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 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 copper(II) and nickel(II) nitrate and chloride complexes with 4-bromo-2-[(2-hydroxyethylimino)-methyl]phenol

The crystal structures of {4-bromo-2-[(2-hydroxyethylimino)-methyl]phenolo}aquacopper(II) nitrate hemihydrate (I), chloro-{4-bromo-2-[(2-hydroxyethylimino)-methyl]phenolo}copper hemihydrate (II), and chloro-{4-bromo-2-[(2-hydroxyethylimino)-methyl]phenolo}aquanickel (III) are determined using X-ray diffraction. Crystals of compound I are formed by cationic complexes, nitrate ions, and solvate water molecules. In the cation, the copper atom coordinates the singly deprotonated molecule of tridentate azomethine and the water molecule. The copper complexes are joined into centrosymmetric dimers by the O _w -H···O hydrogen bonds. The crystal structure of compound II is composed of binuclear copper complexes and solvate water molecules. The copper atom coordinates the O,N,O ligand molecule and the chlorine ion, which fulfills a bridging function. The coordination polyhedron of the metal atom is a distorted tetragonal bipyramid in which the vertex is occupied by the chlorine atom of the neighboring complex in the dimer. Compound III is a centrosymmetric dimer complex. The coordination polyhedra of two nickel atoms related via the inversion center are distorted octahedra shared by the edge.     

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 6-[(2-hydroxy-1,1-bishydroxymethylethylamino)methylene]-2,4-dinitrocyclohexa-2,4-dienone hydrate and complexes of copper(II) chloride and copper(II) nitrate with this ligand

The crystal structures of 6-[(2-hydroxy-1,1-bishydroxymethylethylamino)methylene]-2,4-dinitrocyclohexa-2,4-dienone hydrate L · H₂O (I), chloro-(2-hydroxymethyl-2-methylpropane-1,3-diol-2-iminomethyl-4,6-dinitrophenolo)aquacopper hydrate [Cu(H₂O)(L-H)Cl] · H₂O (II), and (2-hydroxymethyl-2-methylpropane-1,3-diol-2-iminomethyl-4,6-dinitrophenolo)aquacopper nitrate [Cu(H₂O)(L-H)]NO₃ (III) are determined using X-ray diffraction. It is established that the salicylidene fragment of azomethine L in the structure of compound I is in a quinoid tautomeric form. In the crystal, molecules L and water molecules are joined together by hydrogen bonds into two-dimensional layers aligned parallel to the (010) plane. The copper atom in the structure of compound II coordinates the singly deprotonated tridentate molecule L (whose salicylidene fragment is in a benzenoid form), the chlorine ion, and the water molecule. The coordination polyhedron of the central copper atom is a distorted tetragonal pyramid. In the structure of compound III, the polymer chains are formed through the coordination bonds of the copper atom with two oxygen atoms of the amino alcohol fragment of azomethine L of the neighboring complex, which is related to the initial complex by the translation along the x axis. The coordination polyhedron of the central atom is an elongated tetragonal bipyramid. Polymers and nitro groups form a three-dimensional framework through hydrogen bonds.     

Synthesis,Characterization and Crystal Structure of a Mononuclear Copper(II) Complex Derived from 2-Methoxy-6-[(pyridin-2-ylmethylimino)methyl]phenol

Abstract  

Blue needle-shaped crystals of bromo{2-methoxy-6-[(pyridin-2-ylmethylimino)methyl]phenolate}copper(II), [CuBr(C₁₄H₁₃N₂O₂)], have been obtained and characterized by elemental analysis, IR spectrum, and single crystal X-ray diffraction. The complex crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a = 7.059(1) ?, b = 18.504(3) ?, c = 10.664(2) ?, β = 105.415(2)°, V = 1,342.8(4) Ǻ³, Z = 4, R ₁ = 0.0377 and wR ₂ = 0.0751. X-ray structural determination revealed that the molecule of the mononuclear copper(II) complex is nearly coplanar. The Cu atom in the complex is tetra-coordinated by one phenolate O atom, one imine N atom, and one pyridine N atom of the Schiff base ligand, and by one terminal Br atom, forming a square planar coordination.     

Synthesis,Characterization and Crystal Structure of a Mononuclear Zinc(II) Complex Derived from 2-[(2-Propylaminoethylimino)methyl]phenol

Abstract  

A new zinc(II) complex, [Zn(C₁₂H₁₈N₂O)Cl₂]·CH₃CN, derived from the Schiff base ligand 2-[(2-propylaminoethylimino)methyl]phenol, has been synthesized and characterized by elemental analysis, IR spectra, and X-ray crystallography. The complex crystallizes in the orthorhombic space group Pbcn with unit cell dimensions a = 26.387(9) ?, b = 7.389(2) ?, c = 18.731(6) ?, V = 3,652(2) ?³, Z = 8, R ₁ = 0.0455 and wR ₂ = 0.1143. The asymmetric unit of the compound contains a mononuclear [Zn(C₁₂H₁₈N₂O)Cl₂] complex and an acetonitrile molecule linked together by an intermolecular N–H···N hydrogen bond. Crystal packing is stabilized by intermolecular N–H···O hydrogen bonds linking the molecules into chains along the b axis of the unit cell.     

Synthesis and Crystal Structure of [2-(4-chlorobenzoyloxy)-5-methylphenyl]-(4-methylphenyl)methanone

[2-(4-Chlorobenzoyloxy)-5-methylphenyl]-(4-methylphenyl)methanone was synthesized and characterized by spectroscopic and X-ray diffraction methods. The molecule crystallizes in the monoclinic space group P2₁/c with cell parameters a = 13.7530(19) Å, b = 10.0560(19) Å, c = 13.469(3) Å, β = 100.630(7)° and Z = 4. There is a large discrepancy between the carbonyl group bond lengths of ketone and the ester. The structure exhibits intermolecular hydrogen bonds of the type C–H···O.     

Crystallographic and Conformational Analysis of [(Z)-2-ethoxy-6-[(2-hydroxyphenylamino)methylene]cyclohexa-2,4-dienone]

Abstract  The single crystal X-ray diffraction analysis of the title compound, C₁₅H₁₅NO₃, shows that the structure is adopted to its NH tautomeric form and crystallizes in the orthorhombic space group P bcn with a = 21.2424(15) ?, b = 12.7696(9) ?, c = 9.3605(10) ?, Z = 8, V = 2539.1(4) ?³, D _c  = 1.346 g/cm³. The molecular conformation in the crystal is stabilized by an intramolecular H-bond and the crystal structure is stabilized by the bifurcated O–H···O type intermolecular H-bonds. In order to understand the effects on conformational flexibility of the title molecule, molecular energy profile was calculated as a function of the selected torsion angle by means of AM1 semi-empirical method. Index Abstract  Molecular and crystal structure of [(Z)-2-ethoxy-6-[(2-hydroxyphenylamino)methylene]cyclohexa-2,4-dienone], C₁₅H₁₅NO₃, have been determined by single crystal X-ray diffraction study, and conformational analysis of the title molecule with respect to the selected torsion angle has been achieved by AM1 semi-empirical calculations.      

Synthesis and Crystal Structure of Dichlorido{2-[(4-Methoxyphenyl)Iminomethyl]pyridine-k2N,N'}zinc

Crystallography Reports - A coordination complex, [Zn(L)Cl2], consisting of ZnCl2 and Schiff base bidentate ligand (4-methoxyphenyl)pyridine-2ylmethyleneamine (L) was prepared and structurally...     

Investigation of the Molecular Structure of (E)-2-Bromo-6-[(4-bromo-2-methylphenylimino)methyl]-4-chlorophenol

Crystallography Reports - In this study, the molecular structure of (E)-2-bromo-6-[(4-bromo-2-methylphenylimino)methyl]-4-chlorophenol has been investigated using crystallographic (XRD),...     

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 nitrato-4-bromo-2-[(2-hydroxyethylimino)methyl]phenolatoimidazolecopper and nitrato-4-chloro-2-[(2-Hydroxyethylimino)methyl]phenolatoimidazolecopper

Nitrato-4-bromo-2-[(2-hydroxyethylimino)methyl]phenolatoimidazolecopper and nitrato-4-chloro-2-[(2-hydroxyethylimino)methyl]phenolatoimidazolecopper were synthesized and studied by X-ray diffraction. The crystals are isostructural. The coordination polyhedron of the copper atom can be described as a distorted square pyramid whose basal plane is formed by the phenolic and alcoholic oxygen atoms and the nitrogen atom of the monodeprotonated tridentate azomethine molecule and the imidazole nitrogen atom. The apex of the copper polyhedron is occupied by the oxygen atom of the nitrato group. The complexes are linked together by hydrogen bonds with the participation of the nitrato groups to form a three-dimensional framework.     

Molecular Structure and Supramolecular Architecture of (E)-2-Bromo-6-[(2,4,6-Tribromophenylimino)methyl]-4-Chlorophenol

Crystallography Reports - In this study, the molecular structure and supramolecular architecture of a new compound have been studied in depth using single crystal X-ray diffraction (XRD) technique....     

Structure of dichloro[(2,4-dimethyl-5-oxo-2,3,4,5-tetrahydro-2-furyl)methyl]-(4-methoxyphenyl)tellurium(IV)

The crystal structure of TeCl₂(C₇H₇O)(C₇H₁₁O₂) has been determined from three dimensional, single crystal X-ray diffraction data. It crystallizes in the monoclinic space group C2/c with the lattice constantsa=24.551(5),b=11.435(2),c=12.368(2)Å,=97.33(1)° andZ=8,D _X=1.67 g cm^–3. Final least-squares refinement based on 3023 independent observed reflections yieldedR=0.026. The Te^iv ion is in a trigonal bipyramidal configuration with its lone pair of electrons at one of the equatorial positions. Distances and angles are: Te-Cl=2.495(1), 2.517(1); Te-C=2.134(3), 2.106(3)(aryl)Å; Cl-Te-Cl=173.45(4), Cl-Te-C=88.11(9), 88.60(9), 88.72(9), 86.06(9); C-Te-C=96.5(1)°. There are two secondary bonds to the tellurium: TeCl=3.824(1) and TeO(2)=3.006(1)Å. The methyl group to the carbonyl oxygen and the aryltelluro moiety exhibit atrans 2,4 relationship.     

Spectroscopic Studies and Crystal Structure of (<Emphasis Type="Italic">Z</Emphasis>)-6-[(2-hydroxyphenylamino)methylene]-2-methoxycyclohexa-2,4-dienone

Abstract  The Schiff base (Z)-6-[(2-hydroxyphenylamino)methylene]-2-methoxycyclohexa-2,4-dienone has been synthesized from the reaction of 2-aminophenol with 2-hydroxy-3-methoxybenzaldehyde. The title compound has been characterized by elemental analysis, FT-IR, ¹H-NMR, ¹³C-NMR and UV–Visible techniques. The structure of the title compound also was determined crystallographically. The crystal structure has been solved by direct methods and refined by full-matrix least squares. The title compound crystallize in the monoclinic space group P2₁/c with a = 10.438(1), b = 8.851(1), c = 12.746(1) ?, β = 95.72(1)°, V = 1171.7(2) ?³, D _x  = 1.379 g cm⁻³, respectively (R1 = 0.0522 and wR2 = 0.126 for 1442 reflections [I > 2σ(I)]). Index Abstract   N-salicylideneaniline derivatives have been shown to exist as tautomeric forms due to intramolecular proton shifts between the phenol-oxygen and the imine-nitrogen, via intramolecular hydrogen bonding O–H···N or O···H–N.      

Synthesis and Crystal Structure of 2-(2,3,4-Trimethoxy-6-Methylbenzylideneamino)phenol

Abstract  The title compound 2-(2,3,4-trimethoxy-6-methylbenzylideneamino)phenol (C₁₇H₁₉NO₄, M _r = 301.33) was synthesised and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a = 10.4458(14), b = 8.3870(10), c = 17.780(2) ?, β = 91.102(2)^°, V = 1557.4(3) ?³, Z = 4, D _c = 1.285 g/cm³, λ = 0.71073 ?, μ(Mo Kα) = 0.092 mm⁻¹, F(000) = 640. The final refinement gave R = 0.0452, wR(F ²) = 0.1065 for 2,743 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the molecule adopts an E configuration at the C=N functional bond. The dihedral angle between the two phenyl rings is 38.3(3)°. The crystal structure is stabilized by C–H···O, O–H···O and O–H···N hydrogen bonds and π–π stacking interactions. Graphical Abstract  The title compound 2-(2,3,4-trimethoxy-6-methylbenzylideneamino)phenol (C₁₇H₁₉NO₄, M _r = 301.33) was synthesised and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a = 10.4458(14), b = 8.387(1), c = 17.780(2) ?, β = 91.102(2)°, V = 1557.4(3) ?³, Z = 4, D _c = 1.285 g/cm³, λ = 0.71073 ?, μ(Mo Kα) = 0.092 mm⁻¹, F(000) = 640. The final refinement gave R = 0.0452, wR(F ²) = 0.1065 for 2,743 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the molecule adopts an E configuration at the C=N functional bond. The dihedral angle between the two phenyl rings is 38.3(3)°. The crystal structure is stabilized by C–H···O and O–H···O hydrogen bonds and π–π stacking interactions.