Structural and spectral studies of ammonium mucicate

Ammonium mucicate C₆H₈O₈(NH₄)₂,M _r=244.20, monoclinic,P2₁/a,a=13.460(2),b=7.289(2),c=5.109(2)Å,=94.96(4)°,Z=2, molecular symmetry ¯1,V=499.4(3)ų,D _x=1.62 Mg m^–3,(MoK)=1.03 cm^–1,F(000)=260, room temperature. Final conventionalR value is 0.030 (Rw=0.037) for 1272 diffractometer-measured intensities withI3(I). The crystal structure is characterized by an extended system of hydrogen bonding involving the ammonium cations and the mucicate anions. The four hydroxyl groups are all involved as donors and acceptors in intermolecular bonds. The IR-spectra in the crystalline state have been recorded and compared to that of mucic acid.     

Structural and spectral studies of di-(triphenylmethylium-hexachloroantimonate)-benzenesolvate

The crystal structure of (SbCl₆C(C₆H₅)₃)₂·C₆H₆ has been determined. It belongs to space groupP2_1/c , witha=1.765(4),b=.8167(8),c=1.886(3) nm,=115.81(3)° andZ=4. We found a host/guest structure with benzene as a guest molecule. The SbCl6 octahedrons are distorted toC _4v -symmetry and are arranged in chains alongb, with a charge transfer between them. The propeller structure of the triphenylmethylium is discussed. The distances C_meth-C_phen are about 0.01 nm shorter than in triphenylmethanes. The IR-spectra of SbCl₆ in the crystalline state and in solution are recorded and discussed.professor G. Heublein died in 1989.     

Molecular structure and spectral characteristics of bis(S-methyl-N-(2-pyridyl)methylendithiocarbazato)nickel(II), (Ni(NNS)2)

A nickel(II) complex of the pyridine-2-aldehyde Schiff base of S-methyldithiocarbazate (HNNS) has been synthesized and characterized by means of elemental analysis, IR and UV-vis spectra. The crystal structure of the complex has been determined by single-crystal X-ray diffraction. The complex crystallizes in the monoclinic, space P2₁/c, with a = 14.092(2), b = 16.886(2), c = 8.857(2)Å; = 105.78(3) °, V = 2028.2(6) ų, and Z = 4. The nickel atom is octahedrally coordinated by two uninegatively charged tridentate Schiff base in a mer-configuration via the pyridine nitrogen atom, azomethine nitrogen atom, and mecaptide sulfur atom.     

Spectroscopic studies, antimicrobial activities, and crystal structure of N-[2-hydroxy-1-naphthylidene]3, 5-bis(trifluoromethyl)aniline

A new Schiff base compound has been synthesized by the reaction of 2-hydroxy-1-naphthaldehyde with 3,5-bis(trifluoromethyl)aniline.The title compound was characterized by elemental analysis, IR,¹H NMR,¹³C NMR, and UV–Visible techniques.Its UV–Vis spectra was examined in polar and nonpolar solvents and in acidic and basic media. The crystal structure of the compound showed the OH group to be ortho to the imine group. It crystallizes in the monoclinic space group P2₁ with a = 11.328(2), b = 6.125(1), c = 11.937(2) ?, V = 825.1(2) ?³, D _x = 1.543 g cm⁻³and Z = 2. An intramolecular O1- H⋯N1 [2.558(7) ?] hydrogen bond stabilizes the molecule. The compound has also been characterized by its antimicrobial activities. The ligand has been screened in vitro against the organisms Escherichia coli ATCC 11230, Staphylococcus aureus ATCC 6538, Klebsiella pneumoniae UC57, Micrococcus luteus La 2971, Proteus vulgaris ATCC 8427, Pseudomonas aeruginosa ATCC 27853, Mycobacterium smegmatis CCM 2067, Bacillus cereus ATCC 7064, and Listeria monocytogenes ATCC 15313, the yeast cultures Candida albicans ATCC 10231, Kluyveromyces fragilis NRRL 2415, Rhodotorula rubra DSM 70403, Debaryomyces hansenii DSM 70238, and Hanseniaspora guilliermondii DSM 3432.     

Structure of (N-(2-hydroxyphenyl)-salicylaldiminopiperidino) Ni(II) complex

The crystal and molecular structure of the title complex, C₁₈H₁₉N₂O₂Ni, has been determined by direct methods. The compound crystallizes in the monoclinic crystal system witha=22.973(1),b=5.212(1),c=27.076(1)Å, β=106.46(1)°, space groupC2/c,V=3109.1(6)ų, Z=8, andD _x=1.51g cm^?3. The nickel atom is in a slightly distorted square-planar environment of two oxygens [Ni(1)?O(1) 1.824(3) and Ni(1)?O(2) 1.856(3)Å] and two nitrogens [Ni(1)?N(1) 1.849(3) and Ni(1)?N(2) 1.932(3)Å] with O?Ni?N angles between 85.7(1) and 97.1(1)°. The nickel atom is 0.006 Å out of the plane of its ligands.     

Structure of N-(2-thiophenyl)-salicylaldimino-diethylamino nickel(II) complex

N-(2-thiophenyl)-salicylaldimino-diethylamino nickel(II) complex crystallizes in the orthorhombic crystal system witha=19.089(4),b=14.268(7),c=12.091(4) Å, space group Pbca,Z=8, andD _x =1.449 g cm^–3. The central nickel atom is coordinated with S, O, and N atoms. The coordination plane is nearly planar and nearly perpendicular to the diethylamine plane which consist of N(2), C(14), C(15), C(16), and C(17).     

The crystal structure of a N-(2-thiophenyl)-salicylaldiminopiperidino nickel(II) complex

The crystal and molecular structure of the title complex, C₁₈H₁₉N₂OSNi, has been determined by direct methods. The compound crystallizes in monoclinic crystal system witha=11.968(1),b=12.182(1),c=12.399(1) Å, =115.23(1)°, space group P2₁/n. Nickel is in a slightly distorted square-planar environment of two nitrogens [1.881(2) and 1.952(2) Å] and one oxygen [1.856(3) Å] and one sulphur [2.138(2) Å] atom. Ni is 0.005 Å out of the plane of its ligands.     

Synthesis and Structural Characterization of <Emphasis Type="Italic">N</Emphasis>-(2-Pyridylmethyl)-3-Methoxysalicylaldiminato Copper(II) Chloride

Abstract  The copper(II) complex [Cu(C₅H₄NCH₂−N=CH–C₆H₃OCH₃–O)Cl], (1) containing a new tridentate Schiff base ligand (LH), which is the 1:1 condensation product of 2-(aminomethyl)pyridine and o-vaniline, has been synthesised and characterized by IR and UV–Vis spectra. Structural investigation shows that 1 crystallizes to a monoclinic system, having space group P2(1)/c, a = 6.9634(7), b = 18.1209(19), c = 10.3448(11) ?, α = 90°, β = 103.97(2)°, γ = 90° and Z = 4. The coordination geometry around the copper atom is slightly distorted square planar, formed by the N₂O donor set of the Schiff base and one Cl atom. The Cu–N(1), Cu–N(2), Cu–O(1) and Cu–Cl bond distances are 2.0114(14), 1.9414(14), 1.9147(12) and 2.2520(5) ?, respectively. Index Abstract  The copper(II) complex [Cu(C₅H₄NCH₂−N=CH–C₆H₃OCH₃–O)Cl], (1) containing a tridentate Schiff base ligand (LH), synthesised and characterized by IR and UV–Vis spectra. The central copper ion possesses a distorted square-planar geometry.      

Crystal structure of tris-(2,2′,2″)-triaminoethylamino-salicylidene iron(III) complex

Tris-(2,2,2)-triaminoethylamino-salicylidene iron(III) crystallizes in the monoclinic crystal system witha=7.766(2),b=25.423(5),c=13.318(5) Å, =118.04(3)°, space group P2₁/c,V=2320.8(6) ų,Z=4, andD _x=1.464 g cm^–3. The center of the axially distorted octahedron is occupied by the Fe atom which is coordinated by six donor nitrogen and oxygen atoms infac positions. The planes of coordinated atoms (N and O) with the Fe(III) atom are almost planar and the maximum elevated atom from these planes is O(1) (–0.1065 Å).     

The synthesis and crystal structure of one novel ternary complex of 2,2′-bipyridine N-salicylidenetyrosinatocopper(II)

The crystal structure of copper(II)—salicylidene-aminoacidate Schiff base—nitrogen-donor chelating ligand, [Cu(sal-tyr)(bipy)] (sal-tyr: N-salicylidenetyrosinato; bipy: 2,2-bipyridine) which is obtained by means of one-step synthesis, is presented. It crystallizes in space group P2₁2₁2₁ with a = 9.0356(18) Å, b = 11.992(2) Å, c = 20.618(4) Å. The Cu^II ion is five coordinated by one oxygen atom of carboxylate, the imine nitrogen atom, and the hydroxyl oxygen atom of the salicylidene in the Schiff base anion as well as two nitrogen atoms of bipy, resulting in a seriously distorted square pyramid coordination polyhedron. The phenol group and the apical coordination bond Cu(1)–N(2) are in the same side of the Schiff base chelating plane which could be attributed to the intramolecular C–H s interaction between the H(17) of the bipy and the benzene ring of the phenol. The hydrogen bond between the hydroxyl hydrogen atom of the phenol group and the coordinated oxygen atom of the carboxylate from neighboring molecule is helpful to stabilize the crystal.     

Structure and characterization of bis(N-p-chloro-phenyl-salicylideneaminate) Schiff base copper(II) complex: Cu[N-p-Cl-Ph-Sal]2

The crystal and molecular structure of the title compound has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group P2₁/c, with lattice parameters a = 13.678(3), b = 10.729(2), c = 8.1996(2) Å, = 98.96°, V = 1188.7(4) ų, and Z = 4. The crystal structure contains two centrosymmetric molecules of bis (N-p-chloro-phenyl-salicylideneaminate) Schiff base copper(II). Copper(II) ion is coordinated in a slightly distorted trans square-planar configuration, the distortion consisting of a reduction of the N–Cu–O angle with the chelate rings from the ideal value of 90°. The p-chlorophenyl rings with salicylidene moieties form a dihedral angle of 38.96°.     

Structure and characterization of O,O-diethylthiophosphorylhydrazine o-vanillin Schiff base nickel(II) complex: NiC24H36N4O8P2S2

The crystal and molecular structure of the complex of Ni[(C₂H₅O)₂PSNHNCPh(o-O)OMe]₂ has been determined by X-ray crystallography. The compound crystallizes in the monoclinic system, space group P2₁/n, with lattice parameters a = 14.805(3), b = 7.9550(16), c = 15.176(3) Å, = 117.94(3), and Z = 2. The unit cell contains two centrosymmetric molecules of O,O-diethylthiophosphorylhydrazine o-vanillin Schiff base nickel(II). The nickel(II) ion is coordinated in a slightly distorted trans square-planar configuration, the distortion consisting of a reduction of the N—Ni—O angle with the chelate rings from the ideal value of 90° to 87.69°. The coordination geometry of nickel(II) is square planar with two equivalent Ni—N and Ni—O bonds. The two phenyl rings and the phosphorylhydrazine moieties are in one plane forming an extensive delocalized system. Within each molecule, the two ligands are linked by a pair of N—H···O hydrogen bonding interactions. In the solid state, the title compound form a hydrogen bonding network through C—H···O intermolecular hydrogen bonding.     

Synthesis,Crystal Structure and Spectroscopic Studies of 2-{(<Emphasis Type="Italic">E</Emphasis>)-[2-Hydroxyphenyl)imino]methyl} Phenol Schiff Base Molecule

Abstract  A new Schiff-base complex 2-{(E)-[2-hydroxyphenyl)imino]methyl}phenol has been synthesized and characterized by elemental analyses, UV–VIS and IR spectroscopy and single crystal X-ray determination. The structure comprises two independent and similar molecules. The two independent molecules in the asymmetric unit are hydrogen bonded and have different conformations. In each molecule, C₁₃H₁₁NO₂, adopt an E configuration about the azomethine C–N double bond. The complex crystallized in the triclinic space group P-1. Two benzene rings and azomethine group are practically coplanar, as a result of intramolecular hydrogen bonds involving the hydroxy O atom and azomethine N atom. Also hydroxy group of the molecule is the presence intermolecular O–H···O hydrogen bonds with the hydroxy group of the other molecule. Index Abstract and Figure  A new Schiff-base complex 2-{(E)-[2-hydroxyphenyl)imino]methyl}phenol has been synthesized and characterized by elemental analyses, UV–VIS and IR spectroscopy and single crystal X-ray determination. The structure comprises two independent and similar molecules. The two independent molecules in the asymmetric unit are hydrogen bonded and have different conformations. In each molecule, C13H11NO2, adopt an E configuration about the azomethine C–N double bond. The complex crystallized in the triclinic space group P-1. Two benzene rings and azomethine group are practically coplanar, as a result of intramolecular hydrogen bonds involving the hydroxy O atom and azomethine N atom. Also hydroxy group of the molecule is the presence intermolecular O–H···O hydrogen bonds with the hydroxy group of the other molecule.      

Structural and spectral studies of binuclear copper(II) 2-acetylpyridine 3-azacyclothiosemicarbazones with sulfato bridges

Structures of two binuclear copper(II) complexes with sulfato bridges and tridentate 2-acetylpyridine 3-azacyclothiosemicarbazone ligands have been solved. The complex-sulfato-bis{(2-acetylpyridine 3-hexamethyleneiminyl-thiosemicarbazonato)copper(II)} N,N-dimethylformamide, [Cu(Achexim)]₂SO₄·DMF, has the following structural properties: triclinic, P1¯(#2), a = 12.314(4), b = 15.885(4), c = 10.959(4) Å, = 103.25(2), = 103.60(2), = 109.94(2)°, V = 1843(2) ų, and Z = 2; for -sulfato-bis{(2-acetylpyridine 3-piperidylthiosemicarbazonato)copper(II)}chloroform, [Cu(Acpip)]₂SO₄·CHCl₃: triclinic, P1¯(#2), a = 11.657(1), b = 17.101(2), c = 10.338(1) Å, = 98.51(1), = 109.294(7), = 107.016(9)°, V = 1790.3(4) ų, and Z = 2. The size of the azacyclo ring significantly affects the stereochemistry of these binuclear complexes.     

Synthesis and Mesomorphic Properties of New Columnar Liquid Crystal Containing 1,3,5-triiminebenzene with Pendant 1,3,4-thiadiazole Group

A novel discotic liquid crystal series based on 1,3,5-benzenetrisazomethine derivatives with three pendant 2-amino-5-(4′-n-alkoxy)phenyl-1,3,4-thiadiazole has been synthesized, which is the first columnar molecules containing 1,3,4-thiadiazole moiety exhibiting a discotic liquid crystal. The molecular structure of compounds was confirmed by FT-IR, ¹H-NMR, and mass spectroscopy and elemental analysis. The electron excitation properties of these compounds were investigated by UV-vis absorption spectroscopy. Their liquid crystalline properties were studied by polarizing optical microscopy and differential scanning calorimetry. The formation of a columnar mesophase was found to be dependent on the number of methylene unit in alkoxy side chains.     

Syntheses,characterization and crystal structures of two structurally similar Schiff bases isonicotinic acid [1-(3-methoxy-2-hydroxyphenyl)methylidene]hydrazide and isonicotinic acid [1-(4-dimethylaminophenyl)methylidene]hydrazide monohydrate

The Schiff base compounds, isonicotinic acid [1-(3-methoxy-2-hydroxyphenyl) methylidene]hydrazide (C₁₄H₁₃N₃O₃, 1) and isonicotinic acid [1-(4-dimethylaminophenyl) methylidene]hydrazide monohydrate (C₁₅H₁₆N₄O·H₂O, 2) have been synthesized by the condensation of equimolar 3-methoxysalicylaldehyde or 4-dimethylaminobenzaldehyde with isonicotinic acid hydrazide in MeOH or EtOH. The compounds were characterized by elemental analysis, IR, ¹HNMR spectra, and single crystal X-ray diffractions. Compound 1 crystallizes in the monoclinic space group P-1 with unit cell dimensions a = 7.662(1) ?, b = 16.249(2) , c = 10.874(2) ?, β = 110.426(3)°, V = 1268.7(3) ′³, Z = 4, R ₁ = 0.0644, and wR ₂ = 0.1283. Compound 2 crystallizes in the orthorhombic space group P2₁2₁2₁ with unit cell dimensions a = 7.388(1) ?, b = 11.812(1) ?, c = 17.197(2) ?, V = 1500.7(2) ′³, Z = 4, R ₁ = 0.0585, and wR ₂ = 0.1143. X-ray structure determinations revealed that the molecules of both compounds display trans configurations with respect to the C=N double bonds. In the crystal structure of 1, molecules are linked through N–H···N intermolecular hydrogen bonds, forming layers parallel to the bc plane, while in the crystal structure of 2, molecules are linked through N–H···O, O–H···O, and O–H···N intermolecular hydrogen bonds, forming a network. Supplementary material CCDC-615072 and 620235 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam. ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223–336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Synthesis and crystal structures of the bis-Schiff bases of 2-(methylthio)aniline with isophthaldehyde, terephthaldehyde, and para-diacetylbenzene

The crystal structures of the new compounds 1,3-bis(((2-methylthio)phenylimino)methyl)benzene (1), 1,4-bis(((2-methylthio)phenylimino)methyl)benzene (2), and 1,4-bis(1-((2-methylthio)phenylimino)ethyl)benzene (3) were obtained by single crystal X-ray diffraction. Compound 1 crystallizes in the orthorhombic space group Pna2₁ with a=16.8250(13) ?, b=18.1068(13) ?, c=6.3086(5) ?; and Z=4. Compound 2 crystallizes in the triclinic space group with a=6.7532(7) ?, b=9.4433(9) ?, c=15.2473(15) ?; and α=86.339(2)°, β=80.609(2)°, γ=80.962(2)°; and Z=2. Compound 3 crystallizes in the triclinic space group with a=6.787(3) ?, b=7.517(3) ?, c=10.653(4) ?; and α=89.998(7)°, β=72.341(7)°, γ=75.998(7)°; and Z=1. Details of the synthesis, structures, and spectroscopic results are discussed.     

Synthesis and crystal structure of the copper(II) complex with novel Schiff base ligand: Cu(C8H7O2N)2(OH2)

The title complex Cu(C₈H₇O₂N)₂(OH₂) crystallized in the orthorhombic space group, Pbca with unit cell parameters: a = 15.242(2), b = 11.782(4), c = 17.946(4) Å, and Z = 8. Two nitrogen atoms, two phenolic oxygen atoms of the ligand, and one water molecule are coordinated with copper to form a distorted tetragonal pyramidal polyhedron.     

Crystal Structures of the Solvates of Di-ethylaminogossypol with Ethyl Acetate and Pyridine

Abstract  The crystal structures of di-ethylaminogossypol with ethyl acetate (DEAG-EA) and pyridine (DEAG-P) were studied by room-temperature X-ray diffraction. The host-to-guest molecule ratio in these complexes is 2:1 for DEAG-EA and 2:5 for DEAG-P. The crystal and cell parameters for DEAG-EA are C₃₄H₄₀N₂O₆·0.5(C₄H₈O₂), M = 660.78, triclinic, space group P-1, a = 11.316(2) ?, b = 12.082(2) ?, c = 15.085(3) ?, α = 73.34(3)°, β = 73.32(3)°, γ = 73.61(3)°, V = 1,847.3(7) ?³, Z = 2, and d _calc. = 1.188 g/cm³ and for DEAG-P are C₃₄H₄₀N₂O₆·2.5(C₅H₅ N), M = 769.91, triclinic, space group P-1, a = 9.6090(19) ?, b = 14.894(3) ?, c = 16.038(3) ?, α = 90.66(3)°, β = 106.25(3)°, γ = 103.17(3)°, V = 2138.7(9) ?³, Z = 2, and d _calc. = 1.195 g/cm³. In both structures, the di-ethylaminogossypol molecules are in the enamine form, which is the same tautomer found for other reported Schiff base gossypol derivatives. The enantiomeric gossypol molecules of each structure form different centrosymmetric dimer assemblies. These assemblies pack differently in each solvate. Index Abstract  Crystal structures of the solvates of di-ethylaminogossypol with ethyl acetate and pyridine were determined by X-ray diffraction.