Synthesis,Characterization, Crystal Structure,and Thermal Analysis of 4-[(3-acetylphenyl)amino]-2-methylidene-4-oxobutanoic Acid

4-[(3-Acetylphenyl)amino]-2-methylidene-4-oxobutanoic acid (1) is synthesized by a ring opening reaction of itaconic anhydride with 3-aminoacetophenone and characterized by FT-IR, ¹H NMR, UV-Vis, TGA, DTA, and single crystal X-ray diffraction. The crystal of 1 belongs to triclinic unit cell in the P-1 space group with the unit cell dimensions a = 4.9485(3), b = 5.3614(6), c = 22.457(2) Å, α = 88.295(8), β = 89.379(7), γ = 84.495(7), and Z = 2 The crystal structure is solved by direct methods using single-crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R-value of 0.0467 for 1623 observed reflections. Intermolecular N&;sbnd;H?…O and O&;sbnd;H?…O hydrogen bonds links the molecules into chains along [010] direction. In addition the thermal stability of the 1 is determined by using DTA, TGA analysis, and wavelength absorption at λ_max = 297 nm is determined by UV-Vis spectrophotometer.     

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 Methyl and Ethyl N-(2,3-Dimethoxybenzyl)-N-(p-toluenesulfonyl)-2-phenylglycinates

The crystal structures of methyl and ethyl N-(2,3-dimethoxybenzyl)-N-(p-toluenesulfonyl)-2-phenylglycinates 4a and 4b respectively, have been determined by X-ray diffraction analysis. The presence of different alkyl ester groups in both molecules does not affect the geometry retaining a synclinal conformation for the N atom and the O atom of the C=O group [N—C17—C18—O5 38.1(5)° for 4a and 33.3(4)° for 4b ].     

Crystal structure and spectroscopic study of 2-[(2,6-dichlorophenyl)amino]phenylacetoxyacetic acid (Aceclofenac)

The crystal structure of the title compound has been determined. The crystals are monoclinic:P2₁ n(NO. 14),a=12.279(7),b=8.223(1),c=15.504(7)Å,=96.16(2)°,V _c =1556(2)ų,Z=4,D _x =1.511 g cm^–3,=(MoK)=0.71069 Å. The structure was solved by direct methods and refined with 1970 reflections to a finalR value of 0.057. Analytical, mass, spectral, and physicochemical data are also reported.     

Crystal and molecular structure of 2-chloro-4-methyl-6-[[(4-)2,2,6,6,-tetramethylpiperidinyl]amino]-3-pyridinecarbonitrile hydrochloride

The compound C₁₆H₂₄N₄Cl₂ crystallizes in the monoclinic space groupP2 ₁/c witha=16.299(2),b=7.801(1),c=14.780(2) Å,=109.89(1)° andZ=4. The structure was determined by direct methods, and refined by full-matrix least squares toR=0.046 andR _w=0.050 for 2309 reflections. The resulting structure permitted the determination of the main direction of substitution during the synthesis of this compound, and correction of a previously postulated formulae of the dyes formed. The influence of salt formation on the protonation of the N atom and on the formation of hydrogen bonds is analyzed. The influence of substituents on the geometry of pyridine and piperidine ring is discussed.     

Synthesis and Crystal Structures of 4-(3-Nitropyridin-2-ylamino)phenol and 4-(3-Aminopyridin-2-ylamino)phenol

Abstract  

The title compounds, 4-(3-nitropyridin-2-ylamino)phenol (I) and 4-(3-aminopyridin-2-ylamino)phenol (II), are two intermediates for the synthesis of a potential antitumor agent ABT-751. The reaction of 4-aminophenol with 2-chloro-3-nitropyridine yielded I which was converted into II by reduction. Instead of the Pd/C catalytic hydrogenation described in many literature, reduction with cheap sodium sulfide in aqueous media was utilized for shorting the reaction time and simplifying the operation. The crystal structures of the resultant compounds were determined by single-crystal X-ray diffraction. The compound I is crystallized in P2₁/c space group of monoclinic system, with a = 11.5236(19) ?, b = 8.7389(17) ?, c = 10.684(3) ? and α = 90.00°, β = 107.76(3)°, γ = 90.00°. The compound II is crystallized in Cc space group of monoclinic system, with a = 10.688(2) ?, b = 14.2181(18) ?, c = 7.9836(15) ? and α = 90.00°, β = 125.801(7)°, γ = 90.00°. In both crystal structures, the intermolecular N–H–O and O–H–N hydrogen bonds link the molecules, which effectively stabilize the structures.     

Crystal structure of 2-{(R)-1-hydroxy-1-[(2S)-1-tritylaziridin-2-yl] methyl}acrylate and spectroscopic properties of the (R,S) and (S,S) stereoisomers

The crystal and molecular structure of 2-{(R)-1-Hydroxy-1-[(2S)-1-tritylaziridin-2-y1] methy1}acrylate is described. Crystal data: C₂₆H₂₅NO₃, orthorhombic, space group P2₁2₁2₁, a = 9.6954(5), b = 13.1458(5), c = 16.7885(7) Å, V = 2139.8(2) ų, Z = 4. The (R,S) diastereomer shows an intramolecular hydrogen bonding N···H—O under formation of a five-membered ring with N···O distance of 2.664 Å. IR, ¹H NMR and ¹³C NMR data are discussed. The ¹H NMR of the (R,S) diastereomer shows a singlet- whereas the (S,S) diastereomer exhibits a doublet-pattern for the hydroxyl proton.     

Crystal structure of 1,3-di-2-[(4-methoxyphenyl)-1-diazenyl]imidazolidine

The crystal and molecular structure of 1,3-di-2-[(4-methoxyphenyl)-1-diazenyl]imidazolidine (1) has been determined by single crystal X-ray diffraction analysis. This novel bis-triazene assumes a close-to planar structure with the aryltriazene moieties aligned in diametrically opposed directions, unlike many other previously reported bis-triazenes, which assume a folded structure. The structure of 1 is compared with the closely related, non-cyclic bis-triazene analogue (2), and also compared with the structure of the simple mono-triazene (3). Crystal data: 1 C₁₇H₂₀N₆O₂, monoclinic, space group C2/c, a = 34.948(3), b = 5.925(5), c = 8.1225(6) Å, = 100.8420(10)°, and V = 1652.0(2) ų, for Z = 4.     

Crystal and molecular structure ofcis-dicarbonyltetraphosphinechromium(O), [(CO)2(PH3)4Cr]

The crystal and molecular structure ofcis-dicarbonyltetraphosphinechromium(O), [(CO)₂(PH₃)₄Cr] has been determined by X-ray diffraction methods. The compound crystallizes in the monoclinic system: space groupC2/c,a = 6·968(6),b = 11·98(1),c = 12·87(1) Å, = 99·80(8) °,V= 1059(3) ų,Z=4,D _m = 1·534(5),D _x = 1·531(5) gcm^–3, diffraction symmetry 2/m. The structure was solved by conventional methods, and refined by least-squares techniques to an agreement factorR = 0·078. The chromium atoms lie on rotation diads, and thus the molecules must have at least the symmetry 2(C ₂); they were found to have, within the limits of accuracy, the even higher symmetrymm2 (C _2v ). There are two distinct independent Cr-P distances in the molecule, the Cr-P bonds where phosphorus istrans to carbonyl [2·338(4) Å] being significantly longer than those where phosphorus istrans to phosphine [2·282(4) Å]. This difference may be attributed to a difference in the back-bonding capabilities of the two types of ligands.We wish to thank Professor Dr E. O. Fischer for his stimulating interest in this work. Our thanks are due also to the Leibniz Rechenzentrum der Bayerischen Akademie der Wissenschaften for use of their computing facilities. This work would not have been possible without a generous grant from the Deutsche Forschungsgemeinschaft which is gratefully acknowledged.     

Crystal structures of (I) 2-(9,9-dipropylfluorene-2-yl)-9,9- dipropylfluorene and (II) 2-(1,1-dimethylpropyl)-7- {4-[(1,1-dimethylpropyl)-9,9-diethylfluoren-2-yl]phenyl}-9,9-diethylfluorene and (III) 2-(4-ethylphenyl) -7-[7-(ethylphenyl)-9,9-dipropylfluoren-2-yl]-9,9-dipropylfluorene

The crystal structures of the three fluorene related molecules, (I) 2-(9,9-dipropylfluorene-2-yl)-9,9-dipropylfluorene, [Exalite 384, C₃₈H₄₂], (II) 2-(1,1-dimethylpropyl)-7-{4-[(1,1-dimethylpropyl)-9,9-diethylfluoren-2-yl] phenyl}-9,9-diethylfluorene, [Exalite 404, C₅₀ H₅₈], and (III) 2-(4-ethylphenyl)-7-[7-(ethylphenyl)-9,9-dipropylfluoren-2-yl]-9,9-dipropylfluorene, [Exalite 416, C₅₄H₅₈], have been determined. Structural details reveal a novel new bonding arrangement at the C2 atoms of symmetry-related fluorene moieties in all three molecules producing a linear type array with an inversion center connecting adjacent asymmetric units within each molecule. Exalite 384 is monoclinic, space group P2₁/c with a = 9.002(2) Å, b = 16.275(4) Å, c = 10.525(1) Å, = 103.05(1), and V = 1502.1(5) ų with Z = 4, for d _calc = 1.103 g/cm³. Exalite 404 is triclinic, space group P1 with a = 10.383(1) Å, b = 13.404(2) Å, c = 7.7007(9) Å, = 105.296(9), = 104.23(1), = 73.707(9), and V = 974.9(2) ų with Z = 2, for d _calc = 1.141. Exalite 416 is monoclinic, space group P2₁/c with a = 15.99(10) Å, b = 11.178(8) Å, c = 23.766(4) Å, = 104.21(4), and V = 4117(4) ų with Z = 4, for d _calc = 1.141 g/cm³.     

Synthesis and Crystal Structures of (E)-1-Phenyl-3-[(2,4,6-Trimethylphenyl)]prop-2-En-1-One and (E)-1-Phenyl-3-[(4-Trifluoromethylphenyl)]prop-2-En-1-One

Two chalcone compounds, namely (E)-1-phenyl-3-[(2,4,6-trimethylphenyl)]prop-2-en-1-one (1) and (E)-1-phenyl-3-[(4-trifluoromethylphenyl)]prop-2-en-1-one (2), have been synthesized and structurally characterized by elemental analysis, ¹H NMR spectrum, and single-crystal X-ray diffraction analysis. The chalcone molecules in (1) and (2) have the common skeleton of 1,3-diaryl-2-propen-1-one and adopt an (E)-configuration about the C = C double bonds. In addition, X-ray analysis reveals that the π···π stacking interactions are well observed in the crystal structure of (1) and (2).     

Crystal structure and computational studies of (E)-1-(benzo[b]thiophen-3-yl)-N-(4-ethoxyphenyl)methanimine

Crystallography Reports - The title compound, C17H15NOS, crystallizes in the orthorhombic sp. gr. Pca21. Two molecules in the asymmetric unit have similar structure. Crystal structure contains weak...     

Synthesis and Crystal Structures of Copper(II) Complexes Derived from 5-Methoxy-2-[(2-morpholin-4-ylethylimino)methyl]phenolate and (2-Morpholin-4-ylethyl)-(1-pyridin-2-ylethylidene)amine

Abstract  

A pair of copper(II) complexes, [CuL¹(ONO₂)(OH₂)] 1 and [CuBrL²N₃] 2, where L¹ is 5-methoxy-2-[(2-morpholin-4-ylethylimino)methyl]phenolate, and L² is (2-morpholin-4-ylethyl)-(1-pyridin-2-ylethylidene)amine, have been synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. Complex 1 crystallizes in the monoclinic space group P2₁/c, with a = 10.496(2), b = 19.113(3), c = 8.586(2) ?, β = 105.186(10)°. Complex 2 crystallizes in the monoclinic space group C2/c, with a = 16.606(3), b = 7.357(2), c = 26.043(5) ?, β = 94.996(2)°. The Cu atom in each complex is five-coordinate in a square pyramidal geometry.     

Crystal structures of bis-ligand complexes of copper(II) with 2-[(2-hydroxyethylamino)-methyl]-4,6-dinitrophenol, 2,4-dichloro-6-[(2-hydroxyethylamino)-methyl]phenol, and 2,4-dibromo-6-[(2-hydroxyethylamino)-methyl]phenol

The crystal structures of bis{2,4-dibromo-6-[(2-hydroxyethylamino)-methyl]phenolato}copper (I), bis{2,4-dichloro-6-[(2-hydroxyethylamino)-methyl]phenolato}copper (II), and bis{2-[(2-hydroxyethylamino)-methyl]-4,6-dinitrophenolato}copper (III) in which the metal atom is located at the center of symmetry are determined using X-ray diffraction. Crystals of compounds I and II are isostructural. The copper atom in the structures of compounds I and I coordinates two singly deprotonated bidentate molecules of the ligand through the phenol oxygen atoms and the azomethine nitrogen atoms with the formation of a distorted planar square. In the crystals, complexes I and II form one-dimensional infinite chains along the b axis. In the structure of compound III, the coordination polyhedron of the central atom is an elongated tetragonal bipyramid with the base formed by the azomethine nitrogen atoms and the phenol oxygen atoms. Both vertices of the bipyramid are occupied by the oxygen atoms of the amino alcohol groups of the neighboring complexes, which are related to the initial complex through the center of symmetry. In turn, the oxygen atoms of the alcohol groups of the initial complex are located at the vertices of the coordination bipyramids of the metal atoms of the neighboring centrosymmetric complexes, thus forming infinite polymer chains along the a axis.     

Synthesis and Crystal Structure of 3-[(Naphthalen-2-yl)methyl]Isocoumarin

Abstract 3-[(Naphthalen-2-yl) methyl]isocoumarin was synthesized by the reaction of homophthalic acid with 2-(naphthalen-2-yl)acetyl chloride at elevated temperature and its crystal structure has been determined (C₂₀H₁₄O₂), Mr = 286.31, a = 13.704(3), b = 7.356(4), c = 7.042(7) ?, β = 99.21(3)°, space group Pc, Z = 2, and V = 700.7(8) ?³. The isocoumarin and the naphthalene ring systems are individually planar and the dihedral angle between the mean planes of these two ring systems is 70.05(8)°. Graphical Abstract Synthesis and crystal structure of 3-[(Naphthalen-2-yl)methyl]isocoumarin Aamer Saeed, Junmei Liang, Masood Parvez The synthesis and crystal structure of a novel isocoumarin, 3-[(naphthalen-2-yl)methyl]isocoumarin has been presented.      

Crystal structures of bis{4-bromo-2-[(2-hydroxyethylimino)methyl]phenolato}copper and bis{4-chloro-2-[(2-hydroxyethylimino)methyl]phenolato}copper

The crystal structures of bis{4-bromo-2-[(2-hydroxyethylimino)methyl]phenolato}copper (I) and bis{4-chloro-2-[(2-hydroxyethylimino)methyl]phenolato}copper (II) are determined. Crystals I are monoclinic, space group P2₁/c, Z = 2, and R = 0.0732 (for all reflections). Crystals II are likewise monoclinic, space group P2₁/n, Z = 2, and R = 0.1106. In the structures of compounds I and II, the metal atom is situated at the center of symmetry and coordinated by two singly deprotonated bidentate 4-bromo-or 4-chloro-2-[(2-hydroxyethylimino)methylphenol molecules, respectively, through phenol oxygen and azomethine nitrogen atoms, which form a distorted planar square. In the structures of compound II, the coordination polyhedron of the central atom is completed to an elongated tetragonal bipyramid by the amino alcohol oxygen atoms of the adjacent complexes.     

Synthesis and Crystal Structure of [Benzyl N'-[[2-(hydroxy-kO)phenyl]ethylene]-N-[[2-(hydroxy-kO)phenyl]methylene]-carbamohydrazonothioato-kN,kN']-ethanol-dioxido-uranium

Crystallography Reports - The uranyl compound UO2(L')EtOH (L' = benzyl N-(2-(oxidanyl)benzylidene)-N'-((2-(1-oxidanyl)phenyl)ethylidene) carbamohydrazonothioate) was synthesized and its...