In order to study the coordination character of the rare earth elements with hydrazones and the antioxidative activity of the ligand and the complexes, 3,5 dibenzyloxybenzoyl 2,4 dihydroxybenzaldehyde hydrazone (H ...In order to study the coordination character of the rare earth elements with hydrazones and the antioxidative activity of the ligand and the complexes, 3,5 dibenzyloxybenzoyl 2,4 dihydroxybenzaldehyde hydrazone (H 2L), a new chelating ligand, and its six lanthanide complexes, Ln (HL)(OAc) 2· n H 2O [Ln=La, Sm, Eu, Gd, Tb, Dy; n =2, 4, 5], were synthesized and characterized on the basis of elemental analyses, IR and 1H NMR spectra, molar conductivity. The results show that the lanthanide ions are coordinated by O, O and N donors of the phenol (Ar OH) without deprotonation, the enol oxygen of the hydrazone group (NCO -) and the azomethine group (CH=N) from the ligand respectively, and by the four carboxylic oxygen from two acetate groups (CH 3COO -) in the bidentate form. The scavenging activity of the ligand and the six lanthanides complexes on the 2,2 Diphenyl 1 picrylhydrazyl (DPPH) free radicals is also evaluated. The results show that both the ligand and the complexes have the scavenging activity on the DPPH radicals, and the scavenging activity of the complexes is better than the ligand.展开更多
New solid complexes derived from the reaction of aroyl hydrazones, 2-hydroxy-1-naphthaldehyde benzene sulphonyl hydrazone (HNB), and 2-hydroxy-1-naphthaldehyde p-toluene sulphonyl hydrazone (HNT), with Co<sup>2+...New solid complexes derived from the reaction of aroyl hydrazones, 2-hydroxy-1-naphthaldehyde benzene sulphonyl hydrazone (HNB), and 2-hydroxy-1-naphthaldehyde p-toluene sulphonyl hydrazone (HNT), with Co<sup>2+</sup>, Ni<sup>2+</sup>, and Cu<sup>2+</sup> salts have been isolated and characterized using elemental analyses, spectral (UV-vis., IR), molar conductivity and magnetic measurements. The modes of bonding as well as the stereochemistry of the isolated solid complexes were discussed. The results suggested that both HNB and HNT coordinated with the metal ions in a bidentate manner forming a polymeric chain in the case of HNB while monocular complexes were formed in the case of HNT. The amounts of solvent in the solid complexes were determined by TGA measurements. Also, spectral studies of HNT with Co<sup>2+</sup> and Fe<sup>3+</sup> ions in solution were carried and the ratio of complexes was determined by continuous variation, molar ratio, and slope ratio methods. Moreover, the results suggest the formation of 1:1 (M:L) for Co<sup>2+</sup> ions while three species with ratios of 1:1, 1:2, and 2:1 (M:L) have been observed in the case of Ni<sup>2+</sup> and Cu<sup>2+</sup>. Finally, conductance titration of HNB and HNT with Co<sup>2+</sup> ion elucidates the formation of two species with ratios 1:1 and 1:2 (M:L) in the case of the Co<sup>2+</sup>-HNB while 1:1 (M:L) belongs to the Co<sup>2+</sup>-HNT system.展开更多
Complexes of La(Ⅲ),Nd(Ⅲ),Sm(Ⅲ),Eu(Ⅲ),Gd(Ⅲ),Dy(Ⅲ), Er(Ⅲ),Yb(Ⅲ)and Y(Ⅲ)with piperonal isonicotinoyl hydrazone(HPIN) have been synthesized in DMF and EtOH.The complexes have been characte- rized by elemental ana...Complexes of La(Ⅲ),Nd(Ⅲ),Sm(Ⅲ),Eu(Ⅲ),Gd(Ⅲ),Dy(Ⅲ), Er(Ⅲ),Yb(Ⅲ)and Y(Ⅲ)with piperonal isonicotinoyl hydrazone(HPIN) have been synthesized in DMF and EtOH.The complexes have been characte- rized by elemental analysis,molar conductance,i.r.,UV and^1H n.m.r. spectra,magnetic measurements,X-ray powder diffraction and DTA.展开更多
A Schiff base L [2-thiophenecarboxylic acid, 2-（2-pyridinylmethylene）hydrazide] with its lanthanide metal complexes was synthesized. These complexes were characterized by elemental analysis, molar conductivity measu...A Schiff base L [2-thiophenecarboxylic acid, 2-（2-pyridinylmethylene）hydrazide] with its lanthanide metal complexes was synthesized. These complexes were characterized by elemental analysis, molar conductivity measurements, spectral analysis（NMR, FT-IR, and UV-Vis）, luminescence and thermal gravimetric analysis. The Schiff base ligand was a tridentate chelate and coordinates to the central lanthanide ion with 1：2 metal：ligand ratio. The conductivity data showed a 1：1 electrolytic nature with a general formula [LnL_2（NO_3）_2]NO_3. The luminescence emission properties for Sm, Tb, and Eu complexes were observed and showed that the ligand L could absorb and transfer energy to Sm（III）, Tb（III） and Eu（III） ions. The complexes possessed a good antibacterial activity against different bacterial strains. In addition, the scavenging activity of the Ln（III） complexes on DPPH was concentration dependant and the complexes were significantly more efficient in quenching DPPH than the free Schiff base ligand.展开更多
One new polymer, [Na（NPHSNPAB）（CH3OH）]n, where NPHSNPAB stands for Nphenyl-2-[2-hydroxy-3-sulfo-5-nitrophenylhydrazone]butadione-1,3, has been synthesized and characterized by ^1H NMR and FTIR spectroscopy and sin...One new polymer, [Na（NPHSNPAB）（CH3OH）]n, where NPHSNPAB stands for Nphenyl-2-[2-hydroxy-3-sulfo-5-nitrophenylhydrazone]butadione-1,3, has been synthesized and characterized by ^1H NMR and FTIR spectroscopy and single-crystal X-ray diffraction. For this complex： C（17）H（17）N4NaO9S, Mr = 476.39, triclinic system, space group P1, a = 8.8741（18）, b = 10.942（2）, c = 12.039（2） A, α = 65.74（3）, β = 77.49（3）, γ = 84.30（3）o, V = 1040.3（4） A3, Z = 2, Dc = 1.521 g/cm^3, λ = 0.71073 A, F（000） = 492, S = 1.106, R = 0.0614 and w R = 0.1423 for 2945 observed reflections with I 〉 2（I）. X-ray structural analysis revealed that the structure of NPHSNPAB framework was almost planar by C–H···O, N–H···O, O–H···O, and O–H···S hydrogen bonds. Moreover, sodium（I） center was bound by six O and one N atoms, forming the coordination polymer. The molecular packing diagram showed complicated hydrogen bonds and π···π stacking interaction in the polymer. The average bond distance of the two dicyclic units（3.768 A） indicated strong π···π stacking interaction. The complex displays greenyellow emission at room temperature.展开更多
Complex VO(C\-\{12\}H\-\{12\}N\-2O\-2)(C\-\{13\}H\-\{10\}NO\-2)(C\-\{12\}H\-\{12\}N\-2O\+\{\{\}\+\{2-\}\}\-2=acetylacetone benzoylhydrozanate,C\-\{13\}H\-\{10\}NO\+_\-2=\%N\%\|phenylbenzohydroxamate) was synthesized a...Complex VO(C\-\{12\}H\-\{12\}N\-2O\-2)(C\-\{13\}H\-\{10\}NO\-2)(C\-\{12\}H\-\{12\}N\-2O\+\{\{\}\+\{2-\}\}\-2=acetylacetone benzoylhydrozanate,C\-\{13\}H\-\{10\}NO\+_\-2=\%N\%\|phenylbenzohydroxamate) was synthesized and characterized by means of elemental analysis,IR and UV spectroscopies,cyclic voltammetry and single crystal X\|ray diffraction. The complex crystallized in the monoclinic system with space group \%P\%2\-1/\%n\% and the crystal cell parameters \%a\%=1\^3003(1) nm,\%b\%=0\^88836(6) nm,\%c\%=2\^0196(2) nm,\%β\%=95\^065(8)°,\%V\%=2\^3238(3) nm\+3,\%M\%\-r=495\^40 and \%Z\%=4. The two oxygen and one nitrogen atoms of the tridentate hydrazone ligand coordinate to the vanadium atom,forming an equatorial plane. And the coordinated vanadium atom exhibits a distorted octahedral geometry. The atom in the transposition to the oxo O atom is the carbonyl oxygen atom of the hydroxamate ligand in the complex. The half\|wave redox potential of the title complex in the three different solvents positively shifts in the order of CH\-2Cl\-2<CH\-3CN<DMF.展开更多
文摘In order to study the coordination character of the rare earth elements with hydrazones and the antioxidative activity of the ligand and the complexes, 3,5 dibenzyloxybenzoyl 2,4 dihydroxybenzaldehyde hydrazone (H 2L), a new chelating ligand, and its six lanthanide complexes, Ln (HL)(OAc) 2· n H 2O [Ln=La, Sm, Eu, Gd, Tb, Dy; n =2, 4, 5], were synthesized and characterized on the basis of elemental analyses, IR and 1H NMR spectra, molar conductivity. The results show that the lanthanide ions are coordinated by O, O and N donors of the phenol (Ar OH) without deprotonation, the enol oxygen of the hydrazone group (NCO -) and the azomethine group (CH=N) from the ligand respectively, and by the four carboxylic oxygen from two acetate groups (CH 3COO -) in the bidentate form. The scavenging activity of the ligand and the six lanthanides complexes on the 2,2 Diphenyl 1 picrylhydrazyl (DPPH) free radicals is also evaluated. The results show that both the ligand and the complexes have the scavenging activity on the DPPH radicals, and the scavenging activity of the complexes is better than the ligand.
文摘New solid complexes derived from the reaction of aroyl hydrazones, 2-hydroxy-1-naphthaldehyde benzene sulphonyl hydrazone (HNB), and 2-hydroxy-1-naphthaldehyde p-toluene sulphonyl hydrazone (HNT), with Co<sup>2+</sup>, Ni<sup>2+</sup>, and Cu<sup>2+</sup> salts have been isolated and characterized using elemental analyses, spectral (UV-vis., IR), molar conductivity and magnetic measurements. The modes of bonding as well as the stereochemistry of the isolated solid complexes were discussed. The results suggested that both HNB and HNT coordinated with the metal ions in a bidentate manner forming a polymeric chain in the case of HNB while monocular complexes were formed in the case of HNT. The amounts of solvent in the solid complexes were determined by TGA measurements. Also, spectral studies of HNT with Co<sup>2+</sup> and Fe<sup>3+</sup> ions in solution were carried and the ratio of complexes was determined by continuous variation, molar ratio, and slope ratio methods. Moreover, the results suggest the formation of 1:1 (M:L) for Co<sup>2+</sup> ions while three species with ratios of 1:1, 1:2, and 2:1 (M:L) have been observed in the case of Ni<sup>2+</sup> and Cu<sup>2+</sup>. Finally, conductance titration of HNB and HNT with Co<sup>2+</sup> ion elucidates the formation of two species with ratios 1:1 and 1:2 (M:L) in the case of the Co<sup>2+</sup>-HNB while 1:1 (M:L) belongs to the Co<sup>2+</sup>-HNT system.
文摘Complexes of La(Ⅲ),Nd(Ⅲ),Sm(Ⅲ),Eu(Ⅲ),Gd(Ⅲ),Dy(Ⅲ), Er(Ⅲ),Yb(Ⅲ)and Y(Ⅲ)with piperonal isonicotinoyl hydrazone(HPIN) have been synthesized in DMF and EtOH.The complexes have been characte- rized by elemental analysis,molar conductance,i.r.,UV and^1H n.m.r. spectra,magnetic measurements,X-ray powder diffraction and DTA.
基金Project supported by Jordan University of Science and Technology Research Fund Project(2011/202)
文摘A Schiff base L [2-thiophenecarboxylic acid, 2-（2-pyridinylmethylene）hydrazide] with its lanthanide metal complexes was synthesized. These complexes were characterized by elemental analysis, molar conductivity measurements, spectral analysis（NMR, FT-IR, and UV-Vis）, luminescence and thermal gravimetric analysis. The Schiff base ligand was a tridentate chelate and coordinates to the central lanthanide ion with 1：2 metal：ligand ratio. The conductivity data showed a 1：1 electrolytic nature with a general formula [LnL_2（NO_3）_2]NO_3. The luminescence emission properties for Sm, Tb, and Eu complexes were observed and showed that the ligand L could absorb and transfer energy to Sm（III）, Tb（III） and Eu（III） ions. The complexes possessed a good antibacterial activity against different bacterial strains. In addition, the scavenging activity of the Ln（III） complexes on DPPH was concentration dependant and the complexes were significantly more efficient in quenching DPPH than the free Schiff base ligand.
基金supported by the Soft Science project of Shanxi Province(No.2013041020-03)the National Natural Science Foundation of China(No.51174275)
文摘One new polymer, [Na（NPHSNPAB）（CH3OH）]n, where NPHSNPAB stands for Nphenyl-2-[2-hydroxy-3-sulfo-5-nitrophenylhydrazone]butadione-1,3, has been synthesized and characterized by ^1H NMR and FTIR spectroscopy and single-crystal X-ray diffraction. For this complex： C（17）H（17）N4NaO9S, Mr = 476.39, triclinic system, space group P1, a = 8.8741（18）, b = 10.942（2）, c = 12.039（2） A, α = 65.74（3）, β = 77.49（3）, γ = 84.30（3）o, V = 1040.3（4） A3, Z = 2, Dc = 1.521 g/cm^3, λ = 0.71073 A, F（000） = 492, S = 1.106, R = 0.0614 and w R = 0.1423 for 2945 observed reflections with I 〉 2（I）. X-ray structural analysis revealed that the structure of NPHSNPAB framework was almost planar by C–H···O, N–H···O, O–H···O, and O–H···S hydrogen bonds. Moreover, sodium（I） center was bound by six O and one N atoms, forming the coordination polymer. The molecular packing diagram showed complicated hydrogen bonds and π···π stacking interaction in the polymer. The average bond distance of the two dicyclic units（3.768 A） indicated strong π···π stacking interaction. The complex displays greenyellow emission at room temperature.
文摘Complex VO(C\-\{12\}H\-\{12\}N\-2O\-2)(C\-\{13\}H\-\{10\}NO\-2)(C\-\{12\}H\-\{12\}N\-2O\+\{\{\}\+\{2-\}\}\-2=acetylacetone benzoylhydrozanate,C\-\{13\}H\-\{10\}NO\+_\-2=\%N\%\|phenylbenzohydroxamate) was synthesized and characterized by means of elemental analysis,IR and UV spectroscopies,cyclic voltammetry and single crystal X\|ray diffraction. The complex crystallized in the monoclinic system with space group \%P\%2\-1/\%n\% and the crystal cell parameters \%a\%=1\^3003(1) nm,\%b\%=0\^88836(6) nm,\%c\%=2\^0196(2) nm,\%β\%=95\^065(8)°,\%V\%=2\^3238(3) nm\+3,\%M\%\-r=495\^40 and \%Z\%=4. The two oxygen and one nitrogen atoms of the tridentate hydrazone ligand coordinate to the vanadium atom,forming an equatorial plane. And the coordinated vanadium atom exhibits a distorted octahedral geometry. The atom in the transposition to the oxo O atom is the carbonyl oxygen atom of the hydroxamate ligand in the complex. The half\|wave redox potential of the title complex in the three different solvents positively shifts in the order of CH\-2Cl\-2<CH\-3CN<DMF.
