Crystal Structure of 1,7-Bis(4-chlorophenyl)-4-(1,3-dithiolan-2-ylidene)-1,6-heptadiene-3,5-dione

Abstract  The synthesis and crystal structure of 1,7-bis(4-chlorophenyl)-4-(1,3-dithiolan-2-ylidene)-1,6-heptadiene-3,5-dione is described. This compound is a curcuminoid analogue, configurationally symmetric about the C4–C5 atoms and also retains the two fold axis in the crystal phase. This compound crystallizes in the space group C2/c with unit cell parameters a = 19.203(1) ?, b = 13.147(1) ?, c = 8.801(1) ?, β = 112.99(1)°, with half a molecule in the asymmetric unit. The ketenedithioacetal functionality present between the carbonyl groups prevents the possibility of keto-enol tautomerization in this compound. The push-pull nature of the ketenedithioacetal functionality organizes the cinnamoyl groups parallel to each other. Index Abstract  The details regarding synthesis and crystal structure of the title compound which is a curcuminoid analogue is reported in this paper.      

Synthesis and Crystal Structure of 1,7-Bis(4-methoxyphenyl)-4-(1,3-dithiolan-2-ylidene)-1,6-heptadiene-3,5-dione

Abstract  

The synthesis and crystal structure of 1,7-bis(4-methoxyphenyl)-4-(1,3-dithiolan-2-ylidene)-1,6-heptadiene-3,5-dione is described. This compound crystallizes in the space group P2₁ with unit cell parameters a = 14.207 ?, b = 7.752(1) ?, c = 19.473(1) ?, β = 91.00(3)°, with two molecules in the asymmetric unit. The ketenedithioacetal functionality present between the carbonyl groups prevents the possibility of keto-enol tautomerization in this compound. The cinnamoyl groups are organized parallel to each other due to the push–pull nature of the ketenedithioacetal functionality.     

Knoevenagel condensation of the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopentene-1,3-dione with 9-anthracenecarboxaldehyde: Synthesis of the second-generation ligand 2-(anthracen-9-ylidene)-4,5-bis(diphenylphosphino)-4-cyclopentene-1,3-dione

The Knoevenangel condensation between 9-anthracenecarboxaldehyde and the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopentene-1,3-dione (bpcd) takes place rapidly in CH₂Cl₂/MeOH solution in the presence of molecular sieves (4 ?) to produce the functionalized ligand 2-(anthracen-9-ylidene)-4,5-bis(diphenylphosphino)-4-cyclopentene-1,3-dione. The title compound has been isolated and characterized in solution by IR, NMR, and UV-vis spectroscopies, and the solid-state structure has been established by X-ray diffraction analysis. 2-(anthracen-9-ylidene)-4,5-bis(diphenylphosphino)-4-cyclopentene-1,3-dione crystallizes in the triclinic space group P−1, a=10.227(2) ?, b=13.865(2) ?, c=15.905(2) ?, α=112.157(2)°, β=101.424(2)°, γ=100.065(3)°, V=1968.5(5) ?³, Z=2, and d _calc=1.101 Mg/m³; R=0.0873, R _w=0.2604 for 7452 reflections with I>2σ(I). The cyclic voltammetric behavior for 2-(anthracen-9-ylidene)-4,5-bis(diphenylphosphino)-4-cyclopentene-1,3-dione has been studied, and the observed redox data and results from extended Hückel MO calculations are discussed relative to the parent ligand bpcd.

Synthesis,Characterization and Crystal Structure of 4,5-Bis(Cyclohexanecarbonylthio)-1,3-dithiolane-2-thione Crystal

Abstract  

A new crystal of 4,5-bis(cyclohexanecarbonylthio)-1,3-dithiolane-2-thione has been prepared at room temperature and characterized by elemental analysis, UV–Vis–NIR absorption spectrum and X-ray single crystal determination. The complex crystallized in triclinic space group P-1 with unit cell dimensions a = 5.37370(10) ?, b = 12.8618(2) ?, c = 15.2481(2) ?, α = 74.8530(10)°, β = 80.6000(10)°, γ = 85.9550(10)°, V = 1003.18(3) ?³, Z = 2, D _x = 1.3861(1) g cm⁻³. The X-ray structure determination revealed that the crystal is centered-symmetrical and the molecules form dimers with a long intermolecular S···S interaction in the crystal.     

Crystal and molecular structure of the unreactive form of 1,8-bis (p-chlorophenyl)-octa-1,7-diene-3,5-diyne

The title compound (C₂₀ H ₁₂Cl₂,M _r =322, mp 69–70°C) crystallizes in the monoclinic system, space groupP2₁/n, witha=3.942(2),b=6.887(2),c=28.701(4) Å,=91.362(4)°,V _c =778.93(2) ų,Z=2,D _c =1.373,D _m =1.370(1) (in C₆H₆/CCl₄) g cm^–3,F(000)=332 and (MoK)=3.57 cm^–1. The final residuals areR=0.0365 andR _w =0.0368 for 999 observed reflections at the levelI3(I). The molecule as a whole is found to havetrans conformation. This structural study reveals that the title compound does not undergo solid-state polymerization due to close packing.     

Crystal and molecular structure of (Z)-2-(1,3-benzothiazol-2-yl)-2-(6,7,8,9-tetrahydro-5H-benzocyclohepten-5-ylidene)ethanonitrile

The title compound C₂₀H₁₆N₂S is crystallized in the monoclinic space groupP2₁/c with cell parametersa=10.663(4),b=17.585(9),c=9.418(5)Å,=115.23°(4),V=1598(3)ų,Z=4. The structure was refined by full-matrix least-squares methods using X-ray data set collected at room temperature. A finalR _F =0.033 andR _w =0.048 for 2225 unique reflections withI> 3(I) and 272 variables was obtained. The X-ray crystallographic study establishes theZ stereochemistry of the title compound.     

Synthesis and Crystal Structure of 1,3-Bis[2-(pyrrol-2-carbonyloxy)ethoxy]Benzene

Abstract  

A new compound, 1,3-bis[2-(pyrrol-2-carbonyloxy)ethoxy]benzene (1), was synthesized and characterized by X-ray diffraction. The crystal is monoclinic, space group P2₁/c with a = 6.3571(7), b = 11.0416(11), c = 28.156(3) ?, b = 92.821(2), V = 1974.0(4) ?³, Z = 4, Dc = 1.293 g/cm³, F(000) = 808, μ = 0.097 mm⁻¹. The final R = 0.0395 and wR = 0.0927 for 3478 observed reflections with I > 2 σ(I), and R = 0.0660 and wR = 0.1058 for all reflections. The title compound assembles into 2-D structure through a catemer type N–H⋯O hydrogen bonding motif and further forms 3-D structure through C–H···O hydrogen bonds.     

Crystal structure ofcis-bis[1-(2-thienyl)-4, 4,4-trifluoro-1,3-butanedionato]-bis (4-methylpyridine)nickel(II)

The crystal structure of the 4-methylpyridine adduct of bis[1-(2-thienyl)-4, 4,4-trifluoro-1,3-butanedionatolnickel(II) was determined by a three-dimensional x-ray analysis using counter data. The crystals are monoclinic,C2/c, witha = 9.330,b = 18.278,c = 17.855 Å, and = 95.1°. The structure was refined by full-matrix least squares toR = 0.10. The molecule has a two-fold axis, and both enantiomers withcis configuration occur in the crystal. The solvation by 4-methylpyridine is shown to weaken the chelate bonds in the same way as doestrans hydration.     

Crystal Structures of 2-Chloro-3-((3-(trifluoromethyl)phenyl)amino)naphthalene-1,4-dione and 2-Chloro-3-((4-(trifluoromethyl)phenyl)amino)naphthalene-1,4-dione

Crystallography Reports - 2-Chloro-3-((3-(trifluoromethyl)phenyl)amino)naphthalene-1,4-dione (1) and 2-chloro-3-((4-(trifluoromethyl)phenyl)amino)naphthalene-1,4-dione (2) were obtained according...     

Crystal structures of two azo compounds, 2-methyl-2-(4-bromphenylazo)-1,3-indandione and 2-methyl-2-(4-ethoxyphenylazo)-1,3-indandione

In the two title compounds, the 2-methyl-1,3-dioxoindan-2-yl and 4-(brom; ethoxy) phenyl groups aretrans with respect to one another. The phenyl ring and the azo group are not coplanar in the two molecules. The five-membered rings of the two compounds adopt an envelope conformation. The crystallographic parameters are as follows: 2-Methyl-2-(4-bromphenylazo)-1,3-indandione (I): monoclinic, P2₁/a witha=8.098(2),b=14.442(2),c=12.554(1)Å, =100.55(2)^o, andD _calc=1.58 g cm^–3 forZ=4; 2-methyl-2-(4-ethoxyphenylazo)-1, 3-indandione (II): monoclinic, P2₁/a witha=8.258(2),b=14.449(1),c=13.559(2)Å, =101.19(1)^o, andD _calc=1.29 g cm^–3 forZ=4.     

1,3-Bis(4-Pyridinylcarbonyl)-2-Imidazolidinethione and Its First Cluster Complex: Synthesis,Crystal Structure and Luminescence Properties

Abstract  The first cluster complex of 1,3-bis(4-pyridinylcarbonyl)-2-imidazolidinethione (4-bpit) with CuI was prepared and characterized. Single crystal X-ray diffraction analysis established that the compound crystallizes in the monoclinic system, space group C2/m, with a = 15.601(3), b = 12.438(3), c = 12.570(3)?, β = 110.02(3), Z = 4, V = 2291.8(8)?³. This compound is also a coordination polymer with one-dimensional double-ribbon structure containing the adaptable rhomboid Cu₂I₂ cluster unit. The solution-state luminescence spectra showed that the high-energy emission may be associated with a ligand-to-ligand charge-transfer excited state. Graphical Abstract  The first cluster complex of 1,3-bis(4-pyridinylcarbonyl)-2-imidazolidinethione (4-bpit) with CuI was prepared and characterized. This compound is also a coordination polymer with one-dimensional double-ribbon structure containing the adaptable rhomboid Cu₂I₂ cluster unit. The solution-state luminescence spectra showed that the high-energy emission may be associated with a ligand-to-ligand charge-transfer excited state.     

Synthesis and Crystal Structure of 1,3-Bis(p-nitrophenoxy)propane

Abstract  The title compound 1,3-bis(p-nitrophenoxy)propane was synthesized by nucleophilic substitution of p-nitrophenol and 1,3-dibromopropane. Single crystal X-ray diffraction analysis reveals that the molecule in the solid state packs in the monoclinic P2/n space group with crystal cell parameters a = 17.465(5) ?, b = 4.8433(13) ?, c = 17.610(5) ?, β = 100.290(6)o, V = 1465.6(7) ?³, D_calc = 1.442 g/cm⁻³. Two half-molecules are located in the asymmetric unit which are each completed by twofold symmetry making Z = 4, Z′ = 1. Index Abstract  The title compound 1, 3-bis (p-nitrophenoxy) propane was prepared from p-nitrophenol and 1, 3-dibromopropane, crystallized from an ethanolic solution, and the structure was obtained by single crystal X-ray diffraction: monoclinic, P2/n, a = 17.465(5) ?, b = 4.8433(13) ?, c = 17.610(5) ?, β = 100.290(6)°, V = 1465.6(7) ?³.      

Crystal and molecular structure of 2-(1,3-benzothiazol-2-yl)-2-(4-tert-butylcyclohexylidene)ethanonitrile

The crystal and molecular structure of the title compound (C₁₉H₂₂N₂S) has been investigated by single crystal X-ray methods. The crystals are orthorhombic, space groupPbca, with cell dimensions:a=12.082(2)Å,b=11.460(2)Å,c=25.128(4)Å. The structure was solved by direct methods, and refined with 1225 independent reflections by a full-matrix, least-squares procedure, which converged toR=0.042. The benzene and thiazole planes are coplanar and the cyclohexane ring adopts a chair conformation.     

4-(2,3-Dichlorophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-bis(methoxycarbonyl), 4-(2,4-dichlorophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-bis(methoxycarbonyl), and 4-(2,3,5-trichlorophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-bis(methoxycarbonyl): conformational observations in the crystalline state

Hydrogen bonding interactions displayed by three crystalline chloro-substituted 4-phenyl-1,4-dihydropyridine molecules 4-(2,3-Dichlorophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-bis(methoxycarbonyl), 4-(2,4-dichlorophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-bis (methoxycarbonyl) and 4-(2,3,5-trichlorophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-bis (methoxycarbonyl), suggests that, in contrast to previous observation, sp orientation of the 3 or 5 substituted carbonyl group accomodates hydrogen bonding to the carbonyl oxygen atom when polar orthosubstituents exist on the phenyl ring.     

Structure of 2-(1-phenylimidiazolidin-2-ylidene)- malononitrile and 2-(hexahydropyrimidinyl-2-ylidene)- malononitrile

The crystal structure of 2-(1-phenylimidazolidin-2-ylidene)-malononitrile, I, and 2-(hexahydropyrimidin-2-ylidene)-malononitrile, II, were determined with crystal data (I: Monoclinic, P2₁/n, a=8.116(3) ?, b=7.650(3) ?, c=17.399(7) ?, β=93.065(6)°, R _all=0.0980; II: Monoclinic, P2₁/n, a=9.169(2) ?, b=8.103(2) ?, c=10.337(3) ?, β=99.853(4)°, R _all=0.0877). N−H···N hydrogen bonds were responsible for the formation of centrosymmetric dimers of I and one-dimensional zigzag molecular chains of II.     

4-(2-Methylphenyl)-1,2,3,4,5,6,7,8-octahydroquinazoline-2,5-dione (I) and 4-(4chlorophenyl)-1,2,3,4,5,6,7,8-octahydroquinazoline-2,5-dione (II)

The crystal and molecular structures of the title compounds have been determined by x-ray structure analysis. The compounds (I) and (II) crystallize in space groups P2₁2₁2₁ and 12/a respectively. The structures were solved by direct methods and refined to R = 0.058 and R = 0.046. The saturated pyrimidine-2-one ring in both structures deviates from the planarity. There are two intermolecular hydrogen bonds in (I) and (II). The configuration at C4 in (I) is S.