RESUMEN
3-Phenyl-2-(thio-phen-3-yl)-2,3-di-hydro-4H-pyrido[3,2-e][1,3]thia-zin-4-one (C17H12N2OS2, 1) and 2-(1H-indol-3-yl)-3-phenyl-2,3-di-hydro-4H-pyrido[3,2-e][1,3]thia-zin-4-one 0.438-hydrate (C21H15N3OS·0.438H2O, 2) crystallize in space groups P21/n and C2/c, respectively. The asymmetric unit in each case is comprised of two parent mol-ecules, albeit of mixed chirality in the case of 1 and of similar chirality in 2 with the enanti-omers occupying the neighboring asymmetric units. Structure 2 also has water mol-ecules (partial occupancies) that form continuous channels along the b -axis direction. The thia-zine rings in both structures exhibit an envelope conformation. Inter-molecular inter-actions in 1 are defined only by C-Hâ¯O and C-Hâ¯N hydrogen bonds between crystallographically independent mol-ecules. In 2, hydrogen bonds of the type N-Hâ¯O between independent mol-ecules and C-Hâ¯N(π) type, and π-π stacking inter-actions between the pyridine rings of symmetry-related mol-ecules are observed.
RESUMEN
In the title compound, C19H17NO5S, the cyclo-hexene ring adopts nearly an envelope conformation. In the crystal, mol-ecules are linked by C-Hâ¯O hydrogen bonds, forming a three-dimensional network. In addition, C-Hâ¯π inter-actions connect the mol-ecules by forming layers parallel to the (010) plane. According to the Hirshfeld surface analysis, Hâ¯H (36.9%), Oâ¯H/Hâ¯O (31.0%), Câ¯H/Hâ¯C (18.9%) and Sâ¯H/Hâ¯S (7.9%) inter-actions are the most significant contributors to the crystal packing.
RESUMEN
In the title compound, C15H13NO3S, the mol-ecular conformation is stable with the intra-molecular O-Hâ¯O hydrogen bond forming a S(7) ring motif. In the crystal, mol-ecules are connected by C-Hâ¯O hydrogen bonds, forming C(8) chains running along the a-axis direction. Cohesion of the packing is provided by weak van der Waals inter-actions between the chains. A Hirshfeld surface analysis was undertaken to investigate and qu-antify the inter-molecular inter-actions. The thio-phene ring is disordered in a 0.9466â (17):0.0534â (17) ratio over two positions rotated by 180°.
RESUMEN
In the title compound, C20H17BrO5S, mol-ecules are connected by inter-molecular C-Hâ¯S hydrogen bonds with R 2 2(10) ring motifs, forming ribbons along the b-axis direction. C-Hâ¯π inter-actions consolidate the ribbon structure while van der Waals forces between the ribbons ensure the cohesion of the crystal structure. According to a Hirshfeld surface analysis, Hâ¯H (40.5%), Oâ¯H/Hâ¯O (27.0%), Câ¯H/Hâ¯C (13.9%) and Brâ¯H/Hâ¯Br (11.7%) inter-actions are the most significant contributors to the crystal packing. The thio-phene ring and its adjacent di-carboxyl-ate group and the three adjacent carbon atoms of the central hexene ring to which they are attached were refined as disordered over two sets of sites having occupancies of 0.8378â (15) and 0.1622â (15). The thio-phene group is disordered by a rotation of 180° around one bond.
RESUMEN
In the title compound, C20H18N2S, the asymmetric unit comprises two similar mol-ecules (A and B). In mol-ecule A, the central thio-phene ring makes dihedral angles of 89.96â (12) and 57.39â (13)° with the 1H-pyrrole rings, which are bent at 83.22â (14)° relative to each other, and makes an angle of 85.98â (11)° with the phenyl ring. In mol-ecule B, the corresponding dihedral angles are 89.49â (13), 54.64â (12)°, 83.62â (14)° and 85.67â (11)°, respectively. In the crystal, mol-ecular pairs are bonded to each other by N-Hâ¯N inter-actions. N-Hâ¯π and C-Hâ¯π inter-actions further connect the mol-ecules, forming a three-dimensional network. A Hirshfeld surface analysis indicates that Hâ¯H (57.1% for mol-ecule A; 57.3% for mol-ecule B), Câ¯H/Hâ¯C (30.7% for mol-ecules A and B) and Sâ¯H/Hâ¯S (6.2% for mol-ecule A; 6.4% for mol-ecule B) inter-actions are the most important contributors to the crystal packing.
RESUMEN
In the title compounds, C22H16FNO2S2 (I) and C26H20FNO2S2 (II), the benzo-thio-phene rings are essentially planar with maximum deviations of 0.009â (1) and 0.001â (1)â Å for the carbon and sulfur atom in compounds I and II, respectively. In I, the thio-phene ring system is almost orthogonal to the phenyl ring attached to the sulfonyl group, with a dihedral angle of 77.7â (1)°. In compound I, the mol-ecular structure is stabilized by weak C-Hâ¯O intra-molecular inter-actions formed by the sulfone oxygen atoms, which generate two S(5) ring motifs. In the crystal of I, N-Hâ¯O hydrogen bonds link the mol-ecules into R 2 2(8) rings, which are connected into a C(10) chain via C-Hâ¯F hydrogen bonds. Inter-molecular C-Hâ¯π inter-actions are also observed. In compound II, the mol-ecules are linked via C-Hâ¯O and C-Hâ¯F hydrogen bonding, generating infinite C(11) and C(13) chains running parallel to [010].
RESUMEN
In the title compound, C19H15N5S, the thio-phene ring is disordered in a 0.6:0.4 ratio by an approximate 180° rotation of the ring around the C-C bond linking it to the pyridine ring. In the crystal, the mol-ecules are linked by N-Hâ¯N hydrogen bonds into dimers with an R 2 2(12) motif, forming chains along the b-axis direction. These chains are connected to each other by further N-Hâ¯N hydrogen bonds, forming a three-dimensional network. Furthermore, N-Hâ¯π and π-π [centroid-centroid separations = 3.899â (8) and 3.7938â (12)â Å] inter-actions also contribute to the crystal cohesion. A Hirshfeld surface analysis indicated that the most important contributions to the surface contacts are from Hâ¯H (46.1%), Nâ¯H/Hâ¯N (20.4%) and Câ¯H/Hâ¯C (17.4%) inter-actions.
RESUMEN
In both of the title compounds, C26H19NO2S2, (I), and C25H19NO2S2, (II), the benzo-thio-phene rings are essentially planar with maximum deviations of 0.026â (1) and -0.016â (1)â Å for the carbon and sulfur atoms in compounds (I) and (II), respectively. In (I), the thio-phene ring system is almost orthogonal to the phenyl ring attached to the sulfonyl group, subtending a dihedral angle of 88.1â (1)°, and the di-hydro-pyridine ring adopts a screw-boat conformation. In both compounds, the mol-ecular structure is consolidated by weak C-Hâ¯O intra-molecular inter-actions formed by the sulfone oxygen atoms, which generate S(5) ring motifs. In the crystal of II, mol-ecules are linked via C-Hâ¯O hydrogen bonds, generating C(7) chains running along the [100] direction. No significant inter-molecular inter-actions are observed in I.
RESUMEN
The title compounds, C15H14N2OS (1a), C16H16N2OS (1b), and C17H18N2OS (1c), form a homologous series in which the size of the saturated ring increases from six- to eight-membered (with four, five and six methyl-ene groups respectively). For 1b and 1c, the central (CH2) n moieties are all displaced to the same side of their ring, and the CH2-CH2-CH2 angles are much wider than the standard sp 3 value; a database search indicates that these are general features of such ring systems. For 1a, the thio-phene ring lies with the sulfur atom on the opposite side of the Cthio-phene-Cpyridine bond to the cyano group, in contrast to 1b and 1c. For each compound, the packing may be described in terms of two 'weak' C-Hâ¯N hydrogen bonds, which link the mol-ecules to form one-dimensional (1a, 1c) or three-dimensional (1b) assemblies.
RESUMEN
In the title compound, C32H29BrN2O10S3, the benzo-thia-zole and thio-phene ring systems subtend an inter-planar angle of 7.43â (12)°. The NH2 group forms intra-molecular hydrogen bonds to Nthia-zole and Ocarbon-yl. The Sgalactose-Cthio-phene bond is short [1.759â (2)â Å]. The mol-ecules are connected to form ribbons parallel to the b axis by two 'weak' hydrogen bonds and a short Naminoâ¯Sgalactose contact.
RESUMEN
The crystal structures of four thio-phene-carbohydrazide-pyridine derivatives, viz. N'-[(E)-pyridin-3-yl-methyl-idene]thio-phene-2-carbohydrazide, C11H9N3OS, (I), N'-[(E)-pyridin-2-yl-methyl-idene]thio-phene-2-carbohydrazide, C11H9N3OS, (II), N-methyl-N'-[(E)-pyridin-2-yl-methyl-idene]thio-phene-2-carbohydrazide, C12H11N3OS, (III) and N'-[(E)-pyridin-2-yl-methyl-idene]-2-(thio-phen-2-yl)ethano-hydrazide, C12H11N3OS, (IV) are described. The dihedral angles between the thio-phene ring and the pyridine ring are 21.4â (2), 15.42â (14), 4.97â (8) and 83.52â (13)° for (I)-(IV), respectively. The thio-phene ring in (IV) is disordered over two orientations in a 0.851â (2):0.149â (2) ratio. Key features of the packing include N-Hâ¯Np (p = pyridine) hydrogen bonds in (I), which generate C(7) chains propagating in the [001] direction; N-Hâ¯Np links also feature in (II), but in this case they lead to C(6) [001] chains; in (IV), classical amide (C4) N-Hâ¯O links result in [010] chains; in every case adjacent mol-ecules in the chains are related by 21 screw axes. There are no classical hydrogen bonds in the extended structure of (III). Various weak C-Hâ¯X (X = O, N, S) inter-actions occur in each structure, but no aromatic π-π stacking is evident. The Hirshfeld surfaces and fingerprint plots for (I)-(IV) are compared.
RESUMEN
The polymeric title compound, [Cu2Br2(C4H8S)2] n , CP1, represents an example of a two-dimensional coordination polymer resulting from reaction of CuBr with tetra-hydro-thio-phene (THT) in MeCN solution. The two-dimensional layers consist of two different types of rhomboid-shaped dinuclear Cu(µ2-Br)2Cu secondary building units (SBUs); one with a quite loose Cuâ¯Cu separation of 3.3348â (10)â Å and a second one with a much closer inter-metallic contact of 2.9044â (9)â Å. These SBUs are inter-connected through bridging THT ligands, in which the S atom acts as a four-electron donor bridging each Cu(µ2-Br)2Cu unit in a µ2-bonding mode. In the crystal, the layers are linked by very weak C-H⯷Br hydrogen bonds with Hâ¯Br distances of 2.95â Å, thus giving rise to a three-dimensional supra-molecular network.
RESUMEN
The synthesis and spectroscopic data of (E)-2-{4-[3-(thio-phen-3-yl)acrylo-yl]phen-oxy}acetic acid are described. Crystallization from an ethanol-water mixture resulted in the title compound, C30H23KO8S2 or [K(C15H11O4S)(C15H12O4S)] n , containing one mol-ecule of the acid and one mol-ecule of the potassium salt in the asymmetric unit. Both mol-ecules share the H atom between their carboxyl groups and a potassium ion. The C=C bonds display an E configuration. The thio-phene and phenyl rings in the two mol-ecules are inclined by 43.3â (2) and 22.7â (2)°. The potassium ion is octa-hedrally coordinated by six O atoms. This distorted octa-hedron shares on opposite sides two oxygen atoms with inversion-related octa-hedra, resulting in chains of octa-hedra running in the [010] direction, which form ladder-like chains by C-Hâ¯π inter-actions. A Hirshfeld surface analysis indicates that the highest contributions to the surface contacts arise from inter-actions in which H atoms are involved, with the most important contribution being from Hâ¯H (31.6 and 31.9% for the two mol-ecules) inter-actions.
RESUMEN
The title compound, C12H9N3O4S, synthesized by condensation of 5-nitro-thio-phene-2-carbaldehyde and 2-methyl-3-nitro-aniline, crystallizes in the ortho-rhom-bic space group P212121. In the mol-ecule, the aromatic benzene and thio-phene rings are twisted with respect to each other, making a dihedral angle of 23.16â (7)°. In the crystal, mol-ecules are linked by inter-molecular C-Hâ¯O hydrogen bonds into chains extending along the c-axis direction. Weak π-π stacking inter-actions along the a-axis direction provide additional stabilization of the crystal structure. The roles of the various inter-molecular inter-actions were clarified by Hirshfeld surface analysis, which reveals that the crystal packing is dominated by Oâ¯H (39%) and Hâ¯H (21.3%) contacts. The crystal studied was refined as a two-component inversion twin.
RESUMEN
The title compound, C8H11NO2S, crystallizes with two mol-ecules, A and B, in the asymmetric unit. Each molecule features an intramolecular N-Hâ¯O hydrogen bond and the same H atom is also involved in an intermolecular N-Hâ¯S bond to generate A + B dimers. Further N-Hâ¯O hydrogen bonds link the dimers into a [010] chain.
RESUMEN
The title complex, Cu(L)2 or [Cu(C15HF10O2)2], comprised of one copper ion and two fully fluorinated ligands (L -), was crystallized with 3,4-ethyl-ene-dioxy-thio-phene (EDOT, C6H6O2S) as a guest mol-ecule to give in a di-chloro-methane solution a unique co-crystal, Cu(L)2·3C6H6O2S. In the crystal, the oxygen of one guest mol-ecule, EDOT-1, is coordinated to the metal to give an alternate linear arrangement, and the π-planes of the others, EDOT-2 and EDOT-3, inter-act weakly with the penta-fluoro-phenyl groups of the complex through arene-perfluoro-arene inter-actions. Head-to-tail columnar and head-to-head dimeric arrangements are observed for EDOT-2 and EDOT-3, respectively, in the crystal. The Hirshfeld surface analysis indicated that the most important contributions for the crystal packing are from the Fâ¯F (20.4%), Fâ¯H/Hâ¯F (24.5%) and Fâ¯C/Câ¯F (9.6%) inter-actions. The density functional theory (DFT) optimized structure at the ωB97X-D 6-31G* level was compared with the experimentally determined mol-ecular structure in the solid state.
RESUMEN
The title crystal structure is assembled from the superposition of two mol-ecular structures, (E)-1-(5-chloro-thio-phen-2-yl)-3-(3-methyl-thio-phen-2-yl)prop-2-en-1-one, C12H9ClOS2 (93%), and (Z)-1-(5-chloro-thio-phen-2-yl)-3-(3-methyl-thio-phen-2-yl)prop-1-en-1-ol, C12H11ClOS2 (7%), 0.93C12H9ClOS2·0.07C12H11ClOS2. Both were obtained from the reaction of 3-methyl-thio-phene-2-carbaldehyde and 1-(5-chloro-thio-phen-2-yl)ethanone. In the extended structure of the major chalcone component, mol-ecules are linked by a combination of C-Hâ¯O/S, Clâ¯Cl, Clâ¯π and π-π inter-actions, leading to a compact three-dimensional supra-molecular assembly.
RESUMEN
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 35.16â (5)° and 24.94â (3)°.
RESUMEN
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 = 3.29â (9)°], the other makes an angle of 83.96â (4)°.
RESUMEN
Benzo[1,2-c:3,4-c':5,6-c'']tri-thio-phene (D 3h -BTT) is an easily prepared electron donor that readily forms charge-transfer complexes with organic acceptors. We report here two crystal structures of its charge-transfer complexes with 7,7,8,8-tetra-cyano-quinodi-methane (TCNQ) and buckminsterfullerene (C60). The D 3h -BTT·TCNQ complex, C12H6S3·C12H4N4, crystallizes with mixed layers of donors and acceptors, with an estimated degree of charge transfer at 0.09 e. In the D 3h -BTT·C60·toluene complex, C12H6S3·C60·C7H8, the central ring of BTT is 'squeezed' by the C60 mol-ecules from both faces. However, the degree of charge transfer is low. The C60 unit is disordered over two sites in a 0.766â (3):0.234â (3) ratio and was refined as a two-component inversion twin.