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In the title compound, C22H13ClN2, the quinoxaline ring system is close to planar [maximum deviation = 0.061 (2) Å]. The phenyl ring at the 2-position and the phenyl ring of the phenylethynyl substituent make dihedral angles of 49.32 (7) and 11.99 (7) °, respectively, with the quinoxaline mean plane. The two phenyl rings are inclined to one another by 61.27 (9)°. In the crystal, molecules are linked by C—H⋯π and π–π interactions [centroid–centroid distances = 3.6210 (12) and 3.8091 (12) Å].
doi:10.1107/S1600536812020776
PMCID: PMC3379328
PMID: 22719526
In the solid state, the title compound, C22H10N2S, forms centrosymmetric dimers by pairs of non-classical C—H⋯S hydrogen bonds linking approximately coplanar molecules. The benzene ring involved in this interaction makes a dihedral angle of only 7.21 (16)° with the thiophene ring, while the other benzene ring is twisted somewhat out of the plane, with a dihedral angle of 39.58 (9)°. The hydrogen-bonded dimers stack on top of each other with an interplanar spacing of 3.44 Å. C—H⋯N hydrogen bonds link together stacks that run in approximately perpendicular directions. Each molecule thus interacts with 12 adjacent molecules, five of them approaching closer than the sum of the van der Waals radii for the relevant atoms. Optimization of the inter-stack contacts contributes to the non-planarity of the molecule.
doi:10.1107/S1600536808008106
PMCID: PMC2961030
PMID: 21202153
In the centrosymmetric title compound, C64H62N4, the two phenylethynyl groups lie at diagonal meso positions. The 24-membered porphyrin has in-plane distortion with respect to the mean plane of the macrocycle and two intra-ring bifurcated N—H⋯(N,N) hydrogen bonds occur. The dihedral angles between the phenyl rings in the phenylethynyl group and the 3,5-bis(tert-butyl)phenyl group with respect to the mean plane of the porphyrin are 17.2 (2) and 59.2 (3)°. The tert-butyl groups are disordered over two sets of sites in a 0.661 (13):0.339 (13) ratio.
doi:10.1107/S1600536809045954
PMCID: PMC2972159
PMID: 21578743
The title compound, C26H22O4, is a derivative of 1,4-bis(phenylethynyl)benzene substituted by four methoxy groups at the terminal benzene rings. The asymmetric unit consists of two half-molecules; one centrosymmetric molecule is planar but the other is non-planar, with dihedral angles of 67.7 (1)° between the central benzene ring and the terminal benzene rings. In the crystal structure, molecules form a zigzag molecular network due to π–π [the interplanar and centroid–centroid distances between the benzene rings are 3.50 (1) and 3.57 (1) Å, respectively] and C—H⋯π interactions (2.75 Å). Introduction of the four methoxy groups results in the supramolecular architecture.
doi:10.1107/S1600536808013664
PMCID: PMC2961624
PMID: 21202588
The title compound, C26H22O4, is a derivative of 1,4-bis(phenylethynyl)benzene substituted by four methoxy groups on the terminal benzene rings. The molecule is almost planar with an r.m.s. deviation of 0.266 Å. The dihedral angles between the two terminal benzene rings and the central benzene ring are 7.96 (6) and 13.32 (7)°. In the crystal structure, molecules aggregate via C—H⋯O interactions, forming molecular tapes along the a axis, which aggregate to form a herring-bone structure.
doi:10.1107/S160053680900155X
PMCID: PMC2968219
PMID: 21581947
The structure of the title compound, C6H6O3, has been redetermined at low temperature [room-temperature structure: Maartmann-Moe (1965 ▶). Acta Cryst. 19, 155–157]. The molecule is planar with approximate D
3h point symmetry, yet it crystallizes in the chiral orthorhombic space group P212121 with a three-dimensional hydrogen-bonding network containing infinite O—H⋯O—H⋯O—H chains.
doi:10.1107/S1600536808030638
PMCID: PMC2959261
PMID: 21201217
The tellurium atom in the title bis-ethynyl telluride, Te(C9H7)2 or C18H14Te, is located on a crystallographic twofold axis, the C—Te—C angle being 92.23 (15)°. The dihedral angle between the rings is 87.27 (7)°. In the crystal structure, molecules are connected in chains parallel to the b axis and mediated by C—H⋯π interactions.
doi:10.1107/S1600536810006264
PMCID: PMC2983524
PMID: 21580428
In the structure of the title compound, [CoCl2(C9H16N2Si)2], the CoII atom is located on an inversion center in a slightly distorted tetrahedral environment formed by two chloride ions and the pyridine N atoms of two chelating 6-methyl-2-[(trimethylsilyl)amino]pyridine ligands. The dihedral angle between the planes of the pyridine rings is 80.06 (5)°. Cohesion within the crystal structure is accomplished by N—H⋯Cl hydrogen bonds.
doi:10.1107/S1600536809027937
PMCID: PMC2977306
PMID: 21583404
The molecular structure of the title compound, [Fe(C5H5)(C13H4F5)], consists of a ferrocenyl group and a 2,3,4,5,6-pentafluorobenzene group linked through an ethyne spacer. The crystal packing is dominated by intermolecular C—H⋯F hydrogen bonds, C—F⋯π interactions between the pentafluorobenzene groups [F⋯centroid distances = 3.882 (2) and 3.884 (2) Å] and π–π interactions between the pentafluorobenzene and cyclopentadienyl rings [centroid–centroid distance = 3.741 (1) Å].
doi:10.1107/S1600536810026772
PMCID: PMC3007523
PMID: 21588152
The asymmetric unit of the title compound, C26H16F6O2, contains one half of the molecule situated on an inversion centre. In the rod-like molecule, the two terminal benzene rings form a dihedral angle of 71.9 (1)° with the central benzene ring. The trifluoromethyl group is rotationally disordered over two orientations in a 0.53 (1):0.47 (1) ratio. The crystal packing exhibits no classical intermolecular interactions.
doi:10.1107/S160053681102099X
PMCID: PMC3151946
PMID: 21837009
The title compound, C18H23N2Si+·Cl−·H2O, was synthesized from 1-[(trimethylsilyl)methyl]benzimidazole and benzyl chloride in dimethylformamide. The benzimidazole ring system is approximately planar, with a maximum deviation of 0.022 (2) Å, and makes an angle of 74.80 (12)° with the phenyl ring. The crystal packing is stabilized by O—H⋯Cl, C—H⋯Cl, C—H⋯O and C—H⋯π interactions between symmetry-related molecules together with π–π stacking interactions between the imidazolium and benzene rings [centroid–centroid distance = 3.5690 (15) Å] and between the benzene rings [centroid–centroid distance = 3.7223 (14) Å].
doi:10.1107/S1600536810024128
PMCID: PMC3007035
PMID: 21587984
The molecular structure of the title compound, trans-[Cu(C2H)Cl(C26H24P2)2], consists of an RuII cation, located on an inversion centre, in an octahedral environment defined by two chelating phosphines, one acetylide and one chloride ligand. The –C CH and the chlorine ligands are disordered over two equivalent positions (0.5 occupancy each). The coordination geometry is distorted octahedral, with the –C CH fragment and the Cl ligand in trans positions. The four P atoms occupy the equatorial plane of the octahedron and the chloride and acetylide ligands the axial positions.
doi:10.1107/S1600536812044558
PMCID: PMC3588712
PMID: 23468677
The crystal structure of a previously unreported polymorph (form II) of 2,4-dinitrophenylhydrazine (DNPH), C6H6N4O4, was determined at 90 K. The first polymorph (form I) is described in the monoclinic space group P21/c [Okabe et al. (1993 ▶). Acta Cryst. C49, 1678–1680; Wardell et al. (2006 ▶). Acta Cryst. C62, o318–320], whereas form II is in the monoclinic space group Cc. The molecular structures in forms I and II are closely similar, with the nitro groups at the 2- and 4-positions being almost coplanar with the benzene ring [dihedral angles of 3.54 (1) and 3.38 (1)°, respectively in II]. However, their packing arrangements are completely different. Form I exhibits a herringbone packing motif, whereas form II displays a coplanar chain structure. Each chain in form II is connected to adjacent chains by the intermolecular interaction between hydrazine NH2 and 2-nitro groups, forming a sheet normal to (101). The sheet is stabilized by N—H⋯π interactions.
doi:10.1107/S1600536813004571
PMCID: PMC3588540
PMID: 23476598
The title compound, C16H6N6, is a polymorph of the previously reported structure [Kozlov & Goldberg (2008 ▶). Acta Cryst. C64, o498–o501]. Unlike the previously reported monoclinic polymorph (space group P21/c, Z = 8), the title compound reveals orthorhombic symmetry (space group Pnma, Z = 4). The molecule shows crystallographic mirror symmetry, while the previously reported structure exhibits two independent molecules per asymmetric unit. In the title compound, adjacent molecules are essentially parallel along the c axis and tend to be vertical along the b axis with dihedral angles of 72.02 (6)°. However, in the reported polymorph, the entire crystal structure shows an antiparallel arrangement of adjacent columns related by inversion centers and the two independent molecules are nearly parallel with a dihedral angle of 2.48 (6)°.
doi:10.1107/S1600536811047039
PMCID: PMC3238907
PMID: 22199760
The transamination reaction of (2-pyridylmethyl)(triisopropylsilyl)amine with bis{bis(trimethylsilyl)amido}zinc(II) yields the colorless title solvate, [Zn(C15H27N2Si)2]·0.5C7H8·0.25C4H8O. The title compound was crystallized from toluene and tetrahydrofuran. There are two independent molecules in the asymmetric unit. In each molecule, the Zn atom is tetrahedrally coordinated by four N atoms. The two molecules differ in the orientation of the isopropyl groups. The molecules show large N—Zn—N angles [143.0 (2) and 145.7 (2)° between the amide groups].
doi:10.1107/S160053680800888X
PMCID: PMC2961323
PMID: 21202207
The title compound, C6H5NO3, crystallizes in the triclinic system with six independent molecules in the asymmetric unit. In a previous study, the structure of the title compound was determined in the monoclinic P21/n space group at 100 K [Valerga et al. (2009 ▶). Acta Cryst. E65, o1979]. All six independent molecules display an E configuration about the C=C double bond, with the dihedral angles between the planes of the furan rings and the nitroalkenyl groups ranging from 0.61 (7) to 5.03 (7)°. The crystal structure is stabilized by intermolecular C—H⋯O hydrogen-bonding interactions.
doi:10.1107/S160053681002492X
PMCID: PMC3007394
PMID: 21588246
The crystal structure of the title compound, [Fe(C4H6)(CO)3], was previously reported by Mills & Robinson [Acta Cryst. (1963) ▶, 16, 758–761]. The compound crystallizes in the centrosymmetric space goup Pnma with the complex located on a mirror plane. The redetermination of this structure at 100 K yielded almost equilibrated C—C bond lengths within the butadiene ligand according to a metal-to-ligand bonding–back-bonding mechanism. The C—C bond lengths presented herein are significantly shorter than those reported earlier. The H-atom positions that have not been reported so far were located by difference Fourier maps. The positional parameters of all H atoms and individual U
iso values were refined freely.
doi:10.1107/S1600536810039218
PMCID: PMC3009352
PMID: 21588810
The title compound, C13H9N3O5, prepared as a solid derivative of 3-nitroanaline via reaction with 4-nitrobenzoyl chloride, crystallizes in a chiral space group. The molecule is non-planar with a dihedral angle of 26.1 (1)° between the two benzene rings. Both nitro groups are twisted slightly out of the plane of their corresponding benzene rings, making dihedral angles of 10.7 (4) and 13.5 (4)°. The molecules are stacked along the a axis with benzene ring centroid–centroid distances of 3.8878 (6) Å. In the crystal, intermolecular benzene C—H⋯O interactions involving one nitro group and the carbonyl group link the molecules, forming chains along [001]. An additional set of aromatic C—H⋯O interactions with the second nitro group form chains along [101], connecting adjacent chains to create layers perpendicular to the b axis.
doi:10.1107/S1600536811038062
PMCID: PMC3201324
PMID: 22065512
The title compound, [Fe(C8H5)(C22H16P)(C3H9P)3], was synthesized by the addition of phenylethine to a solution of the parent methyl iron complex Fe(CH3){P(C6H5)2(C10H6)}(PMe3)3 at 213 K, accompanied by evolution of methane. The coordination around the iron center can be described as slightly distorted octahedral [Fe—P 2.2485 (12)–2.2902 (12) Å; Fe—C 1.918 (5), 2.015 (4) Å], with a meridional arrangement of the trimethylphosphine ligands and the introduced terminal alkinyl-ligand trans to the P(Ph)2-anchoring group.
doi:10.1107/S1600536808041421
PMCID: PMC2967909
PMID: 21581538
The crystal structure of the title compound, [C(NH2)3]6[Mo7O24]·H2O, previously determined at room temperature in the monoclinic space group C2/c from Weissenberg techniques [Don & Weakley (1981 ▶). Acta Cryst. B37, 451–453], has been redetermined from low-temperature single-crystal data in the monoclinic space group P21/c. The asymmetric unit contains one heptamolybdate anion, six guanidinium cations and one water molecule of hydration. The anions and cations are linked by an extensive network of N—H⋯O hydrogen bonds.
doi:10.1107/S1600536808008234
PMCID: PMC2961279
PMID: 21202171
The title Schiff base compound, C21H26N2O4, is a second triclinic polymorph of a previously reported room-temperature structure [Jia (2009 ▶). Acta Cryst. E65, o646]. Strong intramolecular O—H⋯N hydrogen bonds generate S(6) ring motifs. Intermolecular C—H⋯O interactions link neighbouring molecules into dimers with an R
2
2(16) ring motif. The mean planes of the two benzene rings are almost perpendicular to each other, making a dihedral angle of 88.24 (5)°. An interesting feature of the crystal structure is the intermolecular short C⋯O [3.1878 (13) Å] contact which is shorter than the sum of the van der Waals radii of the relevant atoms. The crystal structure is further stabilized by intermolecular C—H⋯π and π–π interactions [centroid–centroid distance = 3.7414 (6) Å]. The structure has a stereogenic centre but the space group is centrosymmetric, so the molecule exists as a racemate.
doi:10.1107/S1600536809008137
PMCID: PMC2968989
PMID: 21582458
The structure of ortho-vanillin, C8H8O3, has been revisited with modern methods and at low temperature (100 K). The previous structure [Iwasaki et al. (1976 ▶). Acta Cryst. B32, 1264–1266] is confirmed, but geometric precision is improved by an order of magnitude. The C atom of the methoxy group lies close to the benzene ring plane, which is the most common geometry for –OMe groups lying ortho to –OH groups on an aromatic ring. The crystal structure displays one intramolecular O—H⋯O and three weak intermolecular C—H⋯O hydrogen bonds.
doi:10.1107/S1600536812029571
PMCID: PMC3414273
PMID: 22904806
The title compound, C15H22N2O3, was obtained as a by-product of oxidative cleavage of 1,3-dicyclohexyl-(3-oxo-2,3-dihydrobenzofuran-2-yl)imidazolidine-2,4-dione. Herein, we report the crystal structure of a second polymorph, which was obtained by crystallization from an ethanol solution at 253 K, instead of slow evaporation of the same solvent at room temperature. While the first polymorph [Talhi et al. (2011). Acta Cryst. E67, o3243] crystallized in the non-centrosymmetric space group P212121, this second polymorph crystallizes in the centrosymmetric space group P21/n. Compared to the first polymorph, in the crystal no C=O⋯C=O interactions were found (C⋯O intermolecular distance longer than 3.15 Å) and instead, close packing of individual molecular units is mediated by C—H⋯π and weak C—H⋯O interactions.
doi:10.1107/S1600536812043619
PMCID: PMC3515314
PMID: 23284534
The 1,3-dioxin-4-one ring in the title compound, C16H16O3, is in a half-boat conformation with the quaternary O—C(CH3)2—O atom lying 0.546 (1) Å out of the plane defined by the remaining five atoms. The crystal structure is consolidated by C—H⋯O contacts that lead to supramolecular layers.
doi:10.1107/S1600536809041002
PMCID: PMC2971386
PMID: 21578331
In the title compound, [Co(C13H9)(C28H20)], the Co atom is sandwiched between cyclopentadienyl and cyclobutadienyl rings that are inclined at a dihedral angle of 2.6 (3)°. The four phenyl rings are tilted with respect to the cyclobutadienyl plane so that the C4Ph4 unit constitutes a four-bladed propeller. The phenyl ring of the phenyl-alkyne substituent is inclined to the cyclopentadienyl ring at an angle of 34.92 (18)°. The crystal structure is stabilized solely by C—H⋯π interactions which generate a three-dimensional network.
doi:10.1107/S1600536811016928
PMCID: PMC3120504
PMID: 21754635