Structure of lithium (picrate) (2,2′-bipyridyl)

The title compound C₁₆H₁₀N₅O₇Li is triclinic, witha=14.51(1),b=6.90(2),c=9.10(1) Å,=101.5(1),=67.1(2), =105.6°(1),Z=2 and space groupP¯1. Data were measured by photographic methods. The structure was solved by direct methods, and refined by full matrix least-squares. The refinement, based on 1337 reflections, gave the rather highR value of 0.11 because of poor quality data. The complex is dimeric. The coordination around the cation is distorted square-pyramidal. Two coordination sites are occupied by the nitrogen atoms of the bipyridyl ligand, two by the phenolic oxygen and oxygen ofo-nitro group, and the fifth coordination site is occupied by the phenolic oxygen belonging to the symmetry-related molecule (1–x,–y,1–z). Both oxygens act as bridges to form the dimer. The bridging is unsymmetrical, with Li-O (phenolic)=1.84(2) Å and Li¹-O (phenolic)=2.16(2) Å (whereI=1–x,–y, 1–Z).     

Structure of 2-(2′-bromo-5′-nitrostyryl)benzothiazole

The title compound C₁₅H₉BrN₂O₂S (brnsb) is monoclinic, witha=7.730(2),b=26.847(5),c=7.773(2) Å,=117.48(1)°,V=1431(1) ų,Z=4,D _x=1.677,(MoK)=29.9 cm^–1,F(000)=720,T=298K in space groupP2₁/c. The structure was solved by heavy atom and Fourier methods and refined toR=0.034 for 1776 unique observed reflections. The molecule is nearly planar, with a dihedral angle of only 3.8(1.1)° between the benzothiazole and phenyl rings. The C-S-C angle in the thiazole ring is 89.0°, while the C-N-C angle in that ring is 111.5(3)°.     

Structures of NN′-ethylenebis(monothioacetylacetoneiminato)nitrosylcobalt and NN′-ethylenebis(2-hydroxyacetophenoneiminato)nitrosylcobalt

The cobalt atoms in both [Co(NO)(sacacen)] and [Co(NO)(7-Mesalen)] {sacacenH₂ isNN-ethylenebis(monothioacetylacetoneimine) and 7-MesalenH₂ isNN-ethylenebis(2-hydroxyacetophenoneimine)} are 5-coordinate, with a tetragonal-pyramidal arrangement of donor atoms. The cobalt atom in [Co(NO)(sacacen)] lies just above the plane defined by the SNNS donor atoms of the quadridentate ligand, and the nitrosyl group occupies the apical position. A similar geometry is defined by the ONNO donor atoms and the NO group in [Co(NO)(7-Mesalen)]. The Co-N-O angles are strongly bent, as predicted from¹⁵N-nmr studies (127.2(6)°[Co(NO)(sacacen)] and 127.4(3)°[Co(NO)(7-Mesalen)]). Both nitrosyls crystallize in the monoclinic system. For [Co(NO)(sacacen)],a=8.501,b=12.673,c=13.866 Å,=95.00°,Z=4 and space groupP2₁/c. The structure was determined by the heavy-atom method, usingMo K diffractometer data, and refined by full matrix least squares toR=0.062 for 2920 observed reflections. For [Co(NO)(7-Mesalen)],a=9.461,b=13.053,c=13.456,=99.32°,Z=4 and space groupP2₁/c. The structure was determined as above toR=0.040 for 2461 observed reflections.     

Structure of (2,2′-bipyridine)lead(II) saccharinate monohydrate

The structure of (2,2-bipyridine)lead(II) saccharinate monohydrate has been investigated by X-ray diffraction. The compound crystallizes in the monoclinic space group P2 ₁/n with a = 22.903(7), b = 12.608(3), c = 8.682(2) Å, = 96.76(3)°, and Z = 4. The structure consists of Pb²⁺ cations, 2,2-bipyridine ligands, saccharinato anions and water molecules. The Pb²⁺ cation is surrounded by two O atoms and four N atoms. The two saccharinato ions are nonequivalent. The water molecule forms hydrogen bonds of O_W···O_CO [2.810(16) Å] and O_W···O_SO2 [2.893(16) Å] type.     

Structure of 2,2′-bis(4-cyanatophenyl)isopropylidene

The title compound is monoclinic:a=13.345(3),b=11.393(2),c=10.046(5)Å,=108.48(2)°,Z=4,P2₁/c. The structure was determined by direct methods, using MoK diffractometer data, and refined by full-matrix least squares toR=0.045 for 1463 reflections. The structure shows a central tetrahedral carbon atom surrounded by two methyl and two phenylcyanate groups. The geometry of the cyanate group compares well with that in 4-chloro-3,5-dimethyl-phenyl cyanate, the only example of an organic cyanate in the Cambridge Crystallographic database (V.3). The intermolecular nitrile, C-N, distances were examined for evidence of a possible dimerization interaction; no significant distances were found.     

Structural study of nitrovinylindoles: (I) 2-methyl-3-(2′-methyl-2′-nitrovinyl)indole and (II) 3-(2′-nitrovinyl)indole

Compound (I) is 2-methyl-3-(2-methyl-2-nitrovinyl)indole, C₁₂H₁₂N₂O₂,M _r=216.24, monoclinic,P2₁/n,a=16.710(1),b=7.627(1),c=17.646(1) Å,=104.8(1)°,V=2174.7(1) ų,Z=8.D _x=1.321 g cm^–3, MoK, =0.71073 Å,=0.858 cm^–1,F(OOO)=912, room temperature,R=0.061 for 1956 observed reflections. Compound (II) is 3-(2-nitrovinyl)indole, C₁₀H₈N₂O₂,M _r=188.18, monoclinic,P2₁/n,a=10.178(1),b=10.608(1),c=8.411(1) Å,=105.5(2)°,V=875.0(1) ų,Z=4,D _x=1.4284 g cm^–3, CuK, =1.5418 Å,=8.068 cm^–1,F(000)=392, room temperature,R=0.040 for 1330 observed reflections. Compounds (I) and (II) have a similar geometry, the only significant difference lying in the rotation of the nitrovinyl chain. This feature could be responsible for the difference in biological activity. In both compounds, the molecules are associated, forming charge-transfer complexes.     

Structure of 1-ethyl-2-(2′-chloro-4′-nitrostyryl)benzimidazole

The title compound C₁₇H₁₄ClN₃O₂ (et-4-nsbiz) is monoclinic, witha=12.240(2),b=12.144(4),c=10.544(4)Å,=100.09(2)°,V=1543(1)ų,Z=4,D _x =1.411 g cm^–3, (MoK)=0.71073Å,=2.57 cm^–1,F(000)=680,M _r =327.77,T=298K. The structure was solved by heavy atom and Fourier methods and refined toR=0.049 for 1503 unique observed reflections in space groupP2₁/c. Except for the ethyl group, the molecule is almost planar, with a dihedral angle of 9.5(5)° between the benzimidazole and phenyl rings. The dihedral angle between the ethyl group and the benzimidazole ring to which it is attached is 91.5(2)°.     

Structural analysis of 1,1′-bis(diphenylphosphino)ferrocene dioxide

The title compound 1,1′-bis(diphenylphosphino)ferrocene dioxide has been analyzed by X-ray crystal diffraction analysis. The crystals are monoclinic, space group P2(1)/c with a = 22.461(5), b = 10.515(2), c = 12.024(2) Å, α = 90, β = 96.28(3), γ = 90°, V = 2822.7(10) ų, Z = 4, F(000) = 1256, D_c = 1.422 g/cm³, μ = 0.683 mm^?1, the final R = 0.0514 and wR = 0.1369. A total of 22218 reflections were collected, of which 4957 were independent (R_int = 0.0422). In the crystal packing diagram, intermolecular O?H···O hydrogen bonds between the P=O and H₂O stabilize the solid state of the title compound.     

Crystal structure of 3,3′-dimethoxybenzydine (2-hydroxybenzal)diimine

Molecular and crystal structure of 3,3'-dimethoxybenzydine(2-hydroxybenzal)diimine, C₂₈H₂₄N₂O₄, have been determined by single crystal X-ray diffraction study. The title compound is monoclinic, with a= 18.045(2) Å, b= 11.725(4) Å, c= 12.436(6) Å, = 120.03(3)°, Z=4, D _x =1.32 g/cm³, (MoK) =0.089 mm^–1, and space group is C2/c. The structure was solved by direct methods and refined to a final R=0.056 for 2325 reflections with I > 2(I). There is half independent molecule in the asymmetric unit. The molecule has a twofold symmetry on the mid point of the C4 C4 ⁱ bond. The N1-C8 imine bond length of 1.284(3) Å is typical of a double bond. The molecule of the title compound is not planar. There is a strong intramolecular hydrogen bond between hydroxy oxygen atom and imine nitrogen atom. The crystal structure is stabilized by a weak intermolecular hydrogen bond of the C H O type forming three-dimensional cage.     

X-ray structure of 3,3′-bis(4-methylthioquinolinyl) sulfide

The structure of the title compound has been solved by direct methods, and refined to anR value of 0.035 for 1613 reflections. Both methyl carbon atoms deviate from the plane of the pyridine ring by 1.505(3) Å in opposite directions. Both sulfur atoms S(1) and S(2) remain in short contact, at 3.247(1) Å. The two pyridine rings are inclined at 61.4(2)° to each other.Part XIV in the series of Azinyl Sulfides.     

Structures of nitrato-(2-hydroxybenzaldehydo) (2,2′-bipyridyl)copper and nitrato-(2-hydroxy-5-nitrobenzaldehydo)(2,2′-bipyridyl)copper

Nitrato-(2-hydroxy-5-nitrobenzaldehydo)(2,2′-bipyridyl)copper (I) and nitrato-(2-hydroxybenzaldehydo)(2,2′-bipyridyl)copper (II) were synthesized and characterized by X-ray diffraction. The coordination polyhedron of the central copper atom in complex I can be described as a distorted tetragonal pyramid whose base is formed by the phenol and carbonyl oxygen atoms of the monodeprotonated 2-hydroxy-5nitrobenzaldehyde molecule and the nitrogen atoms of the 2,2′-bipyridyl ligand and whose apex is occupied by the oxygen atom of the nitrato group. In the crystal structure, complexes I are linked by the acido ligands and the NO₂ groups of the aldehyde molecule into infinite chains. In complex II, the central copper atom is coordinated by 2-hydroxybenzaldehyde, 2,2′-bipyridyl, and the nitrato group, resulting in the formation of centrosymmetric dimers. The coordination polyhedron of the central copper atom can be described as a bipyramid (4 + 1 + 1) with the same base as in complex I. The axial vertices of the bipyramid are occupied by the oxygen atom of the nitrato group and the bridging phenol oxygen atom of the adjacent complex related to the initial complex by a center of symmetry. In the crystal structure, complexes II are hydrogen bonded into infinite chains.     

Crystal and molecular structure of 2-(2′-chloro-5′-nitrostyryl)benzoselenazole

The title compound C₁₅H₉ClN₂O₂Se (nsbse) is orthorhombic, witha=6.823(2),b=7.860(2),c=26.349(5) Å,Z=4,D _x =1.709,(MoK)=28.3 cm^–1,F(000)=720,T=298K in space groupP2₁2₁2₁. The structure was solved by heavy atom and Fourier methods and refined toR=0.045 for 1095 unique observed reflections. The molecule is almost planar, with a dihedral angle of 4.8(2)° between the benzoselenazole and phenyl rings. The C-Se-C angle in the selenazole ring is very small, 84.6(4)°, while the C-N-C angle in that ring is 113.7(7)°.     

Synthesis and Characterization of Two Pb(II) Complexes of 2,2′-dihydroxy,Dimethoxy-1,1′-binaphthyl-3,3′-dicarboxylic Acid

Two new complexes {[Pb(L¹)(DMSO)₂(H₂O)]·DMF}_n (1, L¹ = 2,2′-dihydroxy-l,l′-dinaphthyl-3,3′-dicarboxylate) and {[Pb(L²)(DMS O)·DMSO}_n (2, L² = 2,2′-dimethoxy-l,l′-dinaphthyl-3,3′-dicarboxylate) have been synthesized under mild conditions and structurally characterized. Crystal structural analysis reveals that complex 1 adopts a 1D infinite chain structure which forms 2D sheet by hydrogen bonds interactions. Complex 2 possesses a 2D sheet structure, which was further assembled into a 3D supramolecular network through the π-π weak interactions. IR spectra indicates the carboxyl group coordinates with the Pb²⁺ ion. TGA shows that complex 2 is highly thermally stable up to 120°C.     

The crystal and molecular structure of spiro[1-(S)-Br-3-(S)-H-4-(R)-l-(1′ R,2′ S,5′R)-menthyloxy-5-oxo-6-oxa-bicyclo[3.1.0]hexane-2,3′-(R)-(4′-(R)-diphenylmethoxy-5′-l-(1′ R,2′ S,5′ R)-menthyloxy-butyrolactone)]

Crystal structure of C₄₁H₅₃O₇Br has been determined by single-crystal X-ray diffraction. The compound crystalline in the orthorhombic space group P2₁2₁2₁, with a = 11.264(2), b = 12.058(2), c = 29.337(6) Å, Z = 4. The bond angles of cyclopropane moiety in the molecule are approximate to 60° and agree with theoretic values of the internal angles in a cyclopropane, and two chiral menthyloxy groups are located above and under the whole chiral molecule, respectively. The configuration of the pentacyclic lactone is shown as envelope form.     

Structural investigation of (Z)-N-acetyl-β(3′-pyridyl)-dehydroalanine methyl ester

The crystal and molecular structure of the methyl ester of (Z)-N-acetyl-(3-pyridyl)-dehydroalanine [methylZ-2-acetamido-3(3-pyridyl) propenoate] have been determined from three-dimensional X-ray data. Crystals are monoclinic, space groupP2₁]. The molecular [=–51.5(5),=157.0(4)°] conformation is discussed making reference to previous experimental results of analogous amino acid derivatives (in particular, ethyl (Z)-N-acetyldehydrophenylalaninate) and theoretical predictions. On the basis of He(I) and He(II) photoelectron spectra, a similar conformation is proposed for the title molecule in the vapor phase also.     

Phenylmercury(II) dithiophosphates. Crystal structure of (O,O′-diethyldithiophosphate) phenylmercury(II)

The phenylmercury(II) derivatives PhHgS₂P(OR)₂ (R=C₂H₅, C₆H₁₁ and C₆H₅) have been synthesized. (O,O-diethyldithiophosphate) phenylmercury(II), C₁₀H₁₅HgO₂PS₂, crystallizes in the monoclinic space groupP2₁/c (n° 14) witha=7.330(5),b=18.085(2),c=11.552(4)Å,=105.96(5)°,V=1472.3(6)ų,Z=4,D=2.088 g.cm^–3. The mercury atom is coordinated to the phenyl carbon atom and to a ligand sulphur atom in an almost linear arrangement (C-Hg-S angle, 176.0(2)°. The ligand is almost monodentate, its second sulphur atom only being involved in a weak secondary intermolecular bond.IR and Raman studies of the other two compounds suggest the same coordination scheme. Positive ion FAB and¹³C,³¹P and¹⁹⁹Hg NMR spectra are also discussed.     

Synthesis and crystal structure of a new organic compound: Bis(4,4′-diaminodiphenylmethane) (4,4′-diammoniodiphenylmethane) dichloride monohydrate

A new organic compound with the formula C₃₉H₄₆Cl₂N₆O was synthesized from aqueous solution of 4,4′-diaminodiphenylmethane and hydrochloric acid at room temperature. This compound crystallizes in the monoclinic space group C2: a = 25.6525(16), b = 5.7107(3), c = 13.7777(8) Å, β = 118.862(2)°, V = 1767.64(22) ų and Z = 2, giving D _x = 1.288 g cm^?3. The refinement converged to R ₁ = 0.027 and wR ₂ = 0.0649. The structural arrangement can be described as infinite layers parallel to bc plane. In these layers cations and non protonated molecules are linked with N-H...N hydrogen bonds building [C₃₉H₄₄N₆]²⁺ organic clusters. These clusters, in turn, are linked by N-H...Cl and O-H...Cl hydrogen bonds.     

Structure of 2,2′-bis(3-allyl-4-cyanatophenyl)isopropylidene

The structure of the title compound (I) was determined by direct methods using MoK diffractometer data, and refined by full-matrix least squares toR=0.066 for 1536 reflections (I3 (I)). The structure shows a central tetrahedral carbon atom surrounded by two methyl and two 3-allyl-4-cyanatophenyl groups. The geometry of the cyanato group in this molecule compares well with those in 2,2-bis(4-cyanatophenyl)isopropylideneII) and 4-chloro-3,5-dimethyl-phenylcyanate (III), the only other examples of organic compounds bearing the cyanato moiety in the Cambridge Crystallographic Database (V.3).     

Molecular and crystal structure of two nickel(II) 1,2-dithiooxalato-S,S′ complexes using 1-(Rbenzyl)pyridinium cation (R = 4′-bromo-2′-fluoro or 4′-bromo)

[BrFPy]₂[Ni(dto)₂] (1) and [BrPy]₂[Ni(dto)₂] (2) complexes have been prepared by reaction of Na₂[Ni(S₂C₂O₂)₂] and the corresponding 1-(Rbenzyl)pyridinium bromide salt (R₁ = 4-bromo-2-fluoro, R₂ = 4-bromo). The crystallographic data for 1: monoclinic P2₁/c, a = 14.2192(1) Å, b = 14.2533(4) Å, c = 15.6535(3) Å, = 96.463(1)°, V = 3152.34(11) ų, Z = 4. Two cations, [Br₁F₁Py]⁺ and [Br₂F₂Py]⁺, both adopt a conformation where both the aromatic rings are twisted to the corresponding N(1)–C(10)–C(11) or N(2)–C(22)–C(23) reference plane. Data for 2: triclinic , a = 9.4042(3) Å, b = 9.6814(4) Å, c = 10.3357(4) Å, = 80.155(1)°, = 65.245(1)°, = 64.259(1)°, V = 769.68(5) ų, Z = 1. The [Ni(dto)₂]^2– anion exhibits a quasi-planar structure in both complexes. An extensive hydrogen bond network of C–H O is clearly observed in 1 and 2, and two complexes show similar crystal packing.     

PL Quenching of Poly(3-hexylthiophene) by 2,2′,7,7′-Tetradiphenylamino-9,9′-Bifluorenylidene

2,2′,7,7′-Tetradiphenylamino-9,9′-bifluorenylidene, TDPABF, was synthesized by reductive dimerization using Lawesson's reagent. It is soluble in common organic solvents such as dichloromethane, chloroform, and 1,2-dichlorobenzene. Its synthesis was confirmed by ¹H-, ¹³C- NMR, MALDI-TOF, and FT-IR spectroscopy. Its HOMO and LUMO energy levels were –5.33 eV and –2.98 eV, respectively, using photoelectron spectroscopy and UV-Vis absorption spectra. Its fluorescence quenching properties were investigated through a Stern-Volmer quenching experiment. The PL intensity significantly decreased on increasing the concentration of TDPABF in a P3HT chloroform solution. The calculated Stern-Volmer quenching constant was 9.1 × 10⁴ M^?1, which is higher than that reported for PC₆₁BM.