Synthesis,Crystal Structure and Fluorescent Study of Bis(2-(2-hydroxyphenyl)benzimidazolate)zinc with Ethanol Solvate

Abstract  The zinc(II) complex with 2-(2-hydroxyphenyl)benzimidazole, namely [Zn(2-(2-hydroxyphenyl)benzimidazolate)₂]·C₂H₅OH (1 · C₂H₅OH) has been synthesized and characterized by X-ray crystallography and photoluminescent analysis. The complex crystallizes in monoclinic space group P2₁/c with cell parameters a = 10.156(1) ?, b = 25.771(3) ?, c = 9.674(1) ?, α = 90°, β = 103.641(2)°, γ = 90°, Z = 4, V = 2460.4(4) ?³. The central Zn(II) is four-coordinate and has a tetrahedral geometry. The steady-state and time-resolved photoluminescent spectra for the title compound have also been studied. The emission property can be ascribed to ligand-centered charge-transfer transition (LCCT) with π → π* property. Index Abstract   A new co-crystal of Zn(II) complex of 2-(2-hydroxylphenyl)benzimidazole with ethanol solvate has been prepared, characterized by X-ray crystallography and fluorescent studies.      

Two Crystal Forms of 4-{(2<Emphasis Type="Italic">E</Emphasis>)-2-[1-(4-Methoxyphenyl)ethylidene] hydrazinyl}-8-(trifluoromethyl)quinoline

Abstract  

The Schiff base, 4-{(2E)-2-[1-(4-methoxyphenyl)ethylidene] hydrazinyl}-8-(trifluoromethyl)quinoline, crystallizes in two polymorphic forms depending on the solvent. One of these forms is monoclinic (1M), space group P2₁/c with a = 10.2906(10) ?, b = 8.9211(7) ?, c = 18.4838(15), β = 97.271(8)°, and the other is orthorhombic (1O), space group Pbca, unit-cell parameters: a = 13.6485(12) ?, b = 9.0588(9) ?, c = 27.400(2) ?. The molecules in either crystalline form have similar bond lengths and angles, but one is nearly planar while the other has a significant twist. In monoclinic form the dihedral angle between terminal ring planes is 17.26(8)° while in the orthorhombic one it is 26.11(5)°, and in this latter case the central chain is almost coplanar with the quinoline ring system while in the former these two planes are significantly twisted. The crystal structures of both forms are determined by the interplay of van der Waals forces and weak directional interactions C–H···F, π···π stacking, and—in the case of 1M—short intermolecular C–F···N contact. The crystals of 1M decomposes slowly into the powder while the other form is stable. The powder diffraction pattern of the product of decomposition of 1M is similar to that calculated for 1O. This suggests that the decomposition is a consequence of the phase transition of the less stable monoclinic into more stable orthorhombic form.     

The Crystal Structures of (Z)-Ethyl 2-(4-chlorophenyl)-3-(2,4-difluorophenyl-amino)acrylate and its Analogues

Abstract  

The title compound, C₁₇H₁₄ClF₂NO₂, crystallizes in monoclinic space group P2₁/c with unit cell dimension of a = 16.276(3) ?, b = 7.5030(15) ?, c = 13.812(3) ?, α = 90°, β = 111.11(3)°, γ = 90° and Z = 4. The structure of the title compound reveals a Z configuration with respect to the C=C double bond in aminoacrylate fragment. The molecule is stabilized by intramolecular N–H···F and N–H···O hydrogen bonds. In the ethyl 2-aryl-3-arylaminoacrylates, electronic properties of the substituents in the aniline motif clearly affected the attached C–N bond length, and such effect is very little relative to Z-/E-configuration with respect to the C=C double bond.     

Crystal Structures of 1,3,5-Tris(bromomethyl)-2,4,6-trimethylbenzene and 2,4,6-Trimethyl-1,3,5-tris(4-oxymethyl-1-formylphenyl)benzene

Abstract  

The synthesis and X-ray crystal structure of 2,4,6-trimethyl-1,3,5-tris(4-oxymethyl-1-formylphenyl)benzene (2) and the crystal structure of its core molecule, 1,3,5-tris(bromomethyl)-2,4,6-trimethylbenzene (1) are reported. The compounds 1 and 2 crystallize in the triclinic system with space group P ī. The lattice parameters of 1 and 2 are a = 9.454(2) ?, b = 9.478(4) ?, c = 9.573(2) ?, α = 116.53(2)°, β = 109.705(14)°, γ = 101.293(18)°, V = 658.5(4) and a = 15.7707(6) ?, b = 16.3646(5) ?, c = 18.2805(6) ?, α = 83.202(2)°, β = 66.0120(10)°, γ = 73.704(2)°, V = 4137.2(2), respectively. In the crystals of 1 and 2, there are one and three molecules in the asymmetric unit, respectively. The packing of the molecules in the solid is stabilized through van der Waals interactions in 1 and weak C–H···O and C–H···π interactions in 2.     

N–H···π Interactions in Two Isomers of an Amino Group Containing <Emphasis Type="Italic">bis</Emphasis>-Phenol

Abstract  

Crystal structures of two bis-phenols namely bis-(3,5-dimethyl-2-hydroxyphenyl)(3-amino phenyl)methane 1 and bis-(3,5-dimethyl-4-hydroxyphenyl)(3-aminophenyl) methane 2 are determined. The compound 1 crystallises in monoclinic P2₁/c with a = 12.2579(16) ?, b = 16.0906(19) ?, c = 10.6664(13) ?, β = 115.417(7)°, V = 1900.2(4) ?³ whereas 2 crystallizes in monoclinic C2/c, a = 9.2538(2) ?, b = 18.6579(4) ?, c = 23.2725(5) ?, β = 98.796(2)°, V = 3970.89(15) ?³. The crystal lattice of both the compounds shows presence of N–H···π interactions but no O–H···π interactions.     

Synthesis and Crystal Structure of a 3D Er(III) Coordination Polymer Based on Tripodal Flexible Ligand

Abstract  

Solvothermal reaction of Er(NO₃)₃·6H₂O and tri(2-carboxyethyl)isocyanurate (H₃tci) in DMF/H₂O (DMF = dimethylformamide) medium leads to the generation of one new 3D coordination polymer, [Er(tci)(H₂O)] DMF·2H₂O (1), which was characterized by the elemental analysis, IR spectroscopy and single crystal X-ray diffraction. X-ray diffraction analysis reveals that 1 crystallizes in triclinic space group P-1, features an interesting 3D coordination framework constructed from the flexible tridentate ligand H₃tci. Unit cell parameters for 1: a = 7.853(2) ?, b = 12.186(3) ?, c = 13.222(2) ?, α = 112.156(14)°, β = 105.457(15)°, γ = 91.541(18)° and Z = 2.     

Synthesis and Crystal Structures of Dioxomolybdenum(VI) Complexes with ONS-Donor Ligands

Abstract  

Three dioxomolybdenum complexes namely dioxo(5-chlorosalicylaldehyde thiosemicarbazonato) dimethylsulfoxide molybdenum(VI) (C1), dioxo(5-chlorosalicylaldehyde 2-ethylthiosemicarbazonato) dimethylsulfoxide molybdenum(VI) (C2) and dioxo(5-chlorosalicylaldehyde N-phenylthiosemicarbazonato) dimethylsulfoxide molybdenum(VI) (C3) were prepared. The compounds all crystallize in the triclinic space group P-1 with a = 7.3184(3) ?, b = 7.5035(3) ?, c = 14.9713(6) ?, α = 85.005(2)°, β = 85.616(2)°, γ = 66.987(2)° for C1, a = 8.2339(1) ?, b = 10.1739(1) ?, c = 10.4017(1) ?, α = 78.486(1)°, β = 89.312(1)°, γ = 81.730(1)° for C2, a = 7.0591(1) ?, b = 9.5603(1) ?, c = 14.5762(2) ?, α = 76.280(1)°, β = 81.351(1)°, γ = 81.985(1)° for C3. In general, the overall geometry of these complexes can be regarded as a distorted octahedron with the tridentate thiosemicarbazonato ligands (L²⁻) bonded to the MoO₂ ²⁺ core, with the imine nitrogen, phenoxyl oxygen, sulfur atom and one of the terminal oxygen atoms of the dioxomolybdenum occupying the equatorial position. The sixth coordination site is occupied by the dimethylsulfoxide (DMSO) solvent molecules. The adjacent molecules of C1 are linked by N–H···N intermolecular hydrogen bonding, forming polymeric chains that run parallel to the bc plane. On the other hand, C2 is a discrete molecule while the molecules of C3 associate via weak N–H···O hydrogen bonding interaction to form a polymeric chain that runs along the a-axis.     

Synthesis and Crystal Structure of Heptyl 3-(3,4-dihydroxyphenyl)-2-propenoate

Abstract  The title compound, C₁₆H₂₂O₄, synthesized by modified Knoevenagel condensation of protocatechualdehyde with monoheptyl-malonate and recrystallized from benzene, was confirmed by single-crystal X-ray diffraction (CCDC 272827). The compound crystallizes in triclinic space group Pī with cell parameters a = 5.296(3) ?, b = 10.711(13) ?, c = 13.870(4) ?, α = 98.84(7)°, β = 90.97(4)°, γ = 96.77(7)° and Z = 2. The structure is the E isomer and its packing is stabilized by intermolecular O–H···O and C–H···O hydrogen bonds. Index Abstract  The title compound, C₁₆H₂₂O₄, synthesized by modified Knoevenagel condensation, was confirmed by single-crystal X-ray diffraction showing its structure is in E isomer and its packing is stabilized by hydrogen bonds.      

Structures of Eight Thio(semi)carbazones Derived from 2-Acetylpyrazine, 2-Acetythiazole and Acetophenone

Abstract  The structures of eight related thio(semi)carbazones are described. These are syn,1E-2-acetylpyrazine-3-thiosemicarbazone (1), syn,1E,4Z-2-acetylpyrazine-4-ethyl-3-thiosemicarbazone, (2) and syn,1Z-2-acetylpyrazine-4,4-dimethyl-3-thiosemicarbazone (3), syn,1E,4Z-2-acetylthiazole-4-phenyl-3-thiosemicarbazone (4), syn,1Z-phenyl-4,4-dimethyl-3-thiosemicarbazone (5), syn,1E,4Z-phenyl-4-methyl-3-thiosemicarbazone (6), syn,1E,4Z-phenyl-4-ethyl-3-thiosemicarbazone (7), syn,1E,4Z-2-acetophenone-5-(N-aminothionyl)-3-thiocarbazone (8). Crystal data: for 1: triclinic, P-1, a = 5.4053(10) ?, b = 7.435(3) ?, c = 11.772(4) ?, α = 81.70(3)°, β = 82.59(2)°, γ = 77.38(2)°, and Z = 2: for 2: triclinic, P-1, a = 7.322(3) ?, b = 7.8239(16) ?, c = 9.783(4) ?, α = 87.73(2)°, β = 79.46(3)°, γ = 80.41(2)°, and Z = 2; for 3: orthorhombic, Pnma, a = 13.5210(15) ?, b = 6.6914(5) ?, c = 11.7214(10) ?, and Z = 4; for 4: triclinic, P-1, a = 5.7058(7) ?, b = 9.8776(15) ?, c = 11.869(2) ?, α = 76.389(12)°, β = 86.364(13)°, γ = 88.322(12)°, and Z = 2; for 5: triclinic, P-1, a = 7.5362(3) ?, b = 8.6331(4) ?, c = 9.8753(4) ?, α = 91.401(4)°, β = 102.532(4)°, γ = 110.540(4)°, and Z = 2; for 6: monoclinic, P2(1)/c, a = 10.7178(4) ?, b = 5.5866(2) ?, c = 18.7647(9) ?, β = 104.392(5)°, and Z = 4; for 7: monoclinic, P2(1)/c, a = 8.9557(3) ?, b = 9.7418(4) ?, c = 13.6864(5) ?, β = 94.044(4)°, and Z = 4; for 8: triclinic, P-1, a = 9.8091(5) ?, b = 10.6173(4) ?, c = 16.4691(7) ?, α = 75.540(4)°, β = 80.305(4)°, γ = 65.192(4)°, and Z = 4. Structures 1, 2, 4, 5, 7, and 8 form intramolecular N4–H···N1 hydrogen-bonds. Structures 3 and 5 exist in the tautomeric form in which N1 is protonated. Graphical Abstract  Structures of thio(semi)carbazones were found to fall into two categories: those with intramolecular N4-H…N1 hydrogen-bonds, and those which show a tautomeric form in which N1 is protonated.      

Crystal and Molecular Structure of the 1:2 Salt Formed Between 1,2-(4-Pyridyl)Ethane and 2-(4-Hydroxyphenylazo)Benzoic Acid

Abstract  Proton transfer occurred during co-crystallization of 1,2-(4-pyridyl)ethane with 2-(4-hydroxyphenylazo)benzoic acid to yield a salt comprising a 1:2 ratio of 1,2-bis(4-pyridinium)ethane dications and 2-(4-hydroxyphenylazo)benzoate anions. Centrosymmetrically related anions associate by charge-assisted O–H···O hydrogen bonds to form 24-membered {···OC₃N₂C₄OH}₂ synthons. These are connected into a supramolecular polymer via charge-assisted N–H···O hydrogen bonds involving the 1,2-bis(4-pyridinium)ethane dications. The compound crystallizes in the triclinic space group P−1 with a = 8.517(4) ?, b = 9.110(5) ?, c = 10.477(5) ?, α = 96.850(13)°, β = 94.446(12)°, γ = 104.946(10)° and Z = 1 {two anions and a dication}. Index Abstract  Supramolecular chains mediated by charge-assisted O–H···O and N–H···O hydrogen bonding are found in the salt containing a 1:2 ratio of 1,2-bis(4-pyridinium)ethane dications and 2-(4-hydroxyphenylazo)benzoate anions.      

Structures of two N-{2-([(5-amino-1,3,4-thiadiazol-2-yl)difluoromethyl]-4-halophenyl}acetamides

Abstract  

The compounds, N-{2-[(5-amino-1,3,4-thiadiazol-2-yl)difluoromethyl]-4-chlorophenyl}acetamide (1: X = Cl) and N-{2([(5-amino-1,3,4-thiadiazol-2-yl)difluoromethyl]-4-bromo-phenyl}acetamide (1: X = Br), are isostructural. The molecules are near ‘‘V’’ shaped with the angles between the two aromatic planes ca. 84° in each case. The various intermolecular interactions, namely N–H···O, N–H···N, N–H···F, and C–H···N hydrogen bonds and C–H···π, C–Cl···π and C–O···π interactions, generate 3-D arrays. Compound (1: X = Cl) crystallizes in the monoclinic space group P21/c with a = 16.9032(7) ?, 10.2193(4) ?, c = 7.5227(4) ?, β = 100.179(3)° and Z = 4. Compound (1: X = Br) crystallizes in the monoclinic space group P21/c with a = 17.2119(4) ?, 10.2167(2) ?, c = 7.5677(2) ?, β = 100.326(2)° and Z = 4.     

Crystal Structures of 1,7-Bis(furyl)-4-(1,3-dithiolan-2-ylidene)-1,6-heptadiene-3,5-dione and 1,7-bis(thienyl)-4-(1,3-dithiolan-2-ylidene)-1,6-heptadiene-3,5-dione

Abstract  

The title compounds (bis(alkenoyl) ketene dithioacetals) were prepared starting from the cyclic acyl ketene dithioacetal and aromatic aldehydes. These compounds were characterized by IR, ¹H NMR, mass spectral studies and X-ray crystal structure analysis. The bis(furyl) ketene dithioacetal crystallized in the space group P[`\text1] P{\bar{\text{1}}} with unit cell dimensions a = 7.7626(12) ?, b = 9.0217(13) ?, c = 26.827(5) ?, α = 86.271(14)°, β = 87.643(14)°, γ = 66.286(11)° and the structure was refined to an R-factor of 0.0528 while bis(thienyl) ketene dithioacetal crystallized in the space group P2₁/c with unit cell dimensions a = 10.2433(9) ?, b = 10.4142(6) ?, c = 18.0973(18) ?, β = 106.0° and the structure was refined to an R-factor of 0.0446. The ketenedithioacetal functionality present between the carbonyl groups prevents the possibility of keto-enol tautomerization in these compounds. In both the crystal structures, the crystal packing is stabilized by C–H···O hydrogen bonds as well as van der Waals interactions.     

Crystal and Molecular Structure of (S)-N-(2-Hydroxyphenyl)pyrrolidine-2-carboxamide

Abstract  

(S)-N-(2-Hydroxyphenyl)pyrrolidine-2-carboxamide was synthesized from Cbz-l-proline through two steps and characterized by NMR and MS. The crystal structure was determined from single-crystal X-ray diffraction data. It crystallizes in the monoclinic space group, P2₁, with unit cell dimensions a = 7.284(6) ?, b = 10.262(9) ?, and c = 7.975(7) ?, α = 90.00°, β = 114.451(14)°, γ = 90.00° and Z = 2. The absolute configuration of the chiral center is determined as S. In the crystal structure, intermolecular and intramolecular hydrogen bonds are responsible for the formation of a 1-dimensional network.     

Synthesis,Crystal Structure and Thermal Properties of <Emphasis Type="Italic">N</Emphasis>-Acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline and <Emphasis Type="Italic">N</Emphasis>-Acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline

Abstract  

Two novel ferrocenyl substituted N-acetyl-2-pyrazolines, N-acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline (3) and N-acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline (4), have been synthesized and characterized by FTIR, ¹H-NMR, ¹³C-NMR techniques, elemental analysis and X-ray structure analysis. Thermal properties of these compounds have been determined by TGA, DTA and DSC analysis. Compound 3 (C₁₉H₁₈N₂O₂Fe) crystallizes in the monoclinic space group P21/c and Z = 4, with a = 8.6970(4) ?, b = 18.4725(9) ?, c = 11.0041(5) ?, β = 110.942(3)°. Compound 4 (C₁₉H₁₈N₂OSFe) crystallizes in the orthorhombic space group Fdd2 and Z = 16, with a = 84.242(2) ?, b = 13.5416(5) ?, c = 5.9405(2) ?, β = 90°. In terms of crystal packing, each compound shows different molecular arrangement, which are stabilized by C–H···O intermolecular weak hydrogen bonds, and/or C–H···π interactions.     

Synthesis, Crystal and Molecular Structure of 1-(2-Chlorobenzyl)-2-methylthio-1H-benzimidazole

Abstract  

1-(2-Chlorobenzyl)-2-methylthio-1H-benzimidazole compound has been synthesized and characterized by elemental analysis, IR and ¹H-NMR spectroscopy and single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P-1 with unit cell parameters a = 17.201 ?, b = 5.873 ?, c = 24.791 ?, α = 67.410(10)°, β = 74.083(11)°, γ = 81.858(12)°. In the crystal packing, no classic hydrogen bonds are founded, but C–H···π interactions are being between the molecules. The molecular geometry and vibrational frequencies of (C₁₅H₁₃ClN₂S) in the ground state have been calculated by using Hartree–Fock (HF) and Density Functional Method (DFT/B3LYP) with 6-31G(d) basis set. The optimized geometric bond lengths and bond angles obtained by using HF and DFT (B3LYP) show the best agreement with the experimental data.     

The Zolmitriptan-Pyridine (1:1) and Zolmitriptan-Propiophenone (3:2) Inclusion Complex

Abstract  

The crystal structures of zolmitriptan with pyridine (I) and propiophenone (II) solvates have been determined by single crystal X-ray diffraction studies. Compound (I) crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 8.5610(5) ?, b = 12.2709(7) ?, c = 19.6201(12) ?, V = 2061.1(2) ?³, and Z = 4, while compound (II) crystallizes in the monoclinic space group P2₁ with a = 15.085(1) ?, b = 19.656(12) ?, c = 21.0860(13) ?, β = 92.068(1)°, V = 6248(4) ?³ and Z = 4. The asymmetric unit of (I), C₁₆H₂₁N₃O₂·C₅H₅N, contains one zolmitriptan molecule and one pyridine solvate, while the asymmetric unit of (II), 3(C₁₆H₂₁N₃O₂)·2(C₉H₁₀O) comprises six zolmitriptan molecules and four propiophenone solvates. In both structures, the N–H···N hydrogen bonds, form an infinite helical chain and generate a C(11)-type motif in (I) and a D₂²(13)-type motif in (II). Both the complexes have layer structures, the layers being constructed from rings (cavity) of four zolmitriptan molecules, hydrogen bonded through N–H···N and N–H···O bonds, where the pyridine (I) and propiophenone (II) solvates are included in an R₄⁴(33) ring.     

Synthesis,Crystal Structure and Luminescent Properties of One Silver Complex with 3,5-Diphenylpyrazole

Abstract  

A new Ag(I) complex Ag(HL)₂(NO₃) 1 has been synthesized with 3,5-diphenylpyrazole (HL) and characterized by IR spectrum, elemental analysis and X-ray crystallography. The crystallographic data for the complex 1: triclinic P[`\text1] P{\bar{\text{1}}} , a = 10.4369(17) ?, b = 10.4837(18) ?, c = 12.963(2) ?, α = 69.318(2)°, β = 86.733(3)°, γ = 88.263(2)°, V = 1324.7(4) ?³, Z = 2, Dc = 1.530 Mg m⁻³, F(000) = 620, μ = 0.803 mm⁻¹, R ₁ = 0.0251, wR ₂ = 0.0638. Ag(I) atom is bound to two nitrogen atoms from two ligands. In solid state there are π···π interactions and C–H···π interactions between adjacent units to generate 2D supramolecular structure. The title complex shows strong luminescent emission at 389 and 467 nm in solid state at room temperature.     

Synthesis,Crystal Structure and Biological Activity of Two 1,2,3-Thiadiazole Derivatives

Abstract  

The title compounds, quinolin-8-yl 4-methyl-1,2,3-thiadiazole-5-carboxylate 2a and 2-nitrophenyl 4-methyl-1,2,3-thiadiazole-5-carboxylate 2b, synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 8-hydroxyquinoline and 2-nitrophenol, were confirmed by single-crystal X-ray diffraction [CCDC 783328 and 784970]. The 2a crystallizes in triclinic space group P-1 with cell parameters a = 7.957(7) ?, b = 8.378(7) ?, c = 10.097(10) ?, α = 100.63(2)°, β = 112.742(17)°, γ = 93.287(4)° and Z = 2. The 2b crystallizes in triclinic space group P-1 with cell parameters a = 7.134(4) ?, b = 8.154(4) ?, c = 10.254(5) ?, α = 99.501(9)°, β = 91.311(7)°, γ = 109.518(8)° and Z = 2. Packing in the compound 2a is dominated by weak C–H···N and C–H···O hydrogen bonds. In the compound 2b, molecules are linked through intermolecular C–H···O hydrogen bonds interactions. The preliminary bioassay showed that the title compound 2a had excellent antifungal activity with the EC₅₀ detected as from 2.99 to 28.35 μg/mL and the EC₉₀ detected as from 21.041 to 175.17 μg/mL. Both of the title compounds 2a and 2b had good inhibition activity of tobacco mosaic virus (TMV) and good induction activity of tobacco against TMV with potential systemic acquired resistance.     

Synthesis and Crystal Structure of Three New Metal-Organic Frameworks in the Ln(III)/2,6-Pyridinedicarboxylate System

Abstract  

In this paper, three new metal-organic frameworks, synthesized by hydrothermal technique, are described. The compounds crystallize in triclinic space group P − 1 with cell parameters, respectively equal to (1) [La(H₂O)₃(dipic)]₂(C₂O₄) · 2H₂O a = 7.9990(1) ?, b = 8.3380(4) ?, c = 9.6180(5) ?, α = 98.194(5)°, β = 100.438(3)°, γ = 102.437(3)°, (2) [Eu(H₂O)₂(C₂O₄)]₂(dipic) · 3H₂O a = 8.2170(6) ?, b = 10.5900(8) ?, c = 13.0670(3) ?, α = 93.951(3)°, β = 103.393(5)°, γ = 107.797(6)°, and (3) [Ce₃(dipic)₃(Hdipic)(SO₄)(H₂O)₃] · 4H₂O a = 11.655(1) ?, b = 12.886(1) ?, c = 16.139(2) ?, α = 106.369(8)°, β = 92.90(1)°, γ = 115.787(7)°. They differ by their dimensionality mono-dimensional for (1), tri-dimensional for (2) and bi-dimensional for (3).     

Crystal Structures of N-(4-butyryl-3-hydroxyphenyl)acetamide Monohydrate and 4-(4-Chlorophenyl)-2-methyl-4-oxobutanoic Acid: Possibilities of Yang Photocyclization

Abstract  

N-(4-butyryl-3-hydroxyphenyl)acetamide monohydrate, (I), and 4-(4-chlorophenyl)-2-methyl-4-oxobutanoic acid, (II), are photochemically inert, which is a result of their conformation. The geometrical parameters describing the molecular conformation and possibilities of the Yang photocyclization in crystals have been calculated and discussed. Compound (I) forms double ribbons along the a axis, stabilized by hydrogen bonds and π⋯π interactions. Compound (II) forms dimers. (I): triclinic, space group \textP[`1] {\text{P}}\bar{1} , a = 6.9291(12) ?, b = 7.5736(16) ?, c = 13.0528(18) ?, α = 79.643(17)°, β = 85.818(15)°, γ = 63.97(2)°, Z = 2. (II): monoclinic, space group P2₁/c, a = 11.904(2) ?, b = 9.6508(12) ?, c = 10.666(2) ?, β = 110.64(2)°, Z = 4.