Four new Schiff bases of 1,10-phenanthroline-2,9-dicarboxaldehyde with sulfur-containing amines such as 2-mercaptoaniline, S-alkyl/aryl dithiocarbazates and thiosemicarbazide have been synthesized and characterized by...Four new Schiff bases of 1,10-phenanthroline-2,9-dicarboxaldehyde with sulfur-containing amines such as 2-mercaptoaniline, S-alkyl/aryl dithiocarbazates and thiosemicarbazide have been synthesized and characterized by spectroscopic and X-ray crystallographic techniques. A comparative study of the methods of synthesis has been made using both traditional and microwave techniques. A significant reduction in reaction time has been observed when the microwave method was used. In some of the reactions, the yields also increased significantly.展开更多
Eight new Schiff bases of 5-nitro and 5-bromo-substituted 1,10-phenanthroline-2,9-dicarboxaldehydes with sulfur-containing amines, thiosemicarbazide, S-alkyl/aryl dithiocarbazates and 2-mercaptoaniline have been synth...Eight new Schiff bases of 5-nitro and 5-bromo-substituted 1,10-phenanthroline-2,9-dicarboxaldehydes with sulfur-containing amines, thiosemicarbazide, S-alkyl/aryl dithiocarbazates and 2-mercaptoaniline have been synthesized and characterized by a variety of spectroscopic methods. The condensation reactions of the dialdehydes with the amines were carried out both in the presence and absence of conc. sulfuric acid. A significant increase in yield of the Schiff bases was observed when the reactions were carried out in the presence of sulfuric acid.展开更多
Metal complex, bis[(2,2’)-dimethyl 2,2’-(1,10-phenanthrline-2,9-diyl)bis(methan-1-yl-1-ylidene)-bis(hydrazinecarrbo dithioate)copper(I)], was synthesized from the reaction of Schiff base, (2,2’)-dimethyl 2,2’-(1,1...Metal complex, bis[(2,2’)-dimethyl 2,2’-(1,10-phenanthrline-2,9-diyl)bis(methan-1-yl-1-ylidene)-bis(hydrazinecarrbo dithioate)copper(I)], was synthesized from the reaction of Schiff base, (2,2’)-dimethyl 2,2’-(1,10-phenanthroline-2,9-diyl)bis(methan-1-yl-1-ylidene)-bis(hydrazinecarbo dithioate) and CuCl2 at reflux condition in methanol. The copper centers of the complex appear to be reduced. This probably was facilitated by in situ oxidative formation of disulfide bond at the uncomplexed ligand moieties. Single crystal X-ray diffraction analysis reveals the distorted tetrahedral geometry around the copper centers. This compound crystallizes in the triclinic space group, P-1 with crystallographic parameters: a = 10.006(3) ?, b = 13.272(3) ?, c = 22.123(6) ?, α = 85.656(6)°, β = 81.656(6)°, γ = 73.097(5)°, μ = 1.223 mm-1 , V = 2779.5(13) ?3, Z = 2, Dc = 1.437 Mg/m3, T = 293 (2) K.展开更多
The reaction of [CpMo(CO)3]2 with dicyclopentamethylenethiuram disulfide in refluxing xylene resulted a novel mono nuclear complex, cis-[(CpMo(CO)2{S2C-N(CH2)5}] as red crystals in moderate yield. The compound was for...The reaction of [CpMo(CO)3]2 with dicyclopentamethylenethiuram disulfide in refluxing xylene resulted a novel mono nuclear complex, cis-[(CpMo(CO)2{S2C-N(CH2)5}] as red crystals in moderate yield. The compound was formed by the oxidative cleavage of metal-metal bond in [CpMo(CO)3]2 together with a reductive sulfur-sulfur bond scission in the ligand.展开更多
文摘Four new Schiff bases of 1,10-phenanthroline-2,9-dicarboxaldehyde with sulfur-containing amines such as 2-mercaptoaniline, S-alkyl/aryl dithiocarbazates and thiosemicarbazide have been synthesized and characterized by spectroscopic and X-ray crystallographic techniques. A comparative study of the methods of synthesis has been made using both traditional and microwave techniques. A significant reduction in reaction time has been observed when the microwave method was used. In some of the reactions, the yields also increased significantly.
文摘Eight new Schiff bases of 5-nitro and 5-bromo-substituted 1,10-phenanthroline-2,9-dicarboxaldehydes with sulfur-containing amines, thiosemicarbazide, S-alkyl/aryl dithiocarbazates and 2-mercaptoaniline have been synthesized and characterized by a variety of spectroscopic methods. The condensation reactions of the dialdehydes with the amines were carried out both in the presence and absence of conc. sulfuric acid. A significant increase in yield of the Schiff bases was observed when the reactions were carried out in the presence of sulfuric acid.
文摘Metal complex, bis[(2,2’)-dimethyl 2,2’-(1,10-phenanthrline-2,9-diyl)bis(methan-1-yl-1-ylidene)-bis(hydrazinecarrbo dithioate)copper(I)], was synthesized from the reaction of Schiff base, (2,2’)-dimethyl 2,2’-(1,10-phenanthroline-2,9-diyl)bis(methan-1-yl-1-ylidene)-bis(hydrazinecarbo dithioate) and CuCl2 at reflux condition in methanol. The copper centers of the complex appear to be reduced. This probably was facilitated by in situ oxidative formation of disulfide bond at the uncomplexed ligand moieties. Single crystal X-ray diffraction analysis reveals the distorted tetrahedral geometry around the copper centers. This compound crystallizes in the triclinic space group, P-1 with crystallographic parameters: a = 10.006(3) ?, b = 13.272(3) ?, c = 22.123(6) ?, α = 85.656(6)°, β = 81.656(6)°, γ = 73.097(5)°, μ = 1.223 mm-1 , V = 2779.5(13) ?3, Z = 2, Dc = 1.437 Mg/m3, T = 293 (2) K.
文摘The reaction of [CpMo(CO)3]2 with dicyclopentamethylenethiuram disulfide in refluxing xylene resulted a novel mono nuclear complex, cis-[(CpMo(CO)2{S2C-N(CH2)5}] as red crystals in moderate yield. The compound was formed by the oxidative cleavage of metal-metal bond in [CpMo(CO)3]2 together with a reductive sulfur-sulfur bond scission in the ligand.
