بهروز نوتاش

A new azo-Schiff base"Ethyl 2-((E)-(4-((E)-(4-ethylphenyl)diazenyl)-2-hydroxybenzylidene)amino)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate" was prepared by the reaction of "Ethyl 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate" and "(E)-5-((4-ethylphenyl)diazenyl)-2-hydroxybenz aldehyde" (1:1 molar ratio) in MeOH under reflux condition. The structure of compound was studied by elemental analysis, including IR and 1HNMR spectroscopy and single crystal X-ray diffraction method. The synthesized compound has been crystallized in triclinic system with Pī space group and a = 9.752 (2)Å, b = 10.349(2)Å, c = 13.263(3)Å, α = 87.72(3)˚, β = 75.80(3)˚, γ = 62.21(3)˚ cell parameters. The final R value is 0.098 for 4038 independent reflections. X-ray diffraction results confirm the planar geometric structure with a slight deviation and intermolecular hydrogen bond for the compound.

Two new polymeric compounds of cadmium acetate and Schiff-base ligand 1,2-bis(1-(pyridine-4-yl)ethylydine)hydrazine, L, [Cd(OAc)2(L)]n ,(1) and [Cd(OAc)2(L)(H2O)]n , (2) were synthesized and characterized by single crystal X-ray diffraction analysis. Structural analysis reveals that both compounds were crystallized in monoclinic crystal system with P21/c and I2/a space group respectively. Coordination polymer 1 was synthesized by solvent evaporation method in dimethyl sulfoxide and has one-dimensional ladder like structure. Coordination polymer 2 was prepared by solvent diffusion method in the mixture of methanol and water solvent and its crystal structure was assembled from one-dimensional linear chains. Also the influence of effective interactions in the crystal packing of prepared compounds and the value of their contributions were investigated by Hirshfeld surface analysis.

The Rh(III) complex[Rh(py)2(CH3CN)Cl3], Where py is pyridine has been prepared and characterized by elemental analysis, IR, and electronic absorption spectroscopies, and X-ray crystallography. The crystal structure of [Rh(py)2(CH3CN)Cl3] shows that the coordination geometry around the Rh(III) is a distorted octahedron. The title complex crystallized in monoclinic, space group P21/c, Z = 4, a = 7.626 (15) Å, b= 27.525(6) Å, c= 7.712 (15) Å and β=14.07(3)°. Electronic spectrum of the complex show that ligand – centered ( LCT ) transitions and metal- to- ligand charge transfer ( MLCT ). The molecular modeling of the complex was studied using a theoretical method and there was a good agreement between the results of the theory and the results of X-ray diffraction. Antibacterial activity of the complex has also been studied against Gram-positive bacteria (Staphylococcus aureus and Bacillus cereus ) and Gram-negative bacteria ( Pseudomunas aeroginosa and Escherichia coli).

Two new polymeric compounds of cadmium acetate using two isomers of pyridine hydrazide ligands have been synthesized and characterized by X-ray diffraction analysis. Structural analysis shows that both compounds were crystallized in monoclinic crystal system with P21/c space group. Coordination polymer [Cd(OAc)2(L1H)]n (1) which L1H is para pyridine hydrazide, has two dimensional sheets with rectangular net and coordination polymer [Cd2(OAc)3(L2H)L2(EtOH)]n (2) which L2H is meta pyridine hydrazide, has got herringbone structure in 2D dimension.

In this manuscript the reaction of 2-mercaptoquinoline-3-carbaldehydes and 1,1,3,3-tetramethyl butylisocyanide as highly substituted isocyanide in the reflux of ethanol without catalyst is described. Formation of C-S, C-C and simultaneously oxidation towards thiophenone derivative is the advantage of this reaction. Also contrary to our impression using hindered isocyanides did not prevent the cyclisation. Only in one example when 2-mercapto quinoline-3-carbaldehyde was used in the reaction, the corresponding alpha keto amide was formed. All of the compounds are new so that they were characterized by mp, FT-IR, H and C-NMR and in some case the structure was confirmed by x-ray single crystallography.

The co-crystal compound of 4,4'-bipyridine 3-nithrophthalic acid (1) was obtained by the reaction of 4,4'-bipyridine, 3-nithrophthalic acid and calcium chloride (1:1:1 molar ratio) in solvents mixture H2O/MeOH under solution condition. The crystal structure of this compound was determined by elemental analysis, IR spectroscopy and single crystal X-ray diffraction method. Crystallographic data for 1 was collected at 298 K. The synthesized compound has been crystallized in monoclinic system with P21/n space group and a = 13.729 (3), b = 6.804(1), c = 18.562(4), β= 109.56(3) cell parameters. The final R value is 0.06 for 2867 independent reflections. There are various types of non-covalent interactions including strong and weak hydrogen bonds N–H∙∙∙O and C–H∙∙∙O which connected the various components in )1( to form 3D supramolecular structure.

A new thiosemicarbzone compound was prepared by the reaction of acenaphthenequinone and thiosemicarbazide (1:1 molar ratio) in absolute methanol at 70°C. The crystal structure of this compound, acenaphthenequinone thiosemicarbazone mono methanol, was determined by X-ray crystallography. The unit cell parameters are as follows: a = 7.0384(14) Ǻ, b = 14.202(3) Ǻ, c = 14.270(3) Ǻ, β = 104.26(3)°. It crystallizes in a monoclinic system, with space group P21/c and four molecules in the unit cell. The final R value is 0.0738 for 2422 independent reflection.  Both inter and intramolecular hydrogen bonds exist in crystalline system.