One of the methyl groups and the 4-methoxyphenyl substituent are in axial positions and the chloro(4-methoxyphenyl)methyl substituent is in the equatorial position of the cyclohexane ring which adopts a chair conformation. The packing features inversion-symmetric dimeric units and strands along [100] and [010] established by weak C—H⋯O and C—H⋯Cl contacts. 23H25ClO4, the cyclohexane ring adopts a chair conformation with the 4-methoxyphenyl substituent in an axial position and the chloro(4-methoxyphenyl)methyl substituent in an equatorial position. The packing features inversion dimers formed by pairs of C—H⋯O contacts and strands along [100] and [010] established by further C—H⋯O and C—H⋯Cl contacts, respectively.In the title compound, C The crude product was recrystallized from diethyl ether/pentane (1:1 v/v) affording the title compound .Zinc chloride , tetrabutylammonium chloride , diethyl ether (0.10 ml) and phenyliodonium-4,4-dimethylcyclohexane-2,6-dione  were dissolved in dichloromethane (6 ml) and cooled to 195 K. Then 4,4′-dimethoxybenzhydryl chloride  in dichloromethane (4 ml) was added dropwise. The reaction solution was stirred at 195 K for 2 h. The resulting mixture was quenched with 2 2, 1.00 Å for aliphatic C—H, 0.95 Å for aromatic H) and treated as riding on their parent atoms, with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(C) for methyl H atoms. The methyl groups were allowed to rotate along the C—C bonds to best fit the experimental electron density.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989016002085/rz5184sup1.cifCrystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989016002085/rz5184Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989016002085/rz5184Isup3.cmlSupporting information file. DOI: 1451618CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the crystal, the anions are linked  7H11N2+·2C7H4NO4−·3H2O, crystallized with two anions and two cations in the asymmetric unit, together with three water molecules. Both 4-dimethylaminopyridinium cations are protonated at their pyridine N atoms with the plane of the N(CH3)2 hetero atoms inclined to the pyridine ring by 4.5 (2) and 1.4 (2)°. In the 2-nitrobenzoate anions, the carboxyl and nitro groups are inclined to their respective benzene rings by 77.1 (3) and 20.0 (3)°, and 75.8 (2) and 20.9 (3)°. In the crystal, the anions are linked via O—H⋯O hydrogen bonds involving the water molecules, forming chains along [100]. The cations are linked to these chains by N—H⋯O hydrogen bonds. The chains are linked via C—H⋯O hydrogen bonds and C—H⋯π and π–π interactions [inter-centroid distances range from 3.617 (1) to 3.851 (1) Å], forming a three-dimensional structure.The title salt, 2C In the 2-nitrobenzoate anions the carboxyl groups (O3/O4/C15 and O5/O6/C28) are inclined to the respective benzene rings (C16–C21 and C22–C27) by 77.1 (3) and 75.8 (2)°. The nitro groups (O1/O2/N5 and O7/O8/N6) are inclined to their respective benzene rings by 20.0 (3) and 20.9 (3)°.The asymmetric unit of the title salt consists of two 4-dimethylaminopyrdinium cations and two 2-nitrobenzoate anions, together with three water molecules Fig. 1. The geovia O—H⋯O hydrogen bonds involving the water molecules, forming chains along [100]; Table 1via C—H⋯O hydrogen bonds and C—H⋯π and π–π interactions, forming a three-dimensional structure .In the crystal, the dihedral angle between the two pyridine rings (N1/C1–C5 and N2/C8–C12) is 5.16 (9)°, while the benzene rings (C16–C21 and C22–C27) form a dihedral angle of 19.56 (9)°. The anions are linked et al., 2000A search of the Cambridge Structural Database  and 2-nitrobenzoic acid  were dissolved in 50 ml of hot ethanol as a solvent. The mixture was stirred well for 8 h to give a homogeneous solution and is was then allowed to evaporate in air at room temperature. Within a few days, small colourless block-like crystals of the title salt were formed.Uiso(H) = 1.5Ueq(O) for the water H atoms. The C-bound H atoms were positioned geometrically and refined using a riding model: C—H = 0.93–0.96 Å with Uiso(H) = 1.5Ueq(C) for methyl H atoms and = 1.2Ueq(C) for other H atoms.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S1600536814020583/su2777sup1.cifCrystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536814020583/su2777Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S1600536814020583/su2777Isup3.cmlSupporting information file. DOI: 1024182CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


N-phenyl ring being inclined to the central p-phenylenediamine ring by 29.34 (4) and 43.43 (7)°, respectively. In the crystal, molecules are linked by a number of weak N—H⋯π, C—H⋯π and π–π interactions [inter-centroid distances = 3.5569 (11)–3.708 (1) Å], forming slabs lying parallel to  and the terminal N-phenyl ring are 29.34 (4) and 43.43 (7)°, respectively. The conformation about the C=N bond is E. In the crystal, molecules are linked by N—H⋯π and C—H⋯π interactions forming chains propagating along the [10-2] direction. These chains are linked via π–π interactions [inter-centroid distances are in the range 3.5569 (11)–3.708 (1) Å], forming slabs lying parallel to (30-4).In the title compound, C Interaction Cg6⋯Cg6ii is a slipped parallel π–π interaction with an interplanar distance of 3.3614 (7) Å and a slippage of 1.163 Å.In the crystal, molecules are connected N-phenyl-p-phenylenediamine gave three hits. Of these three compounds, N1-phenyl-N4-(quinolin-2-ylmethylene)benzene-1,4-diamine {synonym: N-phenyl-4-[(quinolin-2-ylmethylene)amino]aniline; WOJJIQ; Faizi et al., 2014A search of the Cambridge Structural Database  of pyrene-1-carbaldehyde in 5 ml of absolute ethanol was added dropwise under stirring. The mixture was stirred for 10 min, two drops of glacial acetic acid were then added and the mixture was further refluxed for 2h. The resulting yellow precipitate was recovered by filtration, washed several times with small portions of ice-cold ethanol and then with diethyl ether to give 150 mg (87%) of the title compound. Yellow block-like crystals suitable for X-ray analysis were obtained within 3 days by slow evaporation of a solution in MeOH.80 mg (0.435 mmol) of Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989015001814/su5072sup1.cifCrystal structure: contains datablock(s) global, I. DOI: 10.1107/S2056989015001814/su5072Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989015001814/su5072Isup3.cmlSupporting information file. DOI: 1045835CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The thiophene and hydroxy-substitiuted rings form dihedral angles of 23.43 (9) and 35.45 (9)°, respectively, with the benzothiadiazole ring system. An intramolecular O—H⋯N hydrogen bond is observed. In the crystal, weak C—H⋯O hydrogen bonds and π–π stacking interactions [centroid–centroid distance = 3.880 (3) Å] link molecules into chains along [100]. In addition, there are short S⋯S contacts [3.532 (3) Å] which link these chains, forming a two-dimensional network parallel to (010).In the title molecule, C DOI: 10.1107/S1600536814014883/lh5710Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S1600536814014883/lh5710Isup3.cmlSupporting information file. DOI: 1010080CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the crystal, molecules are linked by weak intra- and intermolecular C—H⋯O and C—H⋯π interactions, forming chains along the  50H46N2O4)], crystallizes in the triclinic space group P-1, with two molecules in the asymmetric unit (Z′ = 2). Each NiII atom has a slightly distorted square-planar geometry [ω = 3.91 (5)° and 2.04 (7)°] defined by the two phenolate O and two imine N atoms of the tetradentate Schiff base ligand. The dihedral angles between the central phenolate ring and peripheral phenyl rings are 60.5 (2)/70.0 (2) and 86.4 (2)/56.1 (2)° in molecule A, and 89.43 (19)/18.0 (2) and 63.87 (19)/68.2 (2)° in molecule B. The two central phenolate rings are twisted by angles of 19.37 (19) and 19.36 (18)° in the two molecules. The packing is stabilized through intra- and intermolecular C—H⋯O and C—H⋯π interactions, forming chains parallel to the b axis. The tert-butyl groups in one of the two molecules are positionally disordered with a refined occupancy ratio of 0.707 (13):0.293 (13).The mononuclear title complex, [Ni(C The molecular structure of one of the independent molecules is shown in Fig. 1II atom is coordinated by a tetradentate dianionic ligand involving two phenolato O and two imine N atoms. The coordination geometry around the metal atom is slightly distorted square planar [β = 88.44 (16) and 88.55 (15)°  and ω = 3.8 (4) and 2.2 (4)° (the angle between the coordination planes Ni1–N1A–O1A and Ni1–N2A–O2A in A and Ni2–N1B–O1B and Ni2–N2B–O2B in B) for Ni1 and Ni2, respectively  and 0.006 (3) Å, respectively. Atoms C25 and C26 in A and B are significantly out of plane, as indicated by the N—C—C—N torsion angles, −32.9 (7)° in A and −40.5 (3)° in B. The dihedral angles between the central phenolato ring  and the peripheral phenyl rings  are 60.5 (2) & 70.0 (2)° and 86.4 (2) & 56.1 (2)° in molecule A and 89.43 (19) & 18.0 (2)° and 63.87 (19) & 68.2 (2)° in molecule B. The two central phenolato rings (C1A–C6A & C34A–C39A and C1B–C6B & C34B–C39B) are twisted by angles of 19.37 (19) and 19.36 (18)°, respectively, in the two molecules.The mononuclear title complex crystallizes in the triclinic space group b axis by weak intermolecular C—H⋯O and C—H⋯π interactions  was added dropwise to the stirred hot solution of the tetradentate Schiff base, LH2  in ethanol under argon. The resulting wine-red solution was heated to reflux at 343–353 K. The clear solution thus obtained was filtered and allowed to cool to ambient temperature. Slow evaporation of the solvent resulted in red–brown irregular plate-shaped crystals within a few days . Analysis calculated for C50H46N2O4Ni (%): C 75.29, H 5.81. Found: C 75.40, H 5.60.An ethanolic solution of NiClUiso(H) = 1.5Ueq(C) for methyl H atoms and = 1.2Ueq(C) for other H atoms. The refined occupancy ratios for the disordered t-butyl groups are 0.707 (13):0.293 (13) for atoms C8A/C9A/C10A and C8C/C9C/C10C in molecule A. The ISOR restraint and EADP constraint commands in the SHELXL2014 software were used for the disordered atoms. There are voids in the structure of 348 Å3 due to the packing of the molecules but when these were checked using the SQUEEZE routine  I. DOI: 10.1107/S2056989015021052/zl2639Isup2.hklStructure factors: contains datablock(s) I. DOI: 1435344CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


A. reticulata, crystallizes with two independent molecules (A and B) in the asymmetric unit. The two molecules differ essentially in the orientation of the propenyl group at the 2-position with respect to the mean plane of the furanocoumarin moiety. In the crystal, the two molecules are linked via O—H⋯O hydrogen bonds forming zigzag –A–B–A–B– chains propagating along [001].The title furanocoumarin, isolated from the Indian herb  14H12O4 chromen-7-one], crystallizes with two independent molecules (A and B) in the asymmetric unit. The two molecules differ essentially in the orientation of the propenyl group with respect to the mean plane of the furanocoumarin moiety; the O—C(H)—C=C torsion angle is 122.2 (7)° in molecule A and −10.8 (11)° in molecule B. In the crystal, the A and B molecules are linked via O—H⋯O hydrogen bonds, forming zigzag –A–B–A–B– chains propagating along [001]. The chains are reinforced by bifurcated C—H⋯ hydrogen bonds, forming ribbons which are linked via C—H⋯π and π–π interactions [intercentroid distance = 3.602 (2) Å], forming a three-dimensional structure.The title furanocoumarin, C A. reticulata, by column chromatography over silica gel with a mixture of binary solvent hexane and ethyl acetate by gradient elution. Furanocoumarins, such as oroselone chromen-2-one], whose atomic connectivity has been established by spectrometric and spectroscopic analyses  in the asymmetric unit. The compound is composed of three fused rings  with hydroxyl and propenyl substituents at positions 9 and 2, respectively. The furanocoumarin moieties are essentially planar with r.m.s. deviations of 0.05 Å for molecule A (O1/O2/C1–C11) and 0.079 Å for molecule B (O5/O6/C16–C25). The furan ring in molecule A has an envelope conformation with atom C2 as the flap, deviating by 0.120 (4) Å from the mean plane of the furanocoumarin moiety. In molecule B, the furan ring has a twisted conformation on bond C17–C16 with atoms C16 and C17 deviating by −0.232 (6) and 0.076 (6) Å, respectively, from the other atoms of the twisted five-membered ring. The two molecules differ essentially in the orientation of the propenyl group with respect to the mean plane of the furanocoumarin moiety, as shown by AutoMolFit analysis  ° in molecule B. The bond distances and bond angles in the propenyl side chains  also differ in the two molecules , the circular dichroism (CD) spectrum was measured in a solution of chloroform at concentration of 1 mg/ml using a cell with path length 1 cm. This CD measurement revealed that the absolute configuration of atom C2  is S.The absolute structure of the molecule in the crystal could not be determined by resonant scattering. In order to determine the chirality at atom C2  Å, interplanar distance = 3.4168 (2) Å, slippage 1.284 Å, where Cg2 and Cg9 are the centroids of rings C1/C4–C8 and C15/C18–C22, respectively; symmetry code: (i) − x + 1, y + z].In the crystal, the viz. 2,3-dihydro-9-hydroxy-2-(1-hydroxy-1-methylethyl)-7H-furo(1) benzopyran-7-one monohydrate  at room temperature by slow evaporation of the solvents (m.p. 498 K). 1H NMR data  7.60 , 6.85 , 6.20 , 5.35 , 5.11 , 4.94 , 3.47–3.34 ,3.16–3.04 , 1.78 . EIMS (70 ev) data: m/z (%) 244(15.9) [M+], 226 (68.6) , 185 (30),171 (16.8), 155 (30.1), 140 (16.4), 127 (13.5), 115 , 75 (22.3), 63 (26.5), 41 (16.0).The title compound was isolated as a colourless solid from the methanol extract of Uiso(H) = 1.2Ueq(O). The C-bound H atoms were included in calculated positions and treated as riding atoms: C—H = 0.93–0.98 Å with Uiso(H) = 1.2Ueq(C). The limited number of Friedel pairs measured were merged for refinement.Crystal data, data collection and structure refinement details are summarized in Table 310.1107/S2056989016003303/su5279sup1.cifCrystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989016003303/su5279Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989016003303/su5279Isup3.cmlSupporting information file. DOI: 1422810CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The crystal structure of tris(dimethylamido)bis(dimethylamine) zirconium(IV) iodide is reported. 2H6N)3(C2H7N)2]I. The bond lengths and bond angles are consistent with a slightly distorted trigonal–bipyramidal coordination geometry around the metal atom. N⋯I contacts of 3.6153 (15) and 3.5922 (14) Å are consistent with the presence of N—H⋯I interactions. These N—H⋯I interactions link the complex cations and iodide anions into extended chains that propagate parallel to the a axis.Zirconium amides have become increasingly popular and useful due to their widespread use as precursors to other zirconium complexes and their use in the production of solid oxide fuel cells (SOFCs). Herein we report the molecular structure of tris(dimethylamido)bis(dimethylamine)zirconium(IV) iodide, [Zr(C Additionally, many zirconium amide complexes are precatalysts for hydroamination/cyclization of unactivated aminoalkenes  and 3.5922 (14) Å are consistent with the presence of N—H⋯I interactions Table 1. The ‘twet al., 1988The synthesis or crystal structure of tris(dimethylamido)bis(dimethylamine)zirconium(IV) iodide has not been reported as of 22 April 2015 based on a comprehensive WebCSD and Scifinder Scholar search. Similar compounds have been characterized crystallographically, for example tetrakis(dimethylamido)zirconium(IV) and its lithium dimethylamido adduct phenylene](dimethylamido)diiodidozirconium(IV) and 2-bis(dimethylamido)iodidozirconium(IV) had crystallized in the form of needles, which were not suitable for single-crystal X-ray diffraction. However, a suitable tablet-shaped crystal of tris(dimethylamido)bis(dimethylammine)zirconium(IV) iodide was selected, mounted, and analyzed.1,3-Bis(3′-hexylimidazol-1′-yl)benzene diiodide , tetrakis(dimethylamido)zirconium(IV)  and dry toluene (2.8 mL) were combined in an inert atmosphere of Ar and heated at 383 K for 5 min in a sealed screw-cap vial. While heating, the reaction mixture became homogeneous. Upon cooling to room temperature, an oil formed. The top layer was removed and the oil was washed with toluene (3 × 3 mL). The toluene washings were combined and allowed to sit at room temperature. Colorless crystals formed after 2 months. The mother liquor was decanted and the crystals were covered with paratone oil after using a few crystals for Uiso(H) = 1.5Ueq(C) or 1.2Ueq(N).Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989015023919/pk2563sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S2056989015023919/pk2563Isup2.hklStructure factors: contains datablock(s) I. DOI: 1037746CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the title compound compound, the phenyl and pyrimidine rings are inclined to one another at 31.72 (6)°. The residues are associated into ribbons parallel to [110] by three classical hydrogen bonds. Adjacent ribbons are connected by translation parallel to the  12H10BrN5O3S2·C3H7NO, displays an almost planar amine group. The interplanar angle between the rings is 31.72 (6)°. The residues are associated into ribbons parallel to [110] by three classical hydrogen bonds; one from each amine Hamine to ODMF and one from NHamide to Ooxo. Adjacent ribbons are connected by translation parallel to the c axis by a ‘weak’ hydrogen bond Hmethyl⋯Osulfonyl to form a layer structure parallel to (1-10), while a further contact Hbromophenyl⋯Osulfonyl connects the residues in the third dimension.The title compound, C N-cyanoimido-S,S-dimethyl-dithiocarbonate and other ketene dithioacetals for synthesizing new classes of antimetabolites -6-oxopyrimidin-1(6H)-yl)-4-bromobenzenesulfonamide (I)N-cyanodithioiminocarbonate with N′-(4-bromophenyl)sulfonyl-2-cyanoethanehydrazide. The chemical nature was proposed on the basis of elemental analysis and spectroscopic data and its X-ray structure determination was undertaken to confirm the nature of the product. We have recently presented the structure of a related pyrimidine ·DMF, is shown in Fig. 1x, −y, 1 − z) and H03⋯O4, involve the dimethylformamide oxygen atom and lead to the formation of inversion-symmetric rings of graph set x, 1 − y, 1 − z), also forms inversion-symmetric rings, but of graph set The components are associated into ribbons parallel to [110] Fig. 2 by threeB⋯O3 connects neighbouring ribbons by translation parallel to the c axis, thus completing a layer structure parallel to .There are two short and acceptably linear C—H⋯O contacts that may be assumed to represent ‘weak’ hydrogen bonds; H7x, 2 − y,1 − z) and a weak hydrogen bond of 3.05 Å from H17, with an angle of 124° at hydrogen. These interactions also connect the residues in the third dimension.The bromine atom is involved in two secondary contacts: a halogen bond of 3.4582 (10) Å with O1 was added to a stirred solution of N′-(4-bromophenyl)sulfonyl-2-cyanoethanehydrazide (0.01 mol) in dry dioxane (50 mL) containing potassium hydroxide (0.01 mol) at room temperature. The reaction mixture was stirred for 30 min at room temperature; the precipitated solid was collected by filtration and crystallized from dimethyl formamide to give pale yellow crystals, m.p. 483–485 K, yield 85%.Dimethyl Uiso(H) = 1.5Ueq(C) for methyl H atoms and 1.2Ueq(C) for other H atoms].Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989015018903/lh5790sup1.cifCrystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989015018903/lh5790Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989015018903/lh5790Isup3.cmlSupporting information file. DOI: 1430044CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


O—H⋯O hydrogen bonds between water molecules and ClO4 units lead to the formation of a three-dimensional network in each of the structures.The crystal structures of the tri-, tetra- and nonahydrate phases of Sr(ClO 4)2(H2O)3]n}, strontium perchlorate tetrahydrate {di-μ-aqua-bis(triaquadiperchloratostrontium), [Sr2(ClO4)4(H2O)8]} and strontium perchlorate nonahydrate {heptaaquadiperchloratostrontium dihydrate, [Sr(ClO4)2(H2O)7]·2H2O}, were crystallized at low temperatures according to the solid–liquid phase diagram. The structures of the tri- and tetrahydrate consist of Sr2+ cations coordinated by five water molecules and four O atoms of four perchlorate tetrahedra in a distorted tricapped trigonal–prismatic coordination mode. The asymmetric unit of the trihydrate contains two formula units. Two [SrO9] polyhedra in the trihydrate are connected by sharing water molecules and thus forming chains parallel to [100]. In the tetrahydrate, dimers of two [SrO9] polyhedra connected by two sharing water molecules are formed. The structure of the nonahydrate contains one Sr2+ cation coordinated by seven water molecules and by two O atoms of two perchlorate tetrahedra (point group symmetry ..m), forming a tricapped trigonal prism (point group symmetry m2m). The structure contains additional non-coordinating water molecules, which are located on twofold rotation axes. O—H⋯O hydrogen bonds between the water molecules as donor and ClO4 tetrahedra and water molecules as acceptor groups lead to the formation of a three-dimensional network in each of the three structures.The title compounds, strontium perchlorate trihydrate {di-μ-aqua-aquadi-μ-perchlorato-strontium, [Sr(ClO Thereby, the trigonal base planes are chosen such that each oxygen atom of the perchlorate anions represents a capping atom. The third cap is provided by a water oxygen atom.The crystal structure of strontium perchlorate trihydrate contains two crystallographically distinct Srra Fig. 1. Four of0] Fig. 2. The cry0] Fig. 2 or mercunt Fig. 3b. There2+ cations 7] coordination polyhedra and two towards perchlorate tetrahedra 7] polyhedra additionally are linked via other O—H⋯O hydrogen bonds. The resulting arrangement can be seen in a larger section of the structure . O—H⋯O hydrogen bonds also dominate the crystal packing in the two other structures, in each case leading to the formation of a three-dimensional network 2·3H2O phases, see: Gallucci & Gerkin (1988M = Ba); Hennings et al. (2014aM(ClO4)2·4H2O phases, see: Robertson & Bish 2·3H2O were used as purchased . The isolated crystals were stored in a freezer separated and embedded in perfluorinated ether to avoid contact with humidity. Sr(ClO4)2·4H2O crystallized from an aqueous solution of 75.08 wt% Sr(ClO4)2 at 273 K after two days and Sr(ClO4)2·9H2O from an aqueous solution of 60.12 wt% Sr(ClO4)2 at 238 K after one week. For preparing these aqueous solutions, strontium perchlorate trihydrate was used. The Sr2+ content was analyzed per complexometric titration with EDTA. The crystals are stable in the saturated aqueous solutions over a range of at least four weeks. The samples were stored in a freezer or a cryostat at low temperatures and were separated and embedded in perfluorinated ether for X-ray analysis.Crystals of Sr(ClO4)2·3H2O and Sr(ClO4)2·4H2O distance restraints were applied for all water molecules, with O—H and H—H distance restraints of 0.84 (1) and 1.4 (1) Å, respectively. For Sr(ClO4)2·9H2O Uiso values were set at 1.2Ueq(O) using a riding model approximation. Distance restraints were applied for that structure for all water molecules, with O—H and H—H distance restraints of 0.84 (1) and 1.4 (1) Å, respectively.Crystal data, data collection and structure refinement details are summarized in Table 410.1107/S1600536814024726/wm5080sup1.cifCrystal structure: contains datablock(s) SrClO4_3H2O_100K, SrClO4_4H2O_150K, SrClO4_9H2O_100K. DOI: 10.1107/S1600536814024726/wm5080SrClO4_3H2O_100Ksup2.hklStructure factors: contains datablock(s) SrClO4_3H2O_100K. DOI: 10.1107/S1600536814024726/wm5080SrClO4_4H2O_150Ksup3.hklStructure factors: contains datablock(s) SrClO4_4H2O_150K. DOI: 10.1107/S1600536814024726/wm5080SrClO4_9H2O_100Ksup4.hklStructure factors: contains datablock(s) SrClO4_9H2O_100K. DOI: Click here for additional data file.10.1107/S1600536814024726/wm5080SrClO4_3H2O_100Ksup5.cmlSupporting information file. DOI: Click here for additional data file.10.1107/S1600536814024726/wm5080SrClO4_4H2O_150Ksup6.cmlSupporting information file. DOI: Click here for additional data file.10.1107/S1600536814024726/wm5080SrClO4_9H2O_100Ksup7.cmlSupporting information file. DOI: 1033590, 1033589, 1033588CCDC references:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The asymmetric unit comprises two independent molecules. In the crystal, the two independent molecules are linked by bifurcated N—H⋯O hydrogen bonds, forming a supramolecular chain with a  16H17N3O2S, there are two independent molecules (A and B), which show an E conformation with respect to the C=N bond. An intramolecular O—H⋯N hydrogen bond with an S(6) motif stabilizes the molecular structure. The terminal phenyl and benzene rings are almost orthogonal to each other, the dihedral angle being 87.47 (13)° for molecule A and 89.86 (17)° for molecule B. In the crystal, weak bifurcated N—H⋯ hydrogen bonds link the two independent molecules, forming a supramolecular chain with a C21(14)[R21(5)] motif along the b axis. A weak C—H⋯O interaction is also observed in the chain.In the asymmetric unit of the title compound, C The hydrazine carbothioamide backbone is nearly planar with a maximum deviation of 0.023 (2) Å at atom N2 for molecule A and of 0.054 (2) Å at atom N2′ for B. The closeness of the C=S bond lengths [C9—S1 = 1.666 (2) Å and C9′—S1′ = 1.657 (2) Å] to the expected distance  and longer than corresponding double bonds ° for B. In each molecule (A and B), an intramolecular O—H⋯N interaction (Table 1S(6) ring motif stabilizes the molecular structure  x, −1 + y, z] with b axis. An intermolecular C—H⋯O interaction is also observed within the chain -4-methyl-4-phenyl-1-(2-pyridylmethylene)-3-thiosemicarbazide  indicate some degree of delocalization in the compounds. The C=S bond lengths in all compared compounds lie in the range 1.66–1.67 Å, intermediate between S—Csp2 and S=Csp2 bond lengths , showing a partial double-bond character. Similar bond lengths for the C=S bond have also been observed in hydrazine carbothioamide derivatives  of 2-hydroxy-3-methoxybenzaldehyde in 10 ml of ethanol over a period of 10 min with continuous stirring. The reaction mixture was refluxed for 2 h and allowed to cool whereby a shining yellow compound began to separate. This was filtered and washed thoroughly with ethanol and then dried in vacuum. The compound was recrystallized from a hot ethanol solution, giving colourless block-like crystals (yield 91%). Single crystals suitable for X-ray diffraction were prepared by slow evaporation of an ethanol solution at room temperature.1.81 g (0.01 mol) of Uiso(H) = 1.2Ueq(C) for aromatic and 1.5Ueq(C) for methyl groups. The rotation angles for methyl groups were optimized.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989016005326/is5446sup1.cifCrystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989016005326/is5446Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989016005326/is5446Isup3.cmlSupporting information file. DOI: 1435114CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


II cation is located on a centre of inversion and exhibits a slightly distorted octahedral arrangement of water molecules. The noncoordinating water molecules and dimethylammonium cations connect the sulfate and [Ni(H2O)6]2+ octahedra via O—H⋯O and N—H⋯O hydrogen bonds into a three-dimensional framework.In the salt bis(dimethylammonium) hexaaquanickelate(II) bis(sulfate) dihydrate, the Ni 2H8N)2[Ni(H2O)6)](SO4)2·2H2O, the NiII cation is located on a centre of inversion and exhibits a slightly distorted octahedral arrangement of water molecules. The Ni—O bond lengths in the complex [Ni(H2O)6]2+ cation show a distribution as in the related Tutton salt (NH4)2[Ni(H2O)6](SO4)2, but are longer in average [2.056 (13) versus 2.037 (12) Å]. The noncoordinating water molecules and dimethylammonium cations connect the sulfate and [Ni(H2O)6]2+ octahedra via O—H⋯O and N—H⋯O hydrogen bonds from weak up to medium strength into a three-dimensional framework whereby the complex metal cations and sulfate anions are arranged in sheets parallel (001).In the title salt, (C The NiII cation reaches an overall bond valence sum 6]2+ octahedra. Together with relatively weaker N—H⋯O hydrogen bonds of the ammonium H atoms to sulfate anions, a three-dimensional framework is formed with pronounced formation of sheets of complex metal cations and sulfate anions parallel (001) (Table 1Hydrogen bonds of weak up to medium strength involving coordinating and noncoordinating water molecules as donor groups and O atoms of the sulfate anions as acceptor groups interconnect neighbouring [Ni(H) Table 1.−1) in a stoichiometric ratio of 1:2:1. The resulting solution was kept at room temperature by cooling. The title compound crystallized by slow evaporation of the solvent at room temperature in form of light-green crystals with dimensions up to 4 mm within 12 weeks.The title compound was obtained by reaction of an aqueous solution of nickel(II) sulfate with dimethylamine and sulfuric acid (18 mol lUiso(H) = 1.5Ueq(C) for methyl H atoms, and N—H = 0.90 Å and Uiso(H) = 1.2Ueq(N) for ammonium H atoms. The H atoms of water molecules were refined with a distance restraint of O—H = 0.98 Å and individual Uiso values for each H atom.Details of structure refinement are given in Table 210.1107/S160053681402234X/wm5074sup1.cifCrystal structure: contains datablock(s) I, global. DOI: 10.1107/S160053681402234X/wm5074Isup2.hklStructure factors: contains datablock(s) I. DOI: 1028557CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the crystal, molecules are connected by N—H⋯O hydrogen bonds generating –A–B–A–B– zigzag chains extending along [010]. The chains are linked via C—H⋯π interactions and π–π interactions [with a centroid–centroid distance of 3.444 (3) Å)] between the benzene ring and the imino group of symmetry-related molecules, forming slabs lying parallel to (100).The title compound, C 23H25N3O, crystallized with one single molecule in the asymmetric unit and is present in the zwitterionic form. There is an intramolecular N—H⋯O hydrogen bond in the molecule with the phenol ring being inclined to the central benzene ring by 20.67 (14)°. The terminal aminophenyl ring forms a dihedral angle of 54.21 (14)° with the central benzene ring. The two outer aromatic rings are inclined to one another by 74.54 (14)°. In the crystal, the molecules are connected by N—H⋯O hydrogen bonds, with adjacent molecules related by a 21 screw axis, generating –A–B–A–B– zigzag chains extending along [010]. The chains are linked via C—H⋯π and π–π interactions [with a centroid–centroid distance of 3.444 (3) Å] between the benzene ring and the imino group of symmetry-related molecules, forming slabs lying parallel to (100).The title compound, C It is well known that Schiff bases of salicylaldehyde derivative may exhibit thermochromism or photochromism, depending on the planarity or non-planarity of the molecule, respectively  with respect to the central benzene ring (C12–C17); the dihedral angle between them is 54.21 (14)°. The two outer aromatic rings (C18–C23 and C1–C6) are inclined to one another by 74.54 (14)°. The C—N, C=N and C—C bond lengths are normal and close to the values observed in related structures ; see Table 1Cg1⋯Cg2i = 3.444 (3) Å, where Cg1 and Cg2 are the centroids of atoms C1–C6 and the midpoint of atoms N2/C11, respectively -N′-phenylbenzene-1,4-diamine  of 4-diethylamino-2-hydroxybenzaldehyde in 5 ml of absolute ethanol was dropwisely added under stirring. This mixture was stirred for 10 min, two drops of glacial acetic acid were then added and the mixture was further refluxed for 2 h. The resulting yellow precipitate was recovered by filtration, washed several times with a small portions of EtOH and then with diethyl ether to give 150 mg (88%) of 5-diethylamino-2-[(E)-{[4-(phenylamino)phenyl]iminomethyl}phenol] (DPIM). Crystals of the title compound suitable for X-ray analysis were obtained within three days by slow evaporation of the DMF solvent.100 mg (1 mmol) of Uiso(H) = 1.2–1.5Ueq(C).Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989015019490/lh5793sup1.cifCrystal structure: contains datablock(s) global, I. DOI: 10.1107/S2056989015019490/lh5793Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989015019490/lh5793Isup3.cmlSupporting information file. DOI: 1431311CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


Three closely related methylated hydrazine carbamates show different hydrogen-bonding patterns, although they all result in chains. l-serine are presented, namely benzyl N-{(E)-1-[2-(4-cyanobenzylidene)-1-methylhydrazinyl]-3-hydroxy-1-oxopropan-2-yl}carbamate, C20H20N4O4, tert-butyl N-{(E)-1-[2-(4-cyanobenzylidene)-1-methylhydrazinyl]-3-hydroxy-1-oxopropan-2-yl}carbamate, C17H22N4O4, and tert-butyl N-[(E)-1-(2-benzylidene-1-methylhydrazinyl)-3-hydroxy-1-oxopropan-2-yl]carbamate, C16H23N3O4. One of them shows that an unexpected racemization has occurred during the mild-condition methylation reaction. In each crystal structure, the molecules are linked into chains by O—H⋯O hydrogen bonds, but with significant differences between them.The crystal structures of three methylated hydrazine carbamate derivatives prepared by multi-step syntheses from  The C9—N2 bond length of 1.358 (6)Å is typical of an amide and the N1—N2 bond length of 1.374 (5) is shorter than the reference value of 1.40 Å for a nominal N(sp2)—N(sp2) single bond. This suggests at least some electronic conjugation over the almost planar C7/N1/N2/C9/O1 grouping (r.m.s. deviation = 0.010 Å): the C1 benzene ring is twisted by 6.1 (2)° with respect to these atoms. The C7—N1—N2—C8 torsion angle of −1.9 (6)° shows that the carbon atoms are almost eclipsed with respect to the N—N bond whereas the C9—C10—C11—O2 torsion angle of −50.9 (5)° indicates a gauche conformation about the C10—C11 bond. The C9—C10—N3—H3A torsion angle is 38° and the separation between H2A (bonded to O2) and H3A is 2.5 Å.The molecular structure of (I)S) was assumed to be the same as that of the corresponding atom in the l-serine starting material. In terms of the C7/N1/N2/C9/O1 grouping in (II)A and H3 is 2.7 Å. These values are evidently sufficiently different from the corresponding data for (I)The molecular structure of (II)S configuration. The O2—H2 hydroxy group is disordered over two orientations in a 0.802 (7):0.198 (7) ratio. The geometric parameters for (III)A (major disorder component) torsion angle is −54.9 (4)°. The C9—C10—C11—O2B torsion angle for the minor disorder component is −156.7 (8)°, which has a significant role to play in the hydrogen-bonding pattern in the crystal of (III)Compound (III)A⋯O4i  and much longer N3—H3A⋯O4i hydrogen bonds (Table 1C(7) O—H⋯O and C(4) N—H⋯O chains. A pair of weak C—H⋯π interactions are also observed but there is no aromatic π–π stacking (shortest centroid–centroid separation > 4.7 Å).In the extended structure of (I)s Table 1 to the sC(7) O2—H2A⋯O4i  hydrogen bonds (Table 2i to not form an intermolecular hydrogen bond (H3⋯O4i = 3.2 Å), but instead forms an intramolecular link to O1. A very long intermolecular C—H⋯N interaction is observed but there is no π–π stacking in (II)The extended structure of (II)s Table 2 with alm1 screw axis, so that the C1-benzene ring is ‘flipped’ from one side of the chain to the other in adjacent molecules. As noted above, the hydroxyl group is disordered over two orientations. The hydrogen bond from the major orientation of O2A—H2A is still a bond to O4i  forms an O—H⋯O hydrogen bond in the opposite chain direction to O1ii : O1 also accepts an intramolecular N—H⋯O hydrogen bond, as seen in (II)The packing in the centrosymmetric structure of (III)i Table 3, where i2OH)CON(CH3)N=CH– fragments reported in Version 5.36 of the Cambridge Structural Database CONHN=CH– groupings with different substituents at each end of the fragment, all of which have been reported by us in the last few years -(S)-ROCONHCH(CH2OH)CONHN=CH-benzene compound  was added to a solution of the appropriate , b = 13.003 (19), c = 22.94 (3) Å, α = 92.93 (2), β = 91.48 (3), γ = 98.13 (3)°, V = 2804 (7) Å3]. An atomic model could be developed in space group P1 with Z = 6, but a PLATON ]. The C-bound H atoms were placed geometrically (C—H = 0.95–1.00 Å) and refined as riding atoms. The constraint Uiso(H) = 1.2Ueq(carrier) or 1.5Ueq(methyl carrier) was applied in all cases. The H atoms of the hydroxyl groups were allowed to rotate about their C—O bond (SHELXL HFIX 83 instruction with O—H = 0.84 Å and C—O—H = 109.5°) to best fit the electron density. The methyl groups were allowed to rotate, but not to tip, to best fit the electron density (AFIX 137 instruction).Crystal data, data collection and structure refinement details are summarized in Table 410.1107/S2056989015010440/hg5443sup1.cifCrystal structure: contains datablock(s) I, II, III, global. DOI: 10.1107/S2056989015010440/hg5443Isup2.hklStructure factors: contains datablock(s) I. DOI: 10.1107/S2056989015010440/hg5443IIsup3.hklStructure factors: contains datablock(s) II. DOI: 10.1107/S2056989015010440/hg5443IIIsup4.hklStructure factors: contains datablock(s) III. DOI: Click here for additional data file.10.1107/S2056989015010440/hg5443Isup5.cmlSupporting information file. DOI: Click here for additional data file.10.1107/S2056989015010440/hg5443IIsup6.cmlSupporting information file. DOI: Click here for additional data file.10.1107/S2056989015010440/hg5443IIIsup7.cmlSupporting information file. DOI: 1404006, 1404005, 1404004CCDC references:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


These represent the chiral atropoisomers distinguished by the mutual arrangement of the two acetyl–hydrazone groups with a cis conformation of the C=N bonds. The two cyclopentadienyl (Cp) rings are planar and nearly parallel, the tilt between the two rings being 3.16 (16)° [4.40 (18)° for the second independent molecule]. The conformation of the Cp rings is close to eclipsed, the twist angle being 0.1 (2)° [3.3 (2)°]. The two acetyl–hydrazone substituents are also planar and are inclined at 13.99 (15)/9.17 (16)° [6.83 (17)/14.59 (15)°] relative to the Cp rings. The Fe—C bond lengths range from 2.035 (3) to 2.065 (2) Å, with an average of 2.050 (3) Å , which agrees well with those reported for most ferrocene derivatives. In the crystal, the molecules form dimers via two strong N—H⋯N hydrogen bonds. The dimers are linked into a three-dimensional framework by weak N—H⋯N hydrogen bonds.The title compound, [Fe(C DOI: 10.1107/S1600536814014366/rk2429Isup2.hklStructure factors: contains datablock(s) I. DOI: 1009066CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The CoII atoms are linked by the oxalate anions into a chain running parallel to [100]. The chains are linked by the BPMO ligands into a three-dimensional architecture. In addition, N—H⋯O hydrogen bonds stabilize the crystal packing.In the polymeric title compound, [Co(C DOI: 10.1107/S1600536814015608/bt6986Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S1600536814015608/bt6986fig1.tifx y z x y z x y z x y z . DOI: x + 1, −y, − z + 1; (ii) −x, −y, − z + 1; (iii) x, − y + z + x + 1, − y + z − A view of the molecule of (I). Displacement ellipsoids are drawn at the 30% probability level. (i) − Click here for additional data file.10.1107/S1600536814015608/bt6986fig2.tif. DOI: View of the three-dimensional structure of (I).1012047CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


II cations that are linked by thiocyanato anions into chains which are further connected into layers by intermolecular N—H⋯O and O—H⋯S hydrogen bonding via additional methanol molecules.The crystal structure of the title compound consists of Cd 2(C6H6N2S)]·2CH3OH}n, consists of one cadmium(II) cation that is located on a centre of inversion as well as one thiocyanate anion, one pyridine-4-carbothioamide ligand and one methanol molecule in general positions. The CdII cations are octahedrally coordinated by the pyridine N atom of two pyridine-4-carbothioamide ligands and by the S and N atoms of four thiocyanate anions and are linked into chains along [010] by pairs of anionic ligands. These chains are further linked into layers extending along (201) by intermolecular N—H⋯O and O—H⋯S hydrogen bonds. One of the amino H atoms of the pyridine-4-carbothioamide ligand is hydrogen-bonded to the O atom of a methanol molecule, and a symmetry-related methanol molecule is the donor group to the S atom of another pyridine-4-carbothioamide ligand whereby each of the pyridine-4-carbothioamide ligands forms two pairs of centrosymmetric N—H⋯S and O—H⋯S hydrogen bonds. The methanol molecules are equally disordered over two orientations.The asymmetric unit of the polymeric title compound, {[Cd(NCS) The CdII cation is sixfold coordinated by two N-bonding pyridinethioamide ligands as well as two N- and two S-coordinating thiocyanate anions in an all trans distorted octahedral environment nt Fig. 1. As expent Fig. 1. The CdI0] Fig. 2. The metvia the methanol solvent molecules  by intermolecular N—H⋯O and O—H⋯S hydrogen bonding es Fig. 3. Each pyes Fig. 3. The hydes Fig. 3. This aret al., 2014According to the Cambridge Structural Database 2·3H2O were purchased from Alfa Aesar. Cd(NCS)2 was synthesized by stirring 17.5 g (57.0 mmol) Ba(NCS)2·3H2O and 14.6 g (57.0 mmol) CdSO4·3/8H2O in 300 ml water at room temperature for 3 h. The white residue of BaSO4 was filtered off and the resulting solution dried at 353 K. The homogeneity of the product was checked by X-ray powder diffraction and elemental analysis. The title compound was obtained by reaction of 11.4 mg Cd(NCS)2 (0.05 mmol) with 27.6 mg pyridine-4-carbothioamide (0.2 mmol) in boiling methanol (2 ml). Crystals suitable for single-crystal x-ray diffraction formed after cooling.CdSOUiso(H) = 1.2Ueq (1.5 for methyl and O—H hydrogen atoms) using a riding model with C—H = 0.95 Å for aromatic, C—H = 0.98 Å for methyl, N—H = 0.88 Å and O—H = 0.84 Å, respectively. The methanol molecule is equally disordered over two orientations and was refined using a split model using SAME restraints  I, New_Global_Publ_Block. DOI: 10.1107/S2056989016002632/wm5271Isup2.hklStructure factors: contains datablock(s) I. DOI: 1453442CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


S-benzyl-β-N-(2-hydroxyphenylethylidene)dithiocarbazate groups, connected through an S—S single bond. The two moieties are twisted with a dihedral angle of 87.88 (4)° between the S2C=N planes.The title molecule consists of two Schiff base moieties, namely two  32H30N4O2S4, consists of two Schiff base moieties, namely two S-benzyl-β-N-(2-hydroxyphenylethylidene)dithiocarbazate groups, which are connected through an S—S single bond. These two moieties are twisted with respect to each other, with a dihedral angle of 87.88 (4)° between the S2C=N planes. A bifurcated intramolecular O—H⋯ hydrogen bond is observed in each moiety. In the crystal, molecules are linked by pairs of C—H⋯O hydrogen bonds into inversion dimers. The dimers are further stacked in a column along the b axis through weak C—H⋯π interactions.The title compound, C S-benzyldithiocarbazate (SBDTC) . The (iminoethyl)phenol fragments (C1–C8/O1/N1 and C25–C32/O2/N4) are essentially planar with maximum deviations of 0.0559 (12) Å for N1 and 0.0200 (11) Å for N4 and make dihedral angles of 18.17 (4) and 17.49 (4)° with the N2/S1/S2/C9 and N3/S3/S4/C17 planes, respectively. The C—S distances  of 1.7461 (12)–1.8220 (13) Å are comparable to the values for the most similar dithiocarbazate derivatives dithiocarbazate was prepared by Pramanik et al. , was prepared according to the literature method . The prepared compound (0.17 g) was dissolved in acetonitrile (20 ml) on warming and mixed with ethanol (10 ml). Light-yellow platelet single crystals of the title compound (m.p. 386–387 K) suitable for X-ray study were obtained after 17 days along with colorless needle-shaped crystalline solids (m.p. 413–418 K).The ligand precursor, Uiso(H) = 1.2Ueq.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989016002371/is5440sup1.cifCrystal structure: contains datablock(s) General, I. DOI: 10.1107/S2056989016002371/is5440Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989016002371/is5440Isup3.cmlSupporting information file. DOI: 1452193CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


R stereochemical configuration. No head-to-tail hydrogen bonding is observed in the crystal packing, as is the case in estrone and other derivatives.A new ferrocene complex, 16-ferrocenylmethyl-3β-hydroxyestra-1,3,5(10)-trien-17-one, has been synthesized and structurally characterized by single-crystal X-ray diffraction techniques. The ferrocenylmethyl group is positioned at the β face of the estrone moiety; as a result, a new stereogenic center is formed leading to an  5H5)(C24H27O2)]·C2H6OS, has been synthesized and structurally characterized by single-crystal X-ray diffraction techniques. The molecule crystallizes in the space group P21 with one molecule of dimethyl sulfoxide. A hydrogen bond links the phenol group and the dimethyl sulfoxide O atom, with an O⋯O distance of 2.655 (5) Å. The ferrocene group is positioned in the β face of the estrone moiety, with an O—C—C—C torsion angle of 44.1 (5)°, and the carbonyl bond length of the hormone moiety is 1.216 (5) Å, typical of a C=O double bond. The average Fe—C bond length of the substituted Cp ring [Fe—C(Cp*)] is similar to that of the unsubstituted one [Fe—C(Cp)], i.e. 2.048 (3) versus 2.040 (12) Å. The structure of the complex is compared with those of estrone and ethoxymethylestrone.A new ferrocene complex, 16-ferrocenylmethyl-3β-hydroxyestra-1,3,5(10)-trien-17-one dimethyl sulfoxide monosolvate, [Fe(C In this context, we present herein the synthesis and crystal structure of 16-ferrocenylmethyl-3β-hydroxyestra-1,3,5(10)-trien-17-one dimethyl sulfoxide monosolvate (2) and compare it with the structure of estrogen (1) and 16β-ethoxymethylestrone (3)  Å, which is very similar to in estrogen and 16β-ethoxymethylestrone , corresponding to a carbon–oxygen double (C=O) bond. However, the substitution at C16 of the steroid in 2 and 3, ferrocenylmethyl and ethoxymethyl groups, respectively, makes torsion angles and bond angles at the 16-position slightly different. Both substituents are located on the beta face but, the torsion angle (between C19 and carbonyl group) defined as C19–C16—C17—O2 in 2 is smaller than in 3 (between the carbonyl and the methoxy groups), 44.1 (5) and 49.7 (2)°, respectively. The ferrocene moiety is positioned at 112.6 (3)° from C16 (∠C20—C19—C16) while the ethoxymethyl group is at 108.4 (1)° (∠C16—C1—O3). The average Fe—C bond length of the substituted Cp ring [Fe—C vs 2.040 (12) Å  as mobile phase, affording 67% of 2 as a yellow solid. Yellow rod-shaped crystals were obtained after dissolving the solid 16-ferrocenylmethyl-3β-hydroxyestra-1,3,5(10)-trien-17-one in a solution of CH2Cl2 with a few drops of dimethyl sulfoxide, to assure a concentrate solution, layered in hexane.In a 500 mL Parr bottle, 16-ferrocenylidene-3β-hydroxyestra-1,3,5(10)-trien-17-one complex was dissolved in a mixture of tetrahydrofuran (THF) and ethanol (1:1) and Pd/C . The system was purged three times with Hd(C—H) = 0.95 Å, Uiso(H) = 1.2Ueq(C); d(C—H2) = 0.99 Å,Uiso(H) = 1.2 Ueq (C); d(C—H3) = 0.98 Å, Uiso(H) = 1.5Ueq(C).Crystal data, data collection and structure refinement details are summarized in Table 310.1107/S2056989016008446/bg2586sup1.cifCrystal structure: contains datablock(s) I. DOI: 1479699CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The 5-fluorocytosine and melamine molecules interact via N—H⋯O, N—H⋯N and N—H⋯O, N—H⋯N, C—H⋯F hydrogen bonds.The asymmetric unit of the title compound comprises two independent 5-fluorocytosine molecules and one half-molecule of melamine. The 5-fluorocytosine molecules are linked through two different homosynthons; one is formed  4H4FN3O·C3H6N6, comprises of two independent 5-fluorocytosine (5FC) molecules (A and B) and one half-molecule of melamine (M). The other half of the melamine molecule is generated by a twofold axis. 5FC molecules A and B are linked through two different homosynthons [R22(8) ring motif]; one is formed via a pair of N—H⋯O hydrogen bonds and the second via a pair of N—H⋯N hydrogen bonds. In addition to this pairing, the O atoms of 5FC molecules A and B interact with the N2 amino group on both sides of the melamine molecule, forming a DDAA array of quadruple hydrogen bonds and generating a supramolecular pattern. The 5FC (molecules A and B) and two melamine molecules interact via N—H⋯O, N—H⋯N and N—H⋯O, N—H⋯N, C—H⋯F hydrogen bonds forming R66(24) and R44(15) ring motifs. The crystal structure is further strengthened by C—H⋯F, C—F⋯π and π–π stacking interactions.The asymmetric unit of the title compound, 4C The twofold axis of melamine coincides with the crystallographic twofold axis. An ORTEP view of the crystal structure is shown in Fig. 1A and 1.3492 (18) Å in 5FC B and the corresponding internal angles at the carbon-carrying fluorine atom [C2A—N3A—C4A = 119.96 (13) in 5FC A and C2B—N3B—C4B = 119.92 (13)° in 5FC B] agree with those reported in the literature  molecules  are involved in the generation of a quadruple hydrogen-bonded DDAA array having a fused-ring sequence of via N—H⋯O and N—H⋯N hydrogen bonds. These quadruple arrays are further linked by three large ring motifs: A molecules, two 5FC B molecules and two melamine molecules through several N—H⋯O and N—H⋯N hydrogen bonds, generating a hexameric supermolecule. The A molecule, two 5FC B molecules and one melamine molecule through N—H⋯O, N—H⋯N and C—H⋯F hydrogen bonds, generating a tetrameric supermolecule. Similarly, the A molecules, one 5FC B molecule and one melamine molecule through N—H⋯O, N—H⋯N and C—H⋯F hydrogen bonds, generating another tetrameric supermolecule. The association of these DDAA array and A and B molecules with an interplanar distance of 3.475 (6) Å, centroid-to-centroid distance of 3.6875 (11) Å, and slip angle of 19.52°. The crystal structure is further strengthened by a C—F⋯π interaction [3.4541 (14) Å] between 5-fluorocytosinium molecule A and the melamine molecule  while the melamine molecule interacts with them via N—H⋯O and N—H⋯N hydrogen bonds, generating the supramolecular architecture.In this co-crystal, 5FC molecules et al., 1982et al., 2009et al., 2013abet al., 2012et al., 2013et al., 2001et al., 2014abet al., 2005et al., 2007The crystal structure of 5-fluorocytosine monohydrate (Louis Hot aqueous solutions of 5-fluorocytosine (32 mg) and melamine (31 mg) were mixed in a 1:1 molar ratio. The resulting solution was warmed to 353 K using a water bath for half an hour and kept at room temperature for crystallization. After one week, colourless crystals were obtained.A, N4B) groups were located in a difference Fourier map and refined freely. The other hydrogen atoms were positioned geometrically  and were refined using a riding model with Uiso(H) = 1.2Ueq(parent atom).Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S205698901600476X/hg5470sup1.cifCrystal structure: contains datablock(s) global, I. DOI: 10.1107/S205698901600476X/hg5470Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S205698901600476X/hg5470Isup3.cmlSupporting information file. DOI: 1469709CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


The asymmetric unit is completed by one-half of the 2-({4-[(carboxylatomethyl)carbamoyl]phenyl}formamido)acetate dianion, which is located on a centre of inversion, and by three water molecules. Two [Co(CO3)(C10H8N2)2]+ cations are connected through C—H⋯O contacts by the uncoordinating anions. The aromatic rings of the 2,2′-bipyridine ligands and diacetate anions are involved in π–π stacking and C—H⋯π interactions. The centroid–centroid distances are in the range 3.4898 (4)–3.6384 (5) Å. The crystal structure is stabilized by further O—H⋯O and N—H⋯O hydrogen bonds, which give rise to a three-dimensional supramolecular network.The complex cation of the title compound, [Co(CO DOI: 10.1107/S160053681400631X/wm5010Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S160053681400631X/wm5010Isup3.cdxSupporting information file. DOI: 992984CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


Its geometry is different from saturated peptides but is in excellent agreement with other dehydroalanine compounds. In the crystal, an N—H⋯O hydrogen bond links the molecules in a herringbone packing arrangement.In the crystal structure of the dehydrodipeptide (Boc-Phe-ΔAla-OiPr), the molecule has a  20H28N2O5), the molecule has a trans conformation of the N-methylamide group. The geometry of the dehydroalanine moiety is to some extent different from those usually found in simple peptides, indicating conjugation between the H2C=C group and the peptide bond. The bond angles around dehydroalanine have unusually high values due to the steric hindrance, the same interaction influencing the slight distortion from planarity of the dehydroalanine. The molecule is stabilized by intramolecular interactions between the isopropyl group and the N atoms of the peptide main chain. In the crystal, an N—H⋯O hydrogen bond links the molecules into ribbons, giving a herringbone head-to-head packing arrangement extending along the [100] direction. In the stacks, the molecules are linked by weak C—H⋯O hydrogen-bonding associations.In the title compound, the dehydrodipeptide (Boc–Phe–ΔAla–OiPr, C The unsaturated amino acid is introduced into the structure of these polycyclic peptides by post-translational modification of selected serine and threonine residues -phenylalanyldehydroalanine isopropyl ester and its structure determination by single-crystal X-ray crystallographic methods are presented.Dehydropeptides are a class of compounds containing at least one residue of an α,β-dehydroamino acid. These compounds are of interest in many fields of science because of their structural and chemical properties. Dehydroamino acids are found in natural products (Bonauer N-(tert-butoxycarbonyl)phenylalanyldehydroalanine isopropyl ester  is shown in Fig. 1trans-conformation of the N-methylamide group. The geometry of the dehydroalanine is to some extent different from those usually found in simple peptides glycine , C17—N19—C20 = 126.8 (2) and O18—C17—N19 = 123.5 (2)°] due to the steric hindrance between atoms C21 and O18. The same interaction influences the slight distortion from planarity of the dehydroalanine moiety. The ω, ϕ and ψ torsion angles  of the dehydroalanine residue are −166.9 (2), 175.1 (2) and 178.0 (2)°. The geometries of the phenylaniline and the protecting groups are normal. There are four intramolecular C—H⋯O close contacts but three of them have a D—H⋯A angle of less than 120°.The molecular structure of i hydrogen bonds  of Boc–Phe–ΔAla was dissolved in 5 ml of methanol and calcium carbonate 0.329 g (1 mM) was added. The mixture was stirred for one h at room temperature, after which the solvent was evaporated. The residue was dissolved in 7 ml of DMF and isopropyl iodide  was added in portions to the stirred mixture at room temperature during the reaction, the progress of which was monitored by thin-layer chromatography, using 5% methanol in chloroform as eluent. After completion of the reaction, the solvent was evaporated and the oily residue was dissolved in ethyl acetate and washed consecutively with: 1 M HCl, saturated KHCO3, 0.1 M Na2S2O3 and brine. The organic layer was dried over anhydrous MgSO4 and the title compound was obtained in 81% yield (m.p. = 367–369 K). Recrystallization was performed using mixture of diethyl ether and hexane.The dehydrodipeptide was obtained by condensation of  al. 2008. For thi1H NMR  δ 1.26 , 1.30 , 2.76 , 3.02 , 4.27–4.39 , 5.01 , 5.70 , 6.23 , 7.15–7.36 , δ 9.30 . 13C NMR  δ 21.43, 28.10, 36.63, 56.34, 69.40, 78.41, 108.65, 126.29, 128.07, 129.25, 132.71, 138.03, 155.53, 162.81, 171.53. IR  3600–2800 broad (H-bonding), 1715 (C=Oester), 1700 (C=Ourethane), 1690 IAB (C=Oamide), 1632 (C=C), 1526 IIAB (C–N and N–H), 1317 (CO–N–C=and N–(C=C)–CO), 1196 and 1166 (C–O–C), 896 (=CH2).Uiso (H) = 1.2Ueq(N), C—Haromatic = 0.95 Å and Uiso (H) = 1.2Ueq(C), C—Hmethyl = 0.98 Å and Uiso (H) = 1.5Ueq(C); C—Hmethylene = 0.99 Å or C—Hmethine = 0.95 Å and Uiso (H) = 1.2Ueq(C). Although not definitive, the absolute structure factor  configuration, was −0.1 (6) for 1095 Friedel pairs.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S1600536814025197/zs2321sup1.cifCrystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536814025197/zs2321Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S1600536814025197/zs2321Isup3.cmlSupporting information file. DOI: 1034604CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


Packing in the title keto ester compound is dominated by the formation of inversion dimers by both non-classical hydrogen bonds and offset π–π stacking interactions. 15H10BrClO3, was synthesized in a single-step reaction by condensation of 3-bromobenzoic acid with 2-bromo-1-(4-chlorophenyl)ethanone in dimethylformamide in the presence of triethylamine as a catalyst. The structure consists of an aryl ketone moiety linked to an aryl ester unit by a methylene group. Both units are reasonably planar  and are almost orthogonal, with an angle of 88.60 (3)° between them. In the crystal, molecules form five separate sets of inversion dimers. Three of these are generated by two C—H⋯O interactions and a C—H⋯Br contact, and form chains along c and along the ab cell diagonal. In addition, two inversion-related π–π stacking interactions between like aryl rings again form chains of molecules but in this instance along the bc diagonal. These contacts generate infinite layers of molecules parallel to (011) and stack the molecules along the a-axis direction.2-(4-Chlorophenyl)-2-oxoethyl 3-bromobenzoate, C There is an r.m.s. deviation of 0.119 Å from the best-fit plane through atoms Br1, C1–C8, O1, O2 [maximum deviation 0.2477 (11) Å for O1] while the plane of the carboxylate unit subtends an angle of 15.5 (2)° to that of the bromobenzene ring. In addition, the plane of the aryl ketone unit C8–C15, O3, Cl1 has an r.m.s. deviation of 0.010 Å [maximum deviation 0.0171 (15) Å for C15]. The aryl ketone and aryl ester planes are almost orthogonal with an angle of 88.61 (3)° between them. Bond lengths and angles in the molecule are normal and are generally similar to those found in closely related molecules  Å, and neighbouring 4-chlorophenyl rings Cg2⋯Cg2v = 3.8585 (11) Å, in this case along the bc diagonal, Fig. 3Cg1 and Cg2 are the centroids of the C1–C6 and C10–C15 rings, respectively; symmetry codes (iv) −x, 2 − y, −z; (v) 2 − x, 1 − y, 1 − z]. These contacts combine to generate extended layers of molecules parallel to (011), Fig. 4a-axis direction, Fig. 5In the crystal structure, each molecule forms five separate inversion dimers. C8—H8et al., 2011aet al., 2011b Chidan Kumar et al., 2014abet al., 2014cA search of the Cambridge Crystallographic Database , followed by a solution of 2-bromo-1-(4-chlorophenyl)ethanone (1.0 mmol). The reaction mixture was stirred for 2 h. Progress of the reaction was monitored by TLC. After completion, the mixture was poured into water and the precipitated solid was filtered, dried and recrystallized (EtOAc/hexane) to afford 2-(4-chlorophenyl)-2-oxoethyl 3-bromobenzoate (1). The formation of keto ester (3) was indicated by the appearance of two typical stretching vibrations ν(C=O) ester (1724) and ν(C=O) keto (1698) cm−1, respectively and the disappearance of characteristic IR stretching absorptions ascribable to the carboxylic acid group in the region of 3400–2400 cm−1. In the 1H NMR spectrum, the signals for the aromatic protons appeared in their respective regions and the disappearance of a characteristic signal for the COOH proton confirmed the formation of the title compound (1). The 13C NMR spectrum displayed two characteristic signals for the keto and ester carbonyl carbon atoms at 190.7 and 165.3 p.p.m., respectively. Yield: 88%; m.p. 372–373 K; Rf: 0.72 (10% EtOAc/hexane); IR : 3089 (Csp2-H), 2933, 2856 (Csp3-H), 1724 (C=O ester), 1698 (C=O ketone), 1585, 1479 (C=C Ar), 1225 (C—O); 1H NMR : δ 8.06–8.03 , 7.94–7.90 , 7.73–7.70 , 7.52–7.48 , 7.46–7.36 , 5.57 ; 13C NMR : δ 190.7, 165.3, 140.6, 134.5, 133.1, 132.4, 132.0, 131.0, 129.3, 129.3, 127.3, 122.1, 66.5.The preparation followed a procedure developed for the preparation of a related compound (Khan Uiso(H) = 1.2Ueq(C) for aromatic, and C—H = 0.99 Å and Uiso(H) = 1.2Ueq(C) for the methylene H atoms.All H atoms were refined using a riding model, with C—H = 0.95 Å and 10.1107/S1600536814021643/hg5410sup1.cifCrystal structure: contains datablock(s) global, 1. DOI: 10.1107/S1600536814021643/hg54101sup2.hklStructure factors: contains datablock(s) 1. DOI: 864789CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the title compounds, N—H⋯O hydrogen bonds lead to dimers; the dimers are linked by weak interactions into a three-dimensional network in one case and chains in the other. N-(arylsulfonyl)arylamides, namely N-(3-fluorobenzoyl)benzenesulfonamide, C13H10FNO3S, (I), and N-(3-fluorobenzoyl)-4-methylbenzenesulfonamide, C14H12FNO3S, (II), are described and compared with related structures. The dihedral angle between the benzene rings is 82.73 (10)° in (I) compared to 72.60 (12)° in (II). In the crystal of (I), the molecules are linked by C—H⋯O and C—H⋯π interactions, resulting in a three-dimensional grid-like architecture, while C—H⋯O interactions lead to one-dimensional ribbons in (II). The crystals of both (I) and (II) feature strong but non-structure-directing N—H⋯O hydrogen bonds with R22(8) ring motifs. The structure of (I) also features π–π stacking interactions.The crystal structures of two  N-(Arylsulfonyl)arylamides have received much attention as they constitute an important class of drugs for Alzheimers disease arylamides are known to be potent antitumour agents against a broad spectrum of human tumour xenografts  in nude mice syn to the N—H bond in the central –C—SO2—N—C(=O)– segment. By contrast, in (II)anti with respect to the meta-fluoro substitution on the benzoyl ring. The dihedral angle between the benzene rings is 82.73 (10)° in (I)The C7 chains, forming columns propagating along the b-axis direction  interactions link the molecules into chains along the c axis. These chains are interconnected via C2—H2⋯πaryl (π system of the sulfonylbenzene ring) and C11—H11⋯πaryl (π system of the sulfonylbenzene ring) interactions, forming a three-dimensional grid-like structure rs Fig. 3. These don Fig. 3. In addire Fig. 4. The cryvia C13—H13⋯O1 interactions, as observed in (I)via C5—H5⋯O3 interactions into ac plane rs Fig. 5. The molne Fig. 5. The oveN-(arylsulfonyl)arylamides, namely N-(benzoyl)benzenesulfonamide (III), N-(3-chlorobenzoyl)benzenesulfonamide (IV), N-(3-methylbenzoyl)benzenesulfonamide (V), N-(benzoyl)-4-methylbenzenesulfonamide (VI) and N-(3-methylbenzoyl)-4-methylbenzenesulfonamide (VII) have previously been reported. A comparison of the dihedral angle between the two benzene rings in these closely related structures indicates that introducing a methyl substituent into the para position of the benzenesulfonyl ring lowers the dihedral angle with compound (VII) being an exception. The dihedral angle values are 80.3 (1)° in (III) C(4) chains via strong structure-directing N—H⋯O hydrogen bonds. The structures do not feature any other type of interactions. However, in (I)aryl. Furthermore, introducing the methyl substituent into the benzenesulfonyl ring of (I)The crystal structures of five related Compounds (I)Uiso = 1.2 or 1.5Ueq(parent atom). To improve considerably the values of R1, wR2 and GOOF, reflections with very bad agreement (−20 0 0), (−20 0 10) and (−19 1 15) in (I)Crystal data, data collection and structure refinement details are summarized in Table 310.1107/S2056989016003248/hb7565sup1.cifCrystal structure: contains datablock(s) I, II, global. DOI: 10.1107/S2056989016003248/hb7565Isup2.hklStructure factors: contains datablock(s) I. DOI: 10.1107/S2056989016003248/hb7565IIsup3.hklStructure factors: contains datablock(s) II. DOI: Click here for additional data file.10.1107/S2056989016003248/hb7565Isup4.cmlSupporting information file. DOI: Click here for additional data file.10.1107/S2056989016003248/hb7565IIsup5.cmlSupporting information file. DOI: 1418689, 1418688CCDC references:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


A and B) in the asymmetric unit, which differ essentially in the orientation of the terminal aminophenyl ring with respect to the central benzene ring. In the crystal, molecules are linked via N—H⋯O hydrogen bonds forming –A-B–A–B– zigzag chains propagating along [010].The title compound crystallized with two independent molecules  in the asymmetric unit. There is an intramolecular O—H⋯N hydrogen bond in each molecule with the phenol ring being inclined to the central benzene ring by 4.93 (14) and 7.12 (14)° in molecules A and B, respectively. The conformation of the two molecules differs essentially in the orientation of the terminal aminophenyl ring with respect to the central benzene ring; this dihedral angle is 50.51 (4)° in molecule A and 54.61 (14)° in molecule B. The two outer aromatic rings are inclined to one another by 51.39 (14) and 49.88 (14)° in molecules A and B, respectively. In the crystal, molecules are connected by N—H⋯O hydrogen bonds generating –A-B–A–B– zigzag chains extending along [010]. The chains are linked via C—H⋯π interactions involving neighbouring A molecules, forming slabs lying parallel to (100).The title compound, C In molecules A and B the phenol rings (C1–C6 and C20–C25) are inclined to the central benzene rings (C8–C13 and C27–C32) by 4.93 (14) and 7.12 (14)°, respectively.The title compound crystallized with two independent molecules ° in molecule B. The two outer aromatic rings  are inclined to one another by 51.39 (14) and 49.88 (14)° in molecules A and B, respectively. The C—N, C N and C—C bond lengths are normal and close to the values observed in related structures  with respect to the central benzene rings (C8–C13 and C27–C32); this dihedral angle is 50.51 (4)° in molecule A-B–A–B– zigzag chains extending along [010]; Table 1via C—H⋯π interactions involving neighbouring A molecules, forming slabs lying parallel to (100); see Table 1In the crystal, molecules are connected by N—H⋯O hydrogen bonds, generating –et al., 2013et al., 2012viz. N-[(E)-4-chlorobenzylidene]-N′-phenylbenzene-1,4-diamine (II) ° in molecule B, owing to the presence of the intramolecular O—H⋯N hydrogen bond. The outer phenyl ring is inclined to the central six-membered ring by 44.18 (11)° in (II), compared to 50.51 (4) and 54.61 (14)° in molecules A and B, respectively, of the title compound.There are very few examples of similar compounds in the literature although some metal complexes of similar ligands have been reported on  of salicyladehyde in 5 ml of absolute ethanol was added dropwise with stirring. The mixture was stirred for 10 min, two drops of glacial acetic acid were then added and the mixture was further refluxed for 2 h. The resulting reddish yellow precipitate was recovered by filtration, washed several times with a small portions of EtOH and then with diethyl ether to give 120 mg (75%) of the title compound. Crystals suitable for X-ray analysis was obtained within 3 days by slow evaporation of a solution in methanol.100 mg (1 mmol) of Uiso(H) = 1.2Ueq(N) and = 1.5Ueq(O). All C-bound H atoms were positioned geometrically and refined using a riding model with C—H = 0.93 Å and with Uiso(H) = 1.2Ueq(C).Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989014026309/su5028sup1.cifCrystal structure: contains datablock(s) global, I. DOI: 10.1107/S2056989014026309/su5028Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989014026309/su5028Isup3.cmlSupporting information file. DOI: 1036844CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


II atom is located on a center of symmetry with an overall octahedral coordination environment. Both intra- and intermolecular interactions occur between the amino and acetate groups, leading to a layered structure.In a cadmium complex incorporating 1,3-diaminopropane and nitrophenylacetate ligands, the Cd 8H6NO4)2(C3H10N2)2], the CdII atom is located on a center of symmetry with one independent Cd—O distance of 2.3547 (17) Å and two Cd—N distances of 2.3265 (18) and 2.3449 (19) Å. The CdII atom has an overall octahedral coordination environment. Several types of hydrogen-bonding interactions are evident. Both intra- and intermolecular interactions occur between the amino groups and the O atoms of the acetate group. These N—H⋯O hydrogen bonds lead to a layered structure extending parallel to the bc plane. In addition, weak intermolecular C—H⋯O interactions involving the nitro groups exist, leading to the formation of a three-dimensional network structure.In the structure of the title compound, [Cd(C Several other weak intermolecular hydrogen-bonding interactions of the C—H⋯O type also exist in the structure involving the O atoms of nitro groups and neighboring C—H groups.Somewhat weaker intermolecular N—H⋯O interactions involving the same types of donor and acceptor groups occur between neighboring molecules Table 1 and leadne Fig. 2. It shou2, 0.4 mmol (29.7 mg) of 1,3-diaminopropane, and 0.4 mmol (72.5 mg) of 4-nitrophenylacetic acid were added to 2 ml of methanol in a 5 ml beaker. The sample was covered with aluminum foil containing several small vent holes and left for a week to evaporate. The slow evaporation method was used to crystallize a colorless mononuclear species and crystals were gathered for X-ray crystallographic analysis.0.2 mmol (36.7 mg) of anhydrous CdClUiso(H) = 1.2Ueq(C) and C—H distances of 0.93 Å for aromatic hydrogen atoms, Uiso(H) = 1.2Ueq(C) and C—H distances of 0.97 Å for methylene hydrogen atoms, and Uiso(H) = 1.2Ueq(N) and N—H distances of 0.90 Å for amino hydrogen atoms.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989016000943/wm5258sup1.cifCrystal structure: contains datablock(s) I. DOI: 10.1107/S2056989016000943/wm5258Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989016000943/wm5258Isup3.cdxSupporting information file. DOI: 1447705CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In the crystal, pairs of inversion-related molecules are linked into inversion dimers  23H19NO2, an oxazine Mannich base derivative, the oxazine ring has a half-chair conformation. The 2-hydroxynaphthalen-1-yl substituent is placed in an axial position. There is an intramolecular O—H⋯N hydrogen bond, forming an S(6) graph-set motif. In the crystal, molecules are connected by a pair of C—H⋯π interactions into an inversion dimer, which is reinforced by another pair of weak C—H⋯π interactions. The dimers are linked by a π–π interaction [centroid-centroid distance = 3.6268 (17) Å], consolidating a column along the a axis. Furthermore, the columns interact with each other by a weak C—H⋯π interaction, generating a three-dimensional network.In the title compound, C Recently, we synthesized the title compound by a reaction between the cyclic aminal 1,3,6,8-tetraazatricycloundecane (TATU) with 2-naphthol solvent-free at low temperature. Because a wide range of cured properties can be obtained  Å, θ = 50.0 (3)° and φ = 98.3 (4)° for the ring O1/C1/N1/C2/C12/C11. The methyl group bonded to atom N1 of the oxazine ring is placed in an axial position. The pendant naphthyl group (C21–C30) makes a dihedral angle of 59.94 (4)° with the oxazine ring plane defined by atoms C11, C12 and O1. The bond lengths, N1—C1 and O1—C1, are normal and comparable to the corresponding values observed in the related structure of 6-bromo-2,4-bis(3-methoxy-phenyl)-3,4-dihydro-2H-1,3-naphthoxazine  graph-set motif, where the N⋯O distance is longer by about 0.04 and 0.03 Å, respectively, than the observed values in related structures of 1-(piperidin-1-ylmethyl)-2-naphthol  Å . Neighboring columns are connected by a weak C—H⋯π interaction   were manually ground together, heated to 313 K and stirred for 12 h under solvent-free conditions. Progress of the reaction was determined by TLC monitoring. After completion of the reaction, the mixture was cooled to room temperature and the solid residue was purified by silica gel column chromatography with benzene–ethyl acetate (4:1) as the eluent to give 1-{oxazin-2(3H)-yl]methyl}naphthalen-2-ol as a brown solid in 28% yield. This compound was obtained in its crystalline form by recrystallization from an absolute ethanol solution (m.p. 443 K).2-Naphthol  and 1,3,6,8-tetraazatricyclo[4.3.1.1Uiso(H) value and the C—C—O—H torsion angle were refined. C-bound H atoms were fixed geometrically (C—H = 0.95 or 0.99 Å) and treated as riding with Uiso(H) = 1.2Ueq(C).Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S2056989015015583/is5412sup1.cifCrystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989015015583/is5412Isup2.hklStructure factors: contains datablock(s) I. DOI: Click here for additional data file.10.1107/S2056989015015583/is5412Isup3.cmlSupporting information file. DOI: 1419687CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


In this complex, all CuII atoms have a square-pyramidal coordination sphere, with long axial and short basal Cu—O distances.The dinuclear title compound crystallizes as a dimer forming a tetranuclear copper(II) complex, [Cu 4(CH3O)4(C11H13O2)4], consists of dimeric dinuclear copper(II) complexes oriented around a centre of inversion. Within each dinuclear fragment, the two CuII atoms are in a distorted square-planar coordination sphere. Two neighbouring fragments are linked by four apical Cu—O contacts, yielding an overall square-pyramidal coordination environment for each of the four CuII atoms. The molecules are arranged in layers parallel to (101). Non-classical C—H⋯O hydrogen-bonding interactions are observed between the layers.The structure of the title compound, [Cu The distances and coordination modes between CuII atoms vary and thus, the compound is a suitable study case for investigating different spin-coupling paths. This knowledge is deemed important for the design of tailor-made magnetic compounds.The title compound was obtained as a by-product in the synthesis of an unsymmetrically substituted copper(II) salophene complex  ions Cu1 and Cu2 within the binuclear fragment is 2.9938 (2) Å  title compound consists of two dinuclear complex fragments oriented around a centre of inversion. Within each fragment the two Cu Å Fig. 1 which isi  bond to the methoxido ligand of the neighbouring fragment. For the Cu2 atom, the situation is comparable, with slightly shorter Cu—O distances in comparison with Cu1: Cu2—O3 1.8939 (8) Å, Cu2—O4 1.9473 (9) Å, Cu2—O5 1.9455 (8) Å and Cu2—O6 1.9081 (8) Å. The longer distance Cu2—O1i of 2.4994 (9) Å to the phenoxido ligand atom of the neighbouring fragment causes less sterical congestions at the Cu2 atom and thus, appears to be the cause for the shorter basal Cu—O distances.Short distances Cu1—O1 of 1.9166 (8) Å, Cu1—O2 of 1.9557 (9) Å, Cu1—O5 of 1.9522 (8) Å and Cu1—O6 of 1.9154 (9) Å are found for the Cu1 atom to the basal O atoms within the binuclear fragment. A substantially longer distance of 2.3703 (9) Å is observed for the apical Cu1—O52versus μ3) of the two methoxido ligands in each fragment can be distinguished by the angles C24—O5—O6  versus C23—O6—O5  , resulting in a more pyramidal-like geometry. This differs to the more trigonal-planar geometry of O6 (see Table 1versus 1.2963 (13) Å].The binding modes ° due to repulsion of the In the crystal, the tetranuclear molecules arrange in layers parallel to (101) Fig. 2. Weak notert-butylsalicylaldehyde in 10 ml THF, the mixture was stirred for 22 h at room temperature. Addition of hexane yielded the title compound as a dark crystalline material from the reaction mixture .After treatment of 102 mg (0.35 mmol) 4-Br-salicyl-2-(2-amino)phenylimine with 113 mg of copper(II)acetate monohydrate (0.445 mmol), 1 ml triethylamine in 10 ml THF, and 65.5 mg (0.368 mmol) 4-Uiso(H) = 1.5Ueq(C) for sp2 C atoms and of 0.98 Å and Uiso(H) = 1.5Ueq(C) for sp3 C atoms.Crystal data, data collection and structure refinement details are summarized in Table 310.1107/S205698901500376X/wm5122sup1.cifCrystal structure: contains datablock(s) general, I. DOI: 10.1107/S205698901500376X/wm5122Isup2.hklStructure factors: contains datablock(s) I. DOI: 1050914CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information:


Single crystals of the ligand have been grown and analyzed.Hydrazones and their metal complexes were heavily studied due to their pharmacological applications such as antimicrobial, anticonvulsant analgesic, anti-inflammatory and anti-cancer agents. This work aims to synthesize and characterize novel complexes of VO2+, Co2+, Ni2+, Cu2+, Zn2+, Zr4+ and Pd2+ complexes have the formulas: [VO(OBH–H)2]·H2O, [Co(OBH)2Cl]Cl·½EtOH, [Ni2(OBH)Cl4]·H2O·EtOH, [Cu(OBH)2Cl2]·2H2O, [Zn(OBH–H)2], [Zr(OBH)Cl4]·2H2O, and [Pd2(OBH)(H2O)2Cl4]·2H2O. All complexes are nonelectrolytes except [Co(OBH)2Cl]Cl·½EtOH. OBH ligates as: neutral tetradentate (NNOO) in the Ni2+ and Pd2+ complexes; neutral bidentate (OO) in [Co(OBH)2Cl]Cl·½EtOH, [Zr(OBH)Cl4]·2H2O and [Cu(OBH)2Cl2]·2H2O and monobasic bidentate (OO) in the Zn2+ and VO2+ complexes. The NMR (1H and 13C) spectra support these data. The results proved a tetrahedral for the Zn2+ complex; square-planar for Pd2+; mixed stereochemistry for Ni2+; square-pyramid for Co2+ and VO2+ and octahedral for Cu2+ and Zr4+ complexes. The TGA revealed the outer and inner solvents as well as the residual part. The molecular modeling of [Ni2(OBH)Cl4]·H2O·EtOH and [Co(OBH)2Cl]Cl·½EtOH are drawn and their molecular parameters proved that the presence of two metals stabilized the complex more than the mono metal. The complexes have variable activities against some bacteria and fungi. [Zr(OBH)Cl4]·2H2O has the highest activity. [Co(OBH)2Cl]Cl·½EtOH has more activity against Fusarium.Oxalo bis [OBH] has a monoclinic crystal with P 1 21/n 1 space group. The VO2+ and Co2+ complexes have square-pyramid structure. [Cu(OBH)2Cl2]·2H2O and [Ni2(OBH)Cl4]·H2O·EtOH decomposed to their oxides while [VO(OBH–H)2]·H2O to vanadium. The energies obtained from molecular modeling calculation for [Ni2(OBH)Cl4]·H2O·EtOH are less than those for [Co(OBH)2Cl]Cl·½EtOH indicating the two metals stabilized the complex more than mono metal. The Co(II) complex is polar molecule while the Ni(II) is non-polar.Oxalo bis structure was proved by X-ray crystallography. It coordinates with some transition metal ions as neutral bidentate; mononegative bidentate and neutral tetradentate. The complexes have tetrahedral, square-planar and/or octahedral structures. The VOThe online version of this article (doi:10.1186/s13065-015-0135-y) contains supplementary material, which is available to authorized users. In the preparation of VO−3 mol L−1 DMSO solution of the compounds was measured on Orion 3 STAB Conductivity Bridge. The IR spectra were recorded as KBr discs on a FT/IR-6300 type A (400–4000 cm−1). The electronic spectra of the complexes were recorded on a Cary 5 UV–vis spectrophotometer, varian (200–900 nm). The 1H NMR spectra of the ligand and the diamagnetic complexes were recorded in DMSO-d6, on a Bruker WP 200 SY Spectrometer (400 MHz) at room temperature using tetramethylsilane (TMS) as an external standard. The magnetic measurements were carried out on a Johnson-Matthey magnetic balance, UK. The TGA thermograms were recorded (25–800 °C) on a Shimadzu TGA-60; the nitrogen flow and heating rate were 50 ml/min and 10 °C min−1, respectively. The X-ray single crystal diffraction data were collected on a Rigaku R-Axis Rapid diffractometer using filtered Mo-K α-radiation. The structure was solved by the direct methods and expanded using Fourier techniques at Kuwait University. The ligand and its complexes were investigated for antimicrobial activity against Bacillus, Aspergillus, Escherichia coli, Pennicillium and Fusarium as reported earlier ·H2O, [Co(OBH)2Cl]Cl·½EtOH, [Cu(OBH)2Cl2]·2H2O, [Zn(OBH–H)2], [Zr(OBH)Cl4]·2H2O and binuclear complexes: [Ni2(OBH)Cl4]·H2O·EtOH and [Pd2(OBH)(H2O)2Cl4]·2H2O. All complexes are colored, solid and stable towards air and moisture at room temperature. They have high melting points and are insoluble in most common organic solvents and completely soluble in DMSO. The molar conductance values  complex supports the formation of [Co(OBH)2Cl]+Cl−·½EtOH  and ν(C=N) vibrations at 3325, 1701 and 1605, respectively in its IR spectrum Cl4]·2H2O coordinating through the two amidic carbonyl groups based on the following observations: the υ(C=O) band observed at 1701 cm−1 in ligand spectrum was shifted to 1686–1699 cm−1 in complexes having little intensity indicating that the two amidic carbonyl groups (C=Oamidic) participated in bonding while the other two carbonyl (C=Oketonic) still at the same position. The new band at 464–495 cm−1 is due to υ(M–O) vibration  showed splitting of NH signal as a result of conversion of one of NHC=O to N=C–OH and the existence of the others without participation ketonic, (C=O)amidic free, (C=O)amidic bonded, (C=N), (C=N)*, (C–O) and CH3, respectively. The appearance of (C=N)* (due to conversion of NHC=O to N*=C–O) and (C–O) peaks confirm enolization process   and υ(M–ed water  and abse2(OBH)Cl4]·H2O·EtOH (Structure 2(OBH)(H2O)2Cl4]·2H2O amidic to 1644 in the Pd(II) complex and to 1552 and 1676 in the Ni(II) complex together with appearance of υ(M–N) ·H2O·EtOH has a value of 371.7 (the base peak) corresponding to Ni(OBH)Cl·½EtOH meaning that this species is highly stable. Multi peaks were observed ending with one at 128.9 (intensity 65 %) due to ZrO2.Moreover, the mass spectrum of ·H2O·EtOH is 1.36 BM which is less than the normal values reported for tetrahedral or octahedral coordination containing two unpaired electrons. Its electronic spectrum showed a broad band at 19,050 cm−1 (ɛ = 180 mol−1 L) typical of a square-planar structure with some distortion [2(OBH)(H2O)2Cl4]·2H2O proved the square-pyramid structure in which the metal is surrounded by NO donors, two chloro and one coordinated water. The bands at 37,540 and 28,470 cm−1 are attributed to charge transfer transitions, probably O → Pd transition ·H2O exhibits one band with maximum at 20080 cm−1 assigned to the 2E2g → 2T2g transition in an octahedral geometry [g level. The magnetic moment value (1.45 BM) was found lower than the values reported for the d9–system containing one unpaired electron (1.73–2.25 BM) suggesting interactions between the copper centers.The electronic spectrum of [Cu(OBH)geometry . The ban2Cl]Cl·½EtOH showed three decomposition steps at mid- points of 60, 319 and 500 °C corresponding to the removal of ½Cl2 + ½EtOH ; C16H24N4O6Cl  and C4H4N2  leaving [CoO4N2] moiety .The decomposition steps, the DTG maximum temperature and the removing species are shown in Table 2]·H2O showed also three steps; the first (mid. point 56 °C) represents the removal of the outside water molecule ; the second (mid. point 289 °C) represents the loss of C16H24N4O6  and the third for the repulsion of C4H4N4O2 . The residue is vanadium metal .The TG curve of [VO(OBH-H)2Cl2]·2H2O thermogram showed decomposition steps ending with copper oxide at Temp. >400 °C. The decomposition showed the removal of the two hydrated water in the first step at mid. point of 59 °C. The other two steps were observed at 291 and 374 °C corresponding to the removal of C16H24N4O6 and C4H4N4O3, respectively, leaving CuO as a residue.[Cu(OBH)2(OBH)Cl4]·H2O·EtOH showed four steps. The first at 72 °C is due to the removal of the outside water and EtOH . The second step (368 °C) represents the loss of Cl2 + C8H12N2O2 . The third step represents the repulsion of Cl2 . The fourth step  corresponding to the removal of C2H2N2. The residue is 2NiO  . The first three steps observed at mid. points of 76, 313 and 449 °C are corresponding to the removal of (Cl2 + H2O); (H2O + C8H12N2O2) and Cl2, respectively Cl2(OBH)(H2O)2Cl4]·2H2O showed two main steps at 75 and 322 °C due to the liberation of the outside water and 2H2O + 2Cl2 + C4H12, respectively. High residue  % was found over 500 °C.The thermogram of [Pd2Cl]Cl·½EtOH and [Ni2(OBH)Cl4]·H2O·EtOH (Structure 2(OBH)Cl4]·H2O·EtOH are less than those of [Co(OBH)2Cl]Cl·½EtOH indicating that the presence of two metals stabilized the complex more than the mono metal lowering the energy. The dipole moment calculated for the Co(II) complex is 4.949 D proving the polar nature of the complex. The value of Ni(II) complex is 0.413 D indicating its non-polarity.Trials to grow single crystals for the investigated complexes were failed. In order to calculate the molecular parameters, ·2H2O has higher activity against all tested microorganisms except E. coli. The activity is highest and more with Penicillium (9 mm zone inhibition). The higher activity may be due the presence of non-ionizable chlorine and to the less planarity of the complex making it more lipophilic. Most compounds have high activity against Fusarium. [Cu(OBH)2Cl2]·2H2O has higher value against Fusarium (15 mm). Comparing these data with that of ampicillin and those obtained for different hydrazone complexes showed more or less activity ·2H2O and [Ni2(OBH)Cl4]·H2O·EtOH decomposed to their oxides while [VO(OBH–H)2]·H2O to the metal. The energies from molecular modeling calculation is less in [Ni2(OBH)Cl4]·H2O·EtOH than those for [Co(OBH)2Cl]Cl·½EtOH indicating that the presence of two metals stabilized the complex more than the mono metal. The Co(II) complex is polar molecule while the Ni(II) is non-polar.Oxalo bis has been prepared and characterized by x-ray crystallography. It coordinates as neutral bidentate; mononegative bidentate and neutral tetradentate. The complexes have tetrahedral, square-planar and/or octahedral structures. The VOCrystallographic data for the structure reported in this paper have been deposited with Cambridge Crystallographic Data Center as supplementary publication CCDC-985982.


This article describes data related to the research article titled “Functional characterization of importin α8 as a classical nuclear localization signal receptor”  Specifications TableValue of the data•These data are valuable to researchers interested in the molecular mechanisms by which the importin α-cNLS substrate complex dissociates in the nucleus.•These data show that importin α1 and α8 have substantial differences in dimer-forming ability, despite both proteins belonging to the same subfamily.•These data provide a new insight into the function of nuclear-localized importin αs.1To examine whether importin αs can directly bind with other importin α subtypes, FLAG-tagged importin α6, α7, or α8 recombinant proteins were incubated with either GST-importin α8, or GST-importin α1, and analyzed by western blotting A. To inv22.1EcoRI and NotI, and then subcloned into the pGEX6P3 plasmid . The construct integrity of pGEX6P3/FLAG-h-importin α6 and pGEX6P3/FLAG-h-importin α7 was confirmed by DNA sequencing using the following primers: pGEX 5′ sequencing primer: 5′-GGGCTGGCAAGCCACGTTTGGTG-3′, pGEX 3′ sequencing primer: 5′-CCGGGAGCTGCATGTGTCAGAGG-3′, importin α6 sequencing primer: 5′-GCATCTGGAACTTTTCTGCATACC-3′, or importin α7 sequencing primer: 5′-GTACATTACAGTTTGAAGCTGCCT-3′.The N-terminus FLAG-tagged cDNAs encoding full-length human importin α6  or full-length human-importin α7  were amplified from either HEK293 cells or MRK-nu-1 cells  by PCR using the following primers: importin α6 Forward: 5′-CCCGAATTCCGCCATGGACTACAAGGACGACGACGACAAGATGGATGCCATGGCTAGTCC-3′ and importin α6 Reverse: 5′-CCCGCGGCCGCCTCGAGTTAAAGTTGAAATCCATCC-3′ or importin α7 Forward: 5′-CCCGAATTCCGCCATGGACTACAAGGACGACGACGACAAGATGGAGACCATGGCGAGC-3′ and importin α7 Reverse: 5′-CCCGCGGCCGCCTCGAGTTATAGCTGGAAGCCCTCC-3′. The PCR program was as follows: 2 min at 94 °C followed by 40 cycles of 30 s at 98 °C and 15 min at 68 °C. The PCR products were digested with EcoRI and NotI sites of pGEX6P3, and then sequenced using either the pGEX 5′ or pGEX 3′ sequencing primer and the importin α8 sequencing primer: 5′-CAACATCGCTTCAGGGACTTCG-3′.The human-importin α8  cDNA with the FLAG-tag at the N-terminus was amplified by PCR from the pcDNA5/3xFLAG-h-importin α8 plasmid The construct encoding SV40 large T antigen NLS  was subcloned from pGEX2T-SV40TNLS-GFP BamHI and XhoI sites of pGEX6P1, and then verified by sequencing.The human cDNA encoding the tumor protein p53 (NM_000546) was amplified from MCF7 cells by PCR performed using the following primers: p53 Forward: 5′-CACGGATCCATGGAGGAGCCGCAGTCAGATC-3′ and p53 Reverse: 5′-GGACTCGAGTCAGTCTGAGTCAGGCCCTTCTG-3′. The PCR program was as follows: one cycle of 2 min at 94 °C; 40 cycles of 15 s at 94 °C, 30 sec at 64 °C, and 1 min 20 s at 68 °C; and one cycle of 10 min at 68 °C. The PCR product was subcloned into the 2.2Escherichia coli Rosetta, and then the cells were grown at 37 °C in LB medium containing 50 μg/mL ampicillin. Expression was induced by addition of 1 mM isopropyl-β-d-thiogalactopyranoside (IPTG), followed by incubation at 20 °C for 12 h. The bacteria were lysed in lysis buffer , 0.2 mM phenylmethylsulfonyl fluoride (PMSF), 1 μg/mL aprotinin , 1 μg/mL pepstatin , and 1 μg/mL leupeptin (Peptide Institute)) by freeze–thawing twice and passing through a French press . The cell lysates were sonicated using a Sonifier 250 , and centrifuged at 20,400g at 4 °C for 30 min. The resultant supernatant was incubated with glutathione-Sepharose 4B beads  at 4 °C for 12 h. After the GSH beads were washed five times with lysis buffer, GST-tagged proteins were eluted with elution buffer . Cleavage of GST from the GST-fused protein was performed using PreScission protease  with 10 units/mg of fusion protein at 4 °C for 12 h in cleavage buffer . Finally, the purified proteins were dialyzed against dialysis buffer  and concentrated by ultrafiltration using Amicon Ultra centrifugal filter units .Recombinant proteins fused to GST were purified as follows: The expression vectors were transformed into 2.32.4The following antibodies were used for western blotting: anti-FLAG M2 antibody , anti-GST antibody , anti-GFP antibody , anti-p53 (FL-393) antibody , and horseradish peroxidase (HRP)-conjugated anti-mouse or anti-rabbit IgG secondary antibodies 2.5http://rsbweb.nih.gov/ij/).Samples were loaded on a 10% SDS-PAGE gel, and the separated proteins in the gel were transferred onto an Immobilon-P membrane  using a semi-dry transfer blotting system . The membrane was blocked with blocking buffer consisting of 3% skim milk in Tris-buffered saline  with 0.05% Tween (TBS-T) for 1 h. The membrane was probed with primary antibodies diluted in Can Get Signal Immunoreaction Enhancer Solution 1  at 4 °C overnight, and then incubated with the HRP-conjugated secondary antibody diluted in Can Get Signal Immunoreaction Enhancer Solution 2 (TOYOBO) at room temperature (RT) for 1 h. After the membrane was washed with TBS-T, it was developed with Chemi-Lumi One L or Super . The intensity of each western blot signal was quantified by Image J software (


I with the unsymmetrical ligand N-(pyridine-2-ylmethyl)pyridine-3-amine afforded right- and left-handed helical chains. The AgI atom of the right-handed helical chain adopts a slightly distorted linear coordination geometry, while that of the left-handed helical chain displays a bent geometry.The reaction of Ag 11H11N3)]CF3SO3}n, there are two AgI atoms, two N-(pyridine-2-ylmethyl)pyridine-3-amine ligands (A and B) and two CF3SO3− anions. Both AgI atoms are bridged by two pyridine N atoms from two symmetry-related A or B ligands, forming right- or left-handed helical chains, respectively. The AgI atom of the right-handed helical chain adopts a slightly distorted linear coordination geometry [N—Ag—N = 170.69 (14)°], while that of the left-handed helical chain adopts a bent geometry [N—Ag—N = 149.42 (14)°]. Both helical chains have the same pitch length [10.8437 (5) Å], propagate along the b-axial direction and are alternately arranged via Ag⋯Ag [3.0814 (5) Å] and π–π stacking interactions [centroid–centroid distances = 3.514 (3) and 3.487 (3) Å], resulting in the formation of a two-dimensional supramolecular network extending parallel to the ab plane. Weak Ag⋯O  and Ag⋯F [3.017 (3) Å] interactions as well as N—H⋯O and C—H⋯O, C—H⋯N and C—H⋯F hydrogen-bonding interactions occur between the helical chains and the anions.In the asymmetric unit of the title compound, {[Ag(C The structure of title compound is related to that of the perchlorate salt , two N-(pyridine-2-ylmethyl)pyridine-3-amine  and two trifluoromethanesulfonate anions. The Ag1 atom is coordinated by two pyridine N atoms from two symmetry-related A ligands giving a geometry which is slightly distorted from linear [N1—Ag1—N2 = 170.69 (14)°], forming a right-handed helical chain, while the Ag2 atom is coordinated by two pyridine N atoms from two symmetry-related B ligands in a bent arrangement [N4—Ag2—N5 = 149.42 (14)°], forming a left-handed helical chain. Two pyridine rings coordinating to the Ag1 and Ag2 atoms are tilted by 14.1 (3) and 28.9 (2)°, respectively, with respect to each other.The molecular components of the title structure are shown in Fig. 1b-axial direction and are alternately arranged via Ag1⋯Ag2 interactions [3.0814 (5) Å], resulting in the formation of a two-dimensional supramolecular network extending parallel to the ab plane  Å; symmetry code: (iv) −x, y − z + 3SO3− anions.Both helical chains in the structure have the same pitch length [10.8437 (5) Å], propagate along the ne Fig. 2. Further] Figs. 1 and 2 ▶ N-(pyridin-2-ylmethyl)pyridine-3-amine) was prepared according to a procedure described by Lee et al.  = 0.95 Å for Csp2—H, 0.88 Å for amine N—H and 0.99 Å for methylene C—H. For all H atoms Uiso(H) = 1.2Ueq.Crystal data, data collection and structure refinement details are summarized in Table 210.1107/S1600536814022922/zs2318sup1.cifCrystal structure: contains datablock(s) I, New_Global_Publ_Block. DOI: 10.1107/S1600536814022922/zs2318Isup2.hklStructure factors: contains datablock(s) I. DOI: 1029928CCDC reference:  crystallographic information; 3D view; checkCIF reportAdditional supporting information: