3 Ethyl 5-[(ethoxycarbonyl)oxy]-5,5-diphenylpent-2-ynoate By scripts.iucr.org Published On :: 2019-11-15 The title compound, C22H22O5, crystallizes with two molecules in the asymmetric unit, one of which shows disorder of its ethyl acetate group over two sets of sites in a 0.880 (2):0.120 (2) ratio. The C≡C distances in the two molecules are almost the same [1.1939 (16) and 1.199 (2) Å], but the Csp3—C≡C angles differ somewhat [175.92 (12) and 172.53 (16)°]. In the crystal, several weak C—H⋯O interactions are seen. Full Article text
3 5-(3-Hydroxyphenyl)-1,3,4-oxadiazole-2(3H)-thione hemihydrate By scripts.iucr.org Published On :: 2019-11-15 The title 1,3,4-oxadiazole derivative crystallizes as a hemihydrate, C8H6N2O2S·0.5H2O, with the water molecule located on a twofold rotation axis. The 1,3,4-oxadiazole molecule is essentially planar, the r.m.s. deviation of the non-H atoms being 0.0443 Å. The dihedral angle between the mean planes of the phenyl and oxadiazole rings is 6.101 (17)°. In the crystal, molecules are linked via O—H⋯S and N—H⋯O hydrogen bonds involving the water molecule, the N—H group and the thione S atom into undulating ribbons. Additional π–π interactions generate a two-dimensional supramolecular framework extending parallel to (001). Full Article text
3 Sodium [N,N'-ethylenebis(d-penicillaminato)]indate(III) tetrahydrate By scripts.iucr.org Published On :: 2019-11-19 The asymmetric unit of the title compound {systematic name: sodium [2-({2-[(1-carboxylato-2-methyl-2-sulfanidylpropyl)amino]ethyl}amino)-3-methyl-3-sulfanidylbutanoato-κ4S,N,N',S']indate(III) tetrahydrate}, Na[In(C12H20N2O4S2)]·4H2O, contains four indate(III) complex anions {[In(d-ebp)]−; d-H4ebp = N,N'-ethyelenebis(d-penicillamine)], four sodium(I) cations and sixteen water molecules. The indate(III) anions and sodium cations are alternately connected through coordination bonds between Na+ ions and the carboxylate groups of the complex anions, forming an infinite sixfold right-handed helix along the c-axis direction. In the crystal, the helices are linked by O—H⋯O hydrogen bonds between water molecules bound to Na+ ions and carboxylate groups. The crystal studied was twinned via a twofold axis about [001]. Full Article text
3 [Oxybis(ethane-1,2-diyl)]bis(dimethylammonium) octamolybdate dihydrate By scripts.iucr.org Published On :: 2019-11-19 The title compound, (C8H22N2O)2[Mo8O26]·H2O, (cis-H2L)2[β-Mo8O26]·H2O, where L = (bis[2-N,N-dimethylamino)ethyl] ether), was synthesized from bis[2-(dimethylamino)ethyl] ether and MoO3 under solvothermal conditions and characterized by multinuclear NMR and single-crystal X-ray diffraction techniques. The structure displays two [oxybis(ethane-1,2-diyl)]bis(dimethylammonium), or [cis-H2L]2+, cations, a central [β-Mo8O26]4− anionic cluster consisting of eight distorted MoO6 octahedra, and two water molecules in their deuterated form. The central anion lies across an inversion center. The [cis-H2L]2+ cations are hydrogen bonded to the central [β-Mo8O26]4− cluster via bridging water molecules. In the crystal, O—H⋯O hydrogen bonds link the components into chains along [010]. Weak C—H⋯O hydrogen bonds link these chains into a three-dimensional network. Full Article text
3 μ2-Methanol-κ2O:O-bis[(1,10-phenanthroline-κ2N,N')bis(2,3,4,5-tetrafluorobenzoato)-κO;κ2O,O'-copper(II)] By scripts.iucr.org Published On :: 2019-11-29 In the title compound, [Cu2(C7HF4O2)4(C12H8N2)2(CH3OH)], the molecule lies on a twofold rotation axis in space group C2/c. The Cu2+ ion exhibits a distorted octahedral sphere with two N atoms from the phenanthroline ligand, three O atoms from the 2,3,4,5-tetrafluorobenzoate ligands and one O atom from a methanol molecule. The distortion from an octahedral shape is a consequence of the Jahn–Teller effect of CuII and the small bite angle for the bidentate fluorobenzoate ligand [54.50 (11)°]. The methanol molecule bridges two symmetry-related CuII atoms to form the complete molecule. In the bidentate fluorobenzoate ligand, one F atom is disordered over two positions of equal occupancy. In the crystal structure, only weak intermolecular interactions are observed. Full Article text
3 Rubidium tetrafluoridobromate(III): redetermination of the crystal structure from single-crystal X-ray diffraction data By scripts.iucr.org Published On :: 2019-11-29 Single crystals of rubidium tetrafluoridobromate(III), RbBrF4, were grown by melting and recrystallizing RbBrF4 from its melt. This is the first determination of the crystal structure of RbBrF4 using single-crystal X-ray diffraction data. We confirmed that the structure contains square-planar [BrF4]− anions and rubidium cations that are coordinated by F atoms in a square-antiprismatic manner. The compound crystallizes in the KBrF4 structure type. Atomic coordinates and bond lengths and angles were determined with higher precision than in a previous report based on powder X-ray diffraction data [Ivlev et al. (2015). Z. Anorg. Allg. Chem. 641, 2593–2598]. Full Article text
3 (E)-1-(5-Methylthiophen-2-yl)-N-(4-nitrophenyl)methanimine By scripts.iucr.org Published On :: 2019-12-03 The title compound, C12H10N2O2S, was synthesized via the acid-catalyzed condensation of 4-nitroaniline and 5-methyl-2-thiophenecarboxaldehyde in a methanol–water solution. The dihedral angle between the benzene and thiophene rings is 54.62 (3)°. No directional interactions could be identified in the extended structure. Full Article text
3 Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-κS)(triphenylphosphane-κP)osmium(IV): a monoclinic polymorph By scripts.iucr.org Published On :: 2019-12-06 The structure of the title compound, [Os(C6HF4S)4{P(C6H5)3}], has been previously reported [Arroyo et al. (1994). J. Chem. Soc. Dalton Trans. pp. 1819–1824], in the space group Poverline{1}. We have now obtained a monoclinic polymorph for this compound, crystallized from ethanol, while the previous form was obtained from a hexane/chloroform mixture. The molecular structure is based on a trigonal–bipyramidal OsIV coordination geometry, close to that observed previously in the triclinic form. Full Article text
3 Di-μ3-chlorido-tetra-μ2-chlorido-dichloridotetrakis(N,N-diethylethane-1,2-diamine-κ2N,N')tetracadmium(II) By scripts.iucr.org Published On :: 2019-12-06 In the title compound, [Cd4Cl8(C6H16N2)4], the Cd2+ cations and Cl− anions form M4Cl8 clusters with six of the Cl− ions bridging Cd2+ cations and two being pendant. Each Cd2+ cation has distorted octahedral coordination completed by four Cl− ions and two N atoms of the asymmetrical bidentate amino ligand. The cluster consists of pairs of face-sharing hexahedra linked by a shared edge. Full Article text
3 (2,2'-Bipyridine-κ2N,N')(pyridine-2,6-dicarboxylato-κ2N,O)palladium(II) monohydrate By scripts.iucr.org Published On :: 2019-12-06 In the title compound, [Pd(C7H3NO4)(C10H8N2)]·H2O, the PdII cation is four-coordinated in a distorted square-planar coordination geometry defined by the two N atoms of the 2,2'-bipyridine ligand, one O atom and one N atom from the pyridine-2,6-dicarboxylate anion. The complex and solvent water molecule are linked by intermolecular hydrogen bonds. In the crystal, the complex molecules are stacked in columns along the a axis. Full Article text
3 1,1,3,3-Tetraethyl-5-nitroisoindoline By scripts.iucr.org Published On :: 2019-12-17 The title compound, C16H24N2O2, previously obtained as a yellow oil, exhibits a rather low melting point close to room temperature 297–298 K). In the molecule, the isoindoline ring system is approximately planar and coplanar to the nitro group, forming a dihedral angle of 5.63 (15)°. In the crystal, only weak N—H⋯O and C—H⋯π interactions are observed, linking molecules into chains parallel to the [101] direction. Full Article text
3 6,6'-[(3,3'-Di-tert-butyl-5,5'-dimethoxy-1,1'-biphenyl-2,2'-diyl)bis(oxy)]bis(dibenzo[d,f][1,3,2]dioxaphosphepine) benzene monosolvate By scripts.iucr.org Published On :: 2019-12-10 The crystal structure of the benzene monosolvate of the well known organic diphosphite ligand BIPHEPHOS, C46H44O8P2·C6H6, is reported for the first time. Single crystals of BIPHEPHOS were obtained from a benzene solution after layering with n-heptane at room temperature. One specific property of this type of diphosphite structure is the twisting of the biphenyl units. In the crystal, C—H⋯π contacts and π–π stacking interactions [centroid-to-centroid distance = 3.8941 (15) Å] are observed. Full Article text
3 Diethyl 4-(3-chlorophenyl)-2,6-diphenyl-1,4-dihydropyridine-3,5-dicarboxylate By scripts.iucr.org Published On :: 2019-12-10 In the title compound, C29H26ClNO4, the dihydropyridine ring adopts a shallow boat conformation. The mean plane of the dihydropyridine ring (all atoms) subtends dihedral angles of 66.54 (1), 73.71 (1) and 79.47 (1)° with the two phenyl rings and the chlorophenyl ring, respectively. In the crystal, N—H⋯O hydrogen bonds link the molecules into [001] chains. Full Article text
3 Poly[1-ethyl-3-methylimidazolium [tri-μ-isothiocyanato-manganate(II)]] By scripts.iucr.org Published On :: 2019-12-17 The title compound, {(C9H11N2)[Mn(NCS)3]}n, has been obtained as a side product of the salt metathesis reaction of 1-ethyl-3-methylimidazolium bromide, (EMIm)Br, and K2[Mn(NCS)4]. The structure consists of discrete 1-ethyl-3-methylimidazolium cations and an anionic two-dimensional network of manganese(II)-based complex anions, interconnected by thiocyanate ions. Every Mn2+ ion is coordinated by three S atoms of three NCS− ions and three N atoms of further three NCS− ions in a meridional octahedral fashion. Full Article text
3 5,5'-(1-Phenylethane-1,1-diyl)bis(1H-pyrrole-2-carboxaldehyde) By scripts.iucr.org Published On :: 2019-12-17 In the title compound, C18H16N2O2, the dihedral angle between the pyrrole rings is 79.47 (9)°, with the N—H groups approximately orthogonal (H—N⋯N—H pseudo torsion angle = −106°). In the crystal, N—H⋯O hydrogen bonds link the molecules into [11overline{1}] chains. A C—H⋯O interaction is also observed. Full Article text
3 2-[4,5-Bis(4-bromophenyl)-1-(4-tert-butylphenyl)-1H-imidazol-2-yl]-4,6-dichlorophenol By scripts.iucr.org Published On :: 2019-12-24 In the title compound, C31H24Br2Cl2N2O, the dihedral angles subtended by the tert-butyl-phenyl, 4,6-dichlorophenol and 4-bromophenyl (×2) rings are 70.7 (3), 8.1 (3), 28.1 (3) and 84.2 (3)°, respectively. The orientations of the pendant rings may be related to intramolecular O—H⋯N and C—H⋯π interactions. One of the tert-butyl methyl groups is disordered over two sets of sites in a 0.54 (3):0.46 (3) ratio. In the crystal, a weak C—H⋯π interaction generates inversion dimers. Full Article text
3 Bis{2,6-bis[(E)-(4-fluorobenzylimino)methyl]pyridine}nickel(II) dinitrate dihydrate By scripts.iucr.org Published On :: 2019-12-20 In the title hydrated salt, [Ni(C21H17F2N3)2](NO3)2·2H2O, the central NiII ion is coordinated by six N atoms from two tridentate chelating 2,6-bis[(E)-(4-fluorobenzylimino)methyl]pyridine ligands. While the central NiII ion is six-coordinate, its environment is distorted from an octahedral structure because of the unequal Ni—N distances. The Ni—N bond lengths vary from 1.8642 (14) to 2.2131 (15) Å, while the N—Ni—N angles range from 79.98 (6) to 104.44 (6)°. Three coordinating sites of each chelating agent are almost coplanar with respect to the pyridine ring, and two pyridine moieties are perpendicular to each other. Two non-coordinating nitrate anions within the asymmetric unit balance the charges of the central metal ion, and are linked with two crystal water molecules, forming a water–nitrate cyclic tetrameric unit [O⋯O = 2.813 (2) to 3.062 (2) Å]. In an isolated molecule, the fluorophenyl rings of one ligand are stacked with the central ring of the other ligand via π–π interactions, with the closest centroid-to-plane distances being 3.359 (6), 3.408 (5), 3.757 (6) and 3.659 (5) Å. Full Article text
3 4-Chloro-2-[1-(4-ethylphenyl)-4,5-diphenyl-1H-imidazol-2-yl]phenol By scripts.iucr.org Published On :: 2020-01-03 In the title compound, C29H23ClN2O, the 5-chlorophenol ring and the imidazole ring are nearly coplanar, with a dihedral angle of 15.76 (9)° between them. The ethylphenyl ring and the two phenyl rings subtend angles of 71.09 (7), 43.95 (5) and 36.53 (9)°, respectively, with the imidazole plane. An intramolecular O—H⋯N hydrogen bond supports the molecular conformation, and an intermolecular C—H⋯O interaction, originating from an ortho-phenyl H atom, stabilizes the packing arrangement. In addition, a weak C—H⋯π interaction, also involving an ortho-phenyl H atom, is observed. Full Article text
3 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
3 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
3 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
3 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
3 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
3 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
3 (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
3 [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
3 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
3 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
3 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
3 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
3 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
3 (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
3 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
3 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
3 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
3 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
3 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
3 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
3 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
3 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
3 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
3 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
3 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
3 [(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
3 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
3 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
3 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
3 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
3 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
3 [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