2O, the dihedral angle between the aromatic rings is 1.78 (4)° and an intramolecular O—H⋯N hydrogen bond closes an S(6) ring. In the crystal, C—H⋯O and C—H⋯N hydrogen bonds connect the molecules into [001] chains. Full Article text
world news Bis(1-dodecyl-4-aza-1-azoniabicyclo[2.2.2]octane)tetraisothiocyanatocobalt(II) By scripts.iucr.org Published On :: 2020-01-28 The title compound, [Co(C18H37N2)2(NCS)4], consists of a cobalt(II) ion positioned on the origin of the triclinic unit cell. It is coordinated by the N atoms of two trans-oriented 1-dodecyl-4-aza-1-azoniabicyclo[2.2.2]octane (DABCO+) cations, which carry n-dodecyl chains at the non-coordinating N atoms. The distorted octahedral coordination environment of the CoII ion is completed through four N atoms of isothiocyanate ions, which are arranged within the equatorial plane. Non-classical hydrogen bonding of the types C—H⋯N and C—H⋯S between the filamentous molecules lead to the formation of layers parallel to (001). Full Article text
world news Dichloridobis[2-(pyridin-2-yl-κN)-1H-benzimidazole-κN3]nickel(II) monohydrate By scripts.iucr.org Published On :: 2020-01-28 In the title complex, [NiCl2(C12H9N3)2]·H2O, a divalent nickel atom is coordinated by two 2-(pyridin-2-yl)-1H-benzimidazole ligands in a slightly distorted octahedral environment defined by four N donors of two N,N'-chelating ligands, along with two cis-oriented anionic chloride donors. The title complex crystallized with a water molecule disordered over two positions. In the crystal, a combination of O—H⋯Cl, O—H.·O and N—H⋯Cl hydrogen bonds, together with C—H⋯O, C—H⋯Cl and C—H⋯π interactions, links the complex molecules and the water molecules to form a supramolecular three-dimensional framework. The title complex is isostructural with the cobalt(II) dichloride complex reported previously [Das et al. (2011). Org. Biomol. Chem. 9, 7097–7107]. Full Article text
world news Diethyl 4-(1H-imidazol-2-yl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate By scripts.iucr.org Published On :: 2020-01-17 In the title compound, C16H21N3O4, the 1,4-dihydropyridine ring adopts a flattened boat conformation, with the imidazole substituent in an axial orientation [dihedral angle between ring planes = 82.9 (6)°]. In the crystal structure, pairs of N—H⋯O and N—H⋯N hydrogen bonds with graph-set notation R22(14) connect the molecules into chains running along the c-axis direction. Full Article text
world news Bis(4-phenyl-2-sulfanylidene-2,3-dihydro-1,3-thiazol-3-ido-κ2S2,N)(4-phenyl-1,3-thiazole-2-thiolato-κS2)bismuth By scripts.iucr.org Published On :: 2020-01-28 The title compound, [Bi(C9H6NS2)3], was prepared by reacting BiCl3 and 2-mercapto-4-phenylthiazole (LH) at room temperature in a stoichiometric ratio of 1:4. The molecular structure reveals a slightly distorted square-pyramidal environment around the BiIII atom. Two of the three monoanionic ligands L− coordinate in an N,S-bidentate mode, while one shows a monodentate mode through an S atom. There are no significant intermolecular interactions present in the crystal. Full Article text
world news (E)-1-(4-Fluoro-2-hydroxyphenyl)-3-(2,3,4-trimethoxyphenyl)prop-2-en-1-one By scripts.iucr.org Published On :: 2020-01-24 In the title molecule, C18H17FO5, the conformation about the C=C bond of the central enone group is trans. The dihedral angle between the benzene rings is 13.08 (3)°. The hydroxy group attached to the benzene ring is involved in an intramolecular O—H⋯O hydrogen bond. In the crystal, weak C—H⋯O hydrogen bonds link the molecules into chains along [001]. Full Article text
world news [4-(4-Methoxyphenyl)-8-oxo-3-(phenylselanyl)spiro[4.5]deca-3,6,9-trien-2-yl]methylcyanamide By scripts.iucr.org Published On :: 2020-01-28 The title compound, C25H22N2O2Se, crystallizes in the space group P21/c with one molecule in the asymmetric unit. The compound was synthesized by the addition of phenylselenyl bromide to a cyanamide. The phenylselenyl portion and the cyano group, as well as the ketone functional group in the cyclohexa-2,5-dien-1-one portion of the structure, are disordered, with occupancy factors of 0.555 (14) and 0.445 (14). Full Article text
world news Benzene-1,2-diaminium bis(4-methylbenzene-1-sulfonate) By scripts.iucr.org Published On :: 2020-01-31 The structure of the title salt, C6H10N22+·2C7H7O3S−, consists of a unique benzene-1,2-diaminium dication charge balanced by a pair of crystallographically independent 4-methylbenzene-1-sulfonate anions. The cations and anions are interlinked by several N—H⋯O hydrogen bonds. Full Article text
world news 3-(4-Iodophenyl)-2,3-dihydro-1H-benzo[f]chromen-1-one By scripts.iucr.org Published On :: 2020-01-31 In the title compound, C19H13IO2, the dihedral angle between the naphthyl ring system and the pendant iodophenyl ring is 72.48 (11)°. In the crystal, C—H⋯π interactions and I⋯O [3.293 (2) Å] halogen bonds are observed, which combine to generate a herringbone packing motif. Full Article text
world news 5-Methyl-4-(5-methyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-2-phenyl-1H-pyrazol-3(2H)-one By scripts.iucr.org Published On :: 2020-02-11 The title compound, C20H18N4O2, known as bispyrazolone, was crystallized from dimethyl sulfoxide. The structure has orthorhombic (Pbca) symmetry at 150 K, and displays both intra- and intermolecular hydrogen bonding through C—H⋯O and N—H⋯O contacts, respectively. None of the phenyl and pyrazolone rings in the molecule are coplanar. The dihedral angle between the pyrazolone rings is 66.18 (5)°. Full Article text
world news Redetermination of the crystal structure of caesium tetrafluoridobromate(III) from single-crystal X-ray diffraction data By scripts.iucr.org Published On :: 2020-01-31 Caesium tetrafluoridobromate(III), CsBrF4, was crystallized in form of small blocks by melting and recrystallization. The crystal structure of CsBrF4 was redetermined from single-crystal X-ray diffraction data. In comparison with a previous study based on powder X-ray diffraction data [Ivlev et al. (2013). Z. Anorg. Allg. Chem. 639, 2846–2850], bond lengths and angles were determined with higher precision, and all atoms were refined with anisotropic displacement parameters. It was confirmed that the structure of CsBrF4 contains two square-planar [BrF4]− anions each with point group symmetry mmm, and a caesium cation (site symmetry mm2) that is coordinated by twelve fluorine atoms, forming an anticuboctahedron. CsBrF4 is isotypic with CsAuF4. Full Article text
world news N-[(E)-Quinolin-2-ylmethylidene]-1,2,4-triazol-4-amine hemihydrate By scripts.iucr.org Published On :: 2020-02-03 The title hemihydrate, C12H9N5·0.5H2O, was isolated from the condensation reaction of quinoline-2-carbaldehyde with 4-amino-4H-1,2,4-triazole. The Schiff base molecule adopts an E configuration about the C=N bond and is approximately planar, with a dihedral angle between the quinoline ring system and the 1,2,4-triazole ring of 12.2 (1)°. In the crystal, one water molecule bridges two Schiff base molecules via O—H⋯N hydrogen bonds. The Schiff base molecules are interconnected by π–π stacking interactions [centroid-centroid distances of 3.7486 (7) and 3.9003 (7) Å] into columns along [1overline{1}0]. Full Article text
world news (3S,5R,6S)-Diphenylmethyl 1-oxo-6-bromopenicillanate By scripts.iucr.org Published On :: 2020-02-11 In the title compound, C21H20BrNO4S, a key intermediate in the synthesis of the widely used β-lactamase inhibitor tazobactam, the five-membered thiazolidine ring adopts an envelope conformation and the four-membered azetidine ring is in a distorted planar conformation. The crystal structure features C—H⋯O hydrogen bonds and a weak C—H⋯π interaction. Full Article text
world news Dicaesium tetramagnesium pentakis(carbonate) decahydrate, Cs2Mg4(CO3)5·10H2O By scripts.iucr.org Published On :: 2020-02-11 The title carbonate hydrate, Cs2Mg4(CO3)5·10H2O, was crystallized at room temperature out of aqueous solutions containing caesium bicarbonate and magnesium nitrate. Its monoclinic crystal structure (P21/n) consists of double chains of composition 1∞[Mg(H2O)2/1(CO3)3/3], isolated [Mg(H2O)(CO3)2]2– units, two crystallographically distinct Cs+ ions and a free water molecule. The crystal under investigation was twinned by reticular pseudomerohedry. Full Article text
world news Hydronium bis(trifluoromethanesulfonyl)amide–18-crown-6 (1/1) By scripts.iucr.org Published On :: 2020-02-06 The structure of the title compound, H3O+·C2F6NO4S2−·C12H24O6 or [H3O+·C12H24O6][N(SO2CF3)2−], which is an ionic liquid with a melting point of 341–343 K, has been determined at 113 K. The asymmetric unit consists of two crystallographically independent 18-crown-6 molecules, two hydronium ions and two bis(trifluoromethanesulfonyl)amide anions; each 18-crown-6 molecule complexes with a hydronium ion. In one 18-crown-6 molecule, a part of the ring exhibits conformational disorder over two sets of sites with an occupancy ratio of 0.533 (13):0.467 (13). One hydronium ion is complexed with the ordered 18-crown-6 molecule via O—H⋯O hydrogen bonds with H2OH⋯OC distances of 1.90 (6)–2.19 (7) Å, and the other hydronium ion with the disordered crown molecule with distances of 1.85 (6)–2.36 (6) Å. The hydronium ions are also linked to the anions via O—H⋯F hydrogen bonds. The crystal studied was found to be a racemic twin with a component ratio of 0.55 (13):0.45 (13). Full Article text
world news 2-(Octadecylsulfanyl)-1,3-thiazole By scripts.iucr.org Published On :: 2020-02-11 The title compound, C21H39NS2, crystallizes with two molecules in the asymmetric unit, both having a linear 18-carbon alkyl chain bound through a thioether group. No π–π stacking or hydrogen bonding is observed. The orientation of the alkyl chains facilitates intermolecular interactions between te chains. The structure is metrically orthorhombic but crystallizes in the monoclinic space group P21 and was found to be twinned by pseudomerohedry (emulating orthorhombic symmetry) and by inversion. The twin factions refined to 0.37 (4), 0.13 (4), 0.31 (5), and 0.19 (4). Full Article text
world news 2,2'-[Methylenebis(sulfanediyl)]bis(pyridine 1-oxide) By scripts.iucr.org Published On :: 2020-02-11 The title compound, C11H10N2O2S2, crystallizes with one complete molecule in the asymmetric unit. In the crystal, weak hydrogen bonding is observed between the N-oxide moieties and several C—H units. Full Article text
world news 5-Nitro-2,3-bis(thiophen-2-yl)quinoxaline By scripts.iucr.org Published On :: 2020-02-14 The title compound, C16H9N3O2S2, was synthesized via a condensation reaction in refluxing acetic acid. The dihedral angles between the mean plane of the quinoxaline unit and the thienyl rings are 35.16 (5)° and 24.94 (3)°. Full Article text
world news 6-Nitro-2,3-bis(thiophen-2-yl)quinoxaline By scripts.iucr.org Published On :: 2020-02-14 The title compound, C16H9N3O2S2, was synthesized via a condensation reaction in refluxing acetic acid. One thienyl ring is nearly coplanar with the quinoxaline unit [dihedral angle = 3.29 (9)°], the other makes an angle of 83.96 (4)°. Full Article text
world news 1,4-Bis(4-methoxyphenyl)naphthalene By scripts.iucr.org Published On :: 2020-02-21 The title naphthalene derivative, C24H20O2, features 4-methyoxy-substituted benzene rings in the 1 and 4 positions of the naphthalene ring system. There are two crystallographically independent molecules (A and B) in asymmetric unit. The independent molecules have very similar conformations in which the naphthalene ring systems are only slightly bent, exhibiting dihedral angles between the constituent benzene rings of 3.76 (15) and 3.39 (15)° for A and B, respectively. The pendent 4-methyoxybenzene rings are splayed out of the plane through the naphthalene ring system to which they are connected [range of dihedral angles = 59.63 (13) to 67.09 (13)°]. In the crystal, the molecular packing is consolidated by intermolecular C—H⋯π interactions, leading to supramolecular chains along the b axis. The chains assemble without directional interactions between them. Full Article text
world news 6-[(tert-Butyldimethylsilyl)oxy]-3-ethenyl-7-methoxy-4-[(trimethylsilyl)ethynyl]naphtho[2,3-c]furan-1(3H)-one By scripts.iucr.org Published On :: 2020-02-21 The tricyclic core in the title compound, C26H34O4Si2, shows disorder of the furan ring and deviates slightly from planarity, with the largest displacement from the least-squares plane [0.166 (2) Å] for the major disordered part of the methine C atom. To this C atom the likewise disordered vinyl group is attached, lying nearly perpendicular to the tricyclic core. In the crystal, mutual C—H⋯π interactions between the methine group of the furan ring and the central ring of the tricyclic core of an adjacent molecule lead to inversion-related dimers. Full Article text
world news 2-Aminoanilinium 4-methylbenzenesulfonate By scripts.iucr.org Published On :: 2020-02-21 In the extended structure of the title molecular salt, C6H9N2+·C7H7O3S−, the cations and anions are linked by N—H⋯O hydrogen bonds to generate [010] chains. Full Article text
world news 1,3-Bis(2-oxopropyl)thymine By scripts.iucr.org Published On :: 2020-02-28 In the title compound [systematic name: 5-methyl-1,3-bis(2-oxopropyl)pyrimidine-2,4(1H,3H)-dione], C11H14N2O4, the two 2-oxopropyl groups are nearly perpendicular to the planar thymine unit. One methyl group of oxopropyl substituent is disordered. In the crystal, C—H⋯O interactions help to connect the molecules into (001) layers. Full Article text
world news Bis(N-adamantyl-N'-ethylimidazolium) tetrabromidomanganate(II) By scripts.iucr.org Published On :: 2020-03-03 The title compound, (C15H23N2)2[MnBr4], comprises two N-adamantyl-N'-ethylimidazolium cations and one tetrahedral [MnBr4]2− anion. Next to Coulombic interactions, weak hydrogen bonds of the type C—H⋯Br consolidate the crystal packing, building up a three-dimensional network. Full Article text
world news [(1R*,3S*,4S*)-3-(2-Hydroxybenzoyl)-1,2,3,4-tetrahydro-1,4-epoxynaphthalen-1-yl]methyl 4-nitrobenzoate By scripts.iucr.org Published On :: 2020-02-28 The relative stereo- and regiochemistry of the racemic title compound, C25H19NO7, were established from the crystal structure. The fused benzene ring forms dihedral angles of 77.3 (1) and 60.3 (1)° with the hydroxy-substituted benzene ring and the nitro-substituted benzene ring, respectively. The dihedral angle between the hydroxy-substituted benzene ring and the nitro-substituted benzene ring is 76.4 (1)°. An intramolecular O—H⋯O hydrogen bond closes an S(6) ring. In the crystal, weak C—H⋯O hydrogen bonds connect the molecules, forming layers parallel to (100). Within these layers, there are weak π–π stacking interactions with a ring centroid–ring centroid distance of 3.555 (1) Å. Full Article text
world news Tris(1H-benzimidazol-2-ylmethyl)amine methanol trisolvate By scripts.iucr.org Published On :: 2020-03-05 The structure of the tertiary amine tris(1H-benzimidazol-2-ylmethyl)amine (C24H21N7, abbreviated ntb) has been previously reported twice as solvates, namely the monohydrate and the acetonitrile–methanol–water (1/0.5/1.5) solvate, both with the tripodal conformation formed via multiple hydrogen bonds. Now, we report the trimethanol adduct, ntb·3CH3OH, where the amine has the stair conformation featuring one benzimidazole group oriented in the opposite direction from the other two. The asymmetric unit contains one-half amine, completed through the mirror plane m in space group Pmn21 to form the ntb molecule, with the H atom for each imidazole moiety equally disordered between both N sites available in the imidazole ring. The asymmetric unit also contains one and a half methanol molecules, one being placed in general position with the hydroxy H atom disordered over two sites with occupancy ratio 1:1, while the other lies on the m mirror plane, and has thus its hydroxy H atom disordered by symmetry. As in the previously reported solvates, all imine and amine groups of the ntb molecules and the methanol molecules are involved in N—H⋯O and O—H⋯N hydrogen bonds. In the title compound, however, the involved H atom is systematically a disordered H atom provided by an imidazole group or a methanol molecule. Full Article text
world news 1,2,3,5-Tetrahydronaphtho[2,1-c]oxepine By scripts.iucr.org Published On :: 2020-03-05 In the title compound, C14H14O, the seven-membered ring is in a pseudo-chair conformation. In the crystal, molecules are linked by weak C—H⋯O hydrogen bonds forming layers parallel to (010). In addition, there are weak π–π stacking interactions between inversion-related naphthalene ring systems, with a ring centroid–ring centroid distance of 3.518 (5) Å. Full Article text
world news 12-Ethyl-6a,10a-dihydro-5H-6-oxachrysene By scripts.iucr.org Published On :: 2020-03-05 In the title compound, C19H16O, the pyran ring is in a half-chair conformation. The essentially planar naphthalene ring system (r.m.s. deviation = 0.020 Å) forms a dihedral angle of 14.37 (5)° with the fused benzene ring. In the crystal, pairs of molecules are connected into inversion dimers by weak C—H⋯O hydrogen bonds to generate R22(6) loops. Full Article text
world news The head-to-head photodimer of indenoindene By scripts.iucr.org Published On :: 2020-03-05 Irradiation of 1-(1-benzocyclobutenylidene)benzocyclobutene gives indenoindene and its head-to-head photodimer nonacyclo[9.7.7.72,10.01,11.02,10.03,8.012,17.019,24.026,31]dotriaconta-3,5,7,12,14,16,19,21,23,26,28,30-dodecaene, C32H24. The molecule is built from four essentially planar indane units attached to an elongated cyclobutane ring. In the crystal, C—H⋯π interactions connect molecules into layers parallel to the bc plane. Full Article text
world news Bis(3-methyl-1-propyl-1H-imidazol-3-ium) bis(4,6-disulfanidyl-4,6-disulfanylidene-1,2,3,5,4,6-tetrathiadiphosphinane-κ3S2,S4,S6)nickel By scripts.iucr.org Published On :: 2020-04-24 The title salt, (PMIM)2[Ni(P2S8)2] (PMIM = 3-methyl-1-propyl-1H-imidazol-3-ium, C7H13N2+), consists of a nickel–thiophosphate anion charge-balanced by a pair of crystallographically independent PMIM cations. It crystallizes in the monoclinic space group P21/n. The structure exhibits the known [Ni(P2S8)2]2− anion with two unique imidazolium cations in the asymmetric unit. Whereas one PMIM cation is well ordered, the other is disordered over two orientations with refined occupancies of 0.798 (2) and 0.202 (2). The salt was prepared directly from the elements in the ionic liquid [PMIM]CF3SO3. Whereas one of the PMIM cations is well behaved (it does not exhibit disorder even in the propyl side chain), the other is found in two overlapping positions. The refined occupancies for the two orientations are roughly 80:20. Here, too, there appears to be little disorder in the propyl arm. Full Article text
world news [1–9-NαC]-Linusorb B3 (Cyclolinopeptide A) dimethyl sulfoxide monosolvate By scripts.iucr.org Published On :: 2020-03-13 Crystals of the dimethyl sulfoxide (DMSO) solvate of [1–9-NαC]-linusorb B3 (Cyclolinopeptide A; CLP-A; C57H84N9O9·C2H6OS), a cyclic polypeptide were obtained following peptide extraction and purification from flaxseed oil. There are four intramolecular N—H⋯O hydrogen bonds. In the crystal, the molecules are linked in chains along the a axis by N—H⋯O hydrogen bonds. Each DMSO O atom accepts a hydrogen bond from an NH group at the Phe6 location in the CLP-A molecule. Full Article text
world news 12,15-Dimethyl-8-oxatetracyclo[8.8.0.02,7.011,16]octadeca-1(18),2,4,6,11(16),12,14-heptaen-10-ol By scripts.iucr.org Published On :: 2020-03-10 In the title compound, C19H18O2, the pyran ring is in a half-chair conformation. The fused ring system comprising the benzene and cyclohexene rings is essentially planar (r.m.s. deviation = 0.053 Å) and forms a dihedral angle of 27.95 (6)° with the other benzene ring. In the crystal, O—H⋯O hydrogen bonds connect the molecules into chains propagating along [001]. Full Article text
world news (E)-6-(Furan-2-ylmethylidene)-6,7,8,9-tetrahydropyrido[2,1-b]quinazoline-11-thione By scripts.iucr.org Published On :: 2020-03-13 A quinazolinthione, C17H14N2OS, was synthesized by the condensation reaction of 6,7,8,9-tetrahydro-11H-pyrido[2,1-b]quinazolin-11-thione with furfural. The molecule crystallizes in the monoclinic system (Cc space group) and has an E configuration with respect to the exocyclic C=C bond. In the crystal, molecules are linked through C—H⋯π(furan) interactions, forming zigzag chains propagating along the [001] direction. Full Article text
world news 2,5-Bis[(E)-2-phenylethenyl]-3,6-bis(pyridin-2-yl)pyrazine By scripts.iucr.org Published On :: 2020-03-17 The molecule of the title compound, C30H22N4, exhibits inversion symmetry adopting the shape of a St Andrew's Cross. It shows dihedral angles between adjacent aryl units of around 50° whereas torsion angles of ca 10° are found along the arylene vinylene path. Full Article text
world news 7-Chloro-3-(4-methylbenzenesulfonyl)pyrrolo[1,2-c]pyrimidine By scripts.iucr.org Published On :: 2020-03-27 In the title compound, C14H11ClN2O2S, the dihedral angle between the pyrrolo[1,2-c]pyrimidine ring system (r.m.s. deviation = 0.008 Å) and the benzene ring is 80.2 (9)°. In the crystal, inversion dimers linked by pairs of C—H⋯O interactions generate R22(16) loops. Several aromatic π–π stacking interactions between the pyrrolo[1,2-c]pyrimidine rings, as well as separately between the pyrrolo and pyrimidine groups [shortest centroid–centroid separation = 3.5758 (14) Å], help to consolidate the packing. Full Article text
world news 4-Amino-6-(piperidin-1-yl)pyrimidine-5-carbonitrile By scripts.iucr.org Published On :: 2020-03-17 In the title compound, C10H13N5, the piperidine ring adopts a chair conformation with the exocyclic N—C bond in an axial orientation, and the dihedral angle between the mean planes of piperidine and pyrimidine rings is 49.57 (11)°. A short intramolecular C—H⋯N contact generates an S(7) ring. In the crystal, N—H⋯N hydrogen bonds link the molecules into (100) sheets and a weak aromatic π-π stacking interaction is observed [centroid–centroid separation = 3.5559 (11) Å] between inversion-related pyrimidine rings. Full Article text
world news Poly[(μ4-5,7-dihydro-1H,3H-dithieno[3,4-b:3',4'-e]pyrazine-κ4N:N':S:S')tetra-μ3-iodido-tetracopper]: a three-dimensional copper(I) coordination polymer By scripts.iucr.org Published On :: 2020-03-27 The reaction of ligand 5,7-dihydro-1H,3H-dithieno[3,4-b:3',4'-e]pyrazine (L) with CuI lead to the formation of a three-dimensional coordination polymer, incorporating the well known [CuxIx]n staircase motif (x = 4). These polymer [Cu4I4]n chains are linked via the N and S atoms of the ligand to form the three-dimensional coordination polymer poly[(μ4-5,7-dihydro-1H,3H-dithieno[3,4-b:3',4'-e]pyrazine-κ4N:N':S:S')tetra-μ3-iodido-tetracopper], [Cu4I4(C8H8N2S2)]n (I). The asymmetric unit is composed of half a ligand molecule, with the pyrazine ring located about a center of symmetry, and two independent copper(I) atoms and two independent I− ions forming the staircase motif via centers of inversion symmetry. The framework is consolidated by C—H⋯I hydrogen bonds. Full Article text
world news Trimethyl 4,4',4''-(ethene-1,1,2-triyl)tribenzoate By scripts.iucr.org Published On :: 2020-03-31 The title compound, C26H22O6, is formed as the major product from the reaction between syn-1,2-bis(pinacolatoboron)-1,2-bis(4-methylcarboxyphenyl)ethene and excess methyl 4-iodobenzoate in basic DMSO using a palladium catalyst at 80°C via Suzuki coupling followed by protodeboronation. Crystals were grown by slow evaporation of a hexanes solution at room temperature. Full Article text
world news Crystal structure of the Al8Cr5-type intermetallic Al7.85Cr5.16 By scripts.iucr.org Published On :: 2020-04-09 An aluminium-deficient Al8Cr5-type intermetallic with formula Al7.85Cr5.16 (octaaluminium pentachromium) was uncovered when high-pressure sintering of a mixture with composition Al11Cr4 was carried out. Structure analysis reveals that there are three co-occupied positions with refined occupancy factors for Al atoms being 0.958, 0.772 and 1/2. The present phase is confirmed to be isotypic with the previously reported rhombohedral Al8Cr5 ordered phase [Bradley & Lu (1937). Z. Kristallogr. 96, 20–37] and structurally closely related to the disordered phases of rhombohedral Al16Cr9.5 and cubic Al8Cr5. Full Article text
world news 6-Methyl-4-{[4-(trimethylsilyl)-1H-1,2,3-triazol-1-yl]methyl}-2H-chromen-2-one By scripts.iucr.org Published On :: 2020-04-03 In the title compound, C16H19N3O2Si, the dihedral angle between the coumarin ring system (r.m.s. deviation = 0.031 Å) and the triazole ring is 73.81 (8)°. In the crystal, molecules are linked into [010] chains by weak C—H⋯O interactions. Full Article text
world news Diaquatetrakis(μ-3-methoxybenzoato-κ2O1:O1')dicopper(II) By scripts.iucr.org Published On :: 2020-04-07 The asymmetric unit of the binuclear title compound, [Cu2(C8H7O3)4(H2O)2], comprises two halves of diaquatetrakis(μ-3-methoxybenzoato-κ2O1:O1')dicopper(II) units. The paddle-wheel structure of each complex is completed by application of inversion symmetry, with the inversion centre situated at the midpoint between two CuII atoms in each dimer. The two CuII atoms of each centrosymmetric dimer are bridged by four 3-methoxybenzoate anions resulting in Cu⋯Cu separations of 2.5961 (11) and 2.6060 (12) Å, respectively. The square-pyramidal coordination sphere of each CuII atom is completed by an apical water molecule. Intermolecular O—H⋯O hydrogen bonds of weak nature link the complexes into layers parallel to (100). The three-dimensional network structure is accomplished by C—H⋯O hydrogen bonds interlinking adjacent layers. Full Article text
world news 2,2,3,3,4,4,5,5-Octafluorohexane-1,6-diol By scripts.iucr.org Published On :: 2020-04-07 In the crystal of the title compound, C6H6F8O4, O—H⋯O hydrogen bonds involving the hydroxy groups connect the molecules, forming a two-dimensional network parallel to (100). These hydrogen-bonding interactions appear to drive the O—C—C—O torsion angles into a gauche–trans–trans series of conformations along the backbone of the molecule. Full Article text
world news Tris(4,4'-di-tert-butyl-2,2'-bipyridine)(trans-4-tert-butylcyclohexanolato)deca-μ-oxido-heptaoxidoheptavanadium acetonitrile monosolvate including another unknown solvent molecule By scripts.iucr.org Published On :: 2020-04-07 The title heptanuclear alkoxido(oxido)vanadium(V) oxide cluster complex, [V7(C10H19O)O17(C18H24N2)3]·CH3CN, was obtained by the reaction of [V8O20(C18H24N2)4] with 4-tert-butylcyclohexanol (mixture of cis and trans) in a mixed CHCl3/CH3CN solvent. The complex has a V7O18N6 core with approximately Cs symmetry, which is composed of two VO4 tetrahedra, two VO6 octahedra and three VO4N2 octahedra. In the crystal, these complexes are linked together by weak intermolecular C—H⋯O hydrogen bonds between the 4,4'-di-tert-butyl-2,2'-bipyridine ligand and the V7O18N6 core, forming a one-dimensional network along the c-axis direction. Besides the complex, the asymmetric unit contains one CH3CN solvent molecule. The contribution of other disordered solvent molecules to the scattering was removed using the SQUEEZE option in PLATON [Spek (2015). Acta Cryst. C71, 9–18]. The unknown solvent molecules are not considered in the chemical formula and other crystal data. Full Article text
world news 2,3-Diethylbenzo[g]quinoxaline By scripts.iucr.org Published On :: 2020-04-07 The title compound, C16H16N2, was synthesized by dispersing 3,4-hexanedione in a methanol–water solution containing the acid catalyst NH4HF2, then adding 1,2-diaminonaphthalene. The fused-ring system of the title compound is close to planar (r.m.s. deviation = 0.028 Å); one of the pendant methyl C atoms lies close to the ring plane [deviation = 0.071 (2) Å; N—C—C—C = −0.27 (18)°] whereas the other is significantly displaced [–1.7136 (18) Å; 91.64 (16)°]. The molecules pack in space group Ioverline{4} in a distinctive criss-cross motif supported by numerous aromatic π–π stacking interactions [shortest centroid–centroid separation = 3.5805 (6) Å]. Full Article text
world news Poly[[μ4-3,4,8,10,11,13-hexahydro-1H,6H-bis([1,4]dithiocino)[6,7-b:6',7'-e]pyrazine]di-μ-iodido-dicopper(I)]: a two-dimensional copper(I) coordination polymer By scripts.iucr.org Published On :: 2020-04-07 The reaction of ligand 3,4,8,10,11,13-hexahydro-1H,6H-bis([1,4]dithiocino)[6,7-b:6',7'-e]pyrazine (L) with CuI led to the formation of a two-dimensional coordination polymer, incorporating a [Cu2I2] motif. These units are linked via the four S atoms of the ligand to form the title two-dimensional coordination polymer, poly[[μ4-3,4,8,10,11,13-hexahydro-1H,6H-bis([1,4]dithiocino)[6,7-b:6',7'-e]pyrazine]di-μ-iodido-dicopper(I)], [Cu2I2(C12H16N2S4)]n, (I). The asymmetric unit is composed of a ligand molecule, two copper(I) atoms and two I− ions. Both copper(I) atoms are fourfold S2I2 coordinate with almost regular trigonal-pyramidal environments. In the crystal, the layers, lying parallel to (102), are linked by C—H⋯I hydrogen bonds, forming a supramolecular framework. Full Article text
world news Redetermination of diammonium trivanadate, (NH4)2V3O8 By scripts.iucr.org Published On :: 2020-04-09 The crystal structure of (NH4)2V3O8 has been reported twice using single-crystal X-ray data [Theobald et al. (1984). J. Phys. Chem. Solids, 45, 581–587; Range et al. (1988). Z. Naturforsch. Teil B, 43, 309–317]. In both cases, the orientation of the ammonium cation in the asymmetric unit was poorly defined: in Theobald's study, the shape and dimensions were constrained for NH4+, while in Range's study, H atoms were not included. In the present study, we collected a highly redundant data set for this ternary oxide, at 0.61 Å resolution, using Ag Kα radiation. These accurate data reveal that the NH4+ cation is disordered by rotation around a non-crystallographic axis. The rotation axis coincides with one N—H bond lying in the mirror m symmetry element of space-group type P4bm, and the remaining H sites were modelled over two disordered positions, with equal occupancy. It therefore follows that the NH4+ cations filling the space available in the (001) layered structure formed by (V3O8)2– ions do not form strong N—H⋯O hydrogen bonds with the mixed-valent oxidovanadate(IV,V) anions. This feature could have consequences for the Li-ion intercalation properties of this material, which is used as a cathode for supercapacitors. Full Article text
world news 5-MeO-DALT: the freebase of N,N-diallyl-5-methoxytryptamine By scripts.iucr.org Published On :: 2020-04-17 The title compound {systematic name: N-[2-(5-methoxy-1H-indol-3-yl)ethyl]-N-(prop-2-en-1-yl)prop-2-en-1-amine), C17H22N2O, has a single tryptamine molecule in the asymmetric unit. The molecules are linked by strong N—H⋯N hydrogen bonds into zigzag chains with graph-set notation C(7) along the [010] direction. Full Article text
world news 2,6-Diphenyl-3-(prop-2-en-1-yl)piperidin-4-one By scripts.iucr.org Published On :: 2020-04-21 In the title compound, C20H21NO, the dihedral angle between the phenyl ring is 47.5 (1)° and the piperidine ring adopts a chair conformation. In the crystal, molecules are linked by C—H⋯π interactions into dimers with the molecules related by twofold symmetry. Full Article text
world news 2,4,6-Triphenyl-N-{(3E)-3-[(2,4,6-triphenylphenyl)imino]butan-2-ylidene}aniline By scripts.iucr.org Published On :: 2020-04-30 The title compound, C52H40N2, is disposed about a centre of inversion and the conformation about the imine bond [1.268 (3) Å] is E. The terminal benzene ring is approximately perpendicular to the central 1,4-diazabutadiene mean plane, forming a dihedral angle of 81.2 (3)°. Weak C—H⋯π and π–π [inter-centroid distance = 4.021 (5) Å] interactions help to consolidate the packing. Full Article text