Metal (Me=Fe(III), Mo(VI), Mn(II), Co(II), Ni(II), Zn(II) and Cu(II)) 2-hydroxy-1-naphthaldehyde thiosemicarbazone complexes (MeHNT) were synthesized and used as mimic-enzyme catalysts to mimic the active group of hor...Metal (Me=Fe(III), Mo(VI), Mn(II), Co(II), Ni(II), Zn(II) and Cu(II)) 2-hydroxy-1-naphthaldehyde thiosemicarbazone complexes (MeHNT) were synthesized and used as mimic-enzyme catalysts to mimic the active group of horseradish peroxidase (HRP). The results showed that Fe-HNT, Mo-HNT are effective catalysts, which have similar catalytic activity as HRP. The sequence of catalytic activities of tested biomimic peroxidas is Mo-HNT > Fe-HNT > Zn-HNT > Ni-HNT > Mn-HNT. Among them, Fe-HNT is used as a mimic-enzyme catalyst in determination of ascorbic acid and glucose by coupling the catalytic reaction of glucose oxidase.展开更多
The ion transfer reaction of 2-benzoylpyridine-thiosemicarbazone (HL), which has antimicrobial and antifungal properties and anticancer activity, has been studied to determine its lipophilicity by cyclic voltammetry a...The ion transfer reaction of 2-benzoylpyridine-thiosemicarbazone (HL), which has antimicrobial and antifungal properties and anticancer activity, has been studied to determine its lipophilicity by cyclic voltammetry at the water/1,2-dichloroethane (1,2-DCE) interface. The physicochemical parameters such as standard partition coefficient (lgPI)andthestandardGibbsenergyoftransfer("G0tr,,wI "o)oftheprotonatedformoftheligandwere measured asa function of pH in aqueous phase. The protonated form of the ligand exhibited reversible or quasi-reversible voltammograms at the1,2-DCEintherangeofpH1-5.Theprotonationconstantsoftheligand,pKa1andpKa2,weredeterminedspectrophotometrically and were found to be 12.14 and 3.24, respectively. The standard Gibbs energy of transfer ("G0tr,,wN" o) and the partition coefficient of neutral species (lgPN) were also determined by the shake-flask method. The standard Gibbs energy of transfer of this compound across the water/1,2-DCE interface was evaluated as the quantitative measure of its lipophilicity. The difference between lgPI and lgPN was related to the degree of charge delocalization and was used to evaluate qualitatively the lipophilicity of the ligand.展开更多
Acetylthiophene thiosemicarbazone(C4H4S) C (CH3)=NNHC-SNH2-·1/2H2O has been prepared by the condensation of 2-acetylthiophene with thiosemicarbazide. This compound crystallized in monoclinic space group P21/c wi...Acetylthiophene thiosemicarbazone(C4H4S) C (CH3)=NNHC-SNH2-·1/2H2O has been prepared by the condensation of 2-acetylthiophene with thiosemicarbazide. This compound crystallized in monoclinic space group P21/c with unit cell parameters: a = 15. 909 (2) , b = 5 .424 (3)A,β=108. 59 (1)°,V=1989 (1)A 3, Z=8, Dc= 1.391g/cm3, F(000)= 872, λ=0.71073 A,μ(MoKα) = 4. 7 cm-1, final RO= 0.36 for 2852 observed reflections. Analysis of molecular structure reveals that this Schiff base possesses the E-form configuration. Each asymmetric unit contains two thiosemicarbazones and one water molecule which form hydrogen bonds statistically.展开更多
The title compound crystallized in space goups P2(1)/c with Z=4, in a unit cell of dimensions, a=12.964(4), b=5.131(5), c=14.970(1)Angstrom; V=9331(1) Angstrom(3) Dc=1.429gcm(-3), mu=0.541mm(-1), R=0.045, Rw=0.059. Th...The title compound crystallized in space goups P2(1)/c with Z=4, in a unit cell of dimensions, a=12.964(4), b=5.131(5), c=14.970(1)Angstrom; V=9331(1) Angstrom(3) Dc=1.429gcm(-3), mu=0.541mm(-1), R=0.045, Rw=0.059. The equilibrium constant of the ligand with CdBr2 was obtained by polarographic method. Crystal structure determination revealed that the molecule is in transconformation and non-hydrogen atoms of the molecule are in one plane except N(3) atom.展开更多
Nickel(II) reacts with 2-acetylpyridine-4-methyl-3-thiosemicarbazone (APMT) and forms a yellow colored complex, which was extracted into n-hexanol from sodium acetate and acetic acid buffer at pH 6.0. The absorbance v...Nickel(II) reacts with 2-acetylpyridine-4-methyl-3-thiosemicarbazone (APMT) and forms a yellow colored complex, which was extracted into n-hexanol from sodium acetate and acetic acid buffer at pH 6.0. The absorbance value of the Ni(II)-APMT complex was measured at different intervals of time at 375 nm to ascertain the time stability of the complex. The extraction of the complex into the solvent was instantaneous and stable for more than 72 hrs. The system obeyed Beer’s law in the concentration range of 0.235 - 2.43 μg·ml–1 of nickel(II), with an excellent linearity and a correlation coefficient of 0.999. The molar absorptivity and Sandell’s sensitivity of the extracted species were found to be 2.16 × 104 L mol–1 ·cm–1 and 0.003 μg·cm–2 at 375 nm, respectively. Hence a detailed study of the extraction of nickel(II) with APMT has been undertaken with a view to developing a rapid and sensitive extractive spectrophotometric method for the determination of nickel(II) when present alone or in the presence of diverse ions which are usually associated with nickel(II) in environmental matrices like soil and industrial effluents. Various standard alloy samples (CM 247 LC, IN 718, BCS 233, 266, 253 and 251) have been tested for the determination of nickel for the purpose of validation of the present method. The results of the proposed method are comparable with those from atomic absorption spectrometry and were found to be in good agreement.展开更多
Ti(Ⅳ),Ni(Ⅱ),Cu(Ⅰ) complexes bearing mono(2-chlorobenzaldehyde)-thiosemicarbazone(HL) were synthesized in non-aqueous solvent containing ligand(HL) by the electrochemical oxidation of anodic metal with Ti,Ni and Cu,...Ti(Ⅳ),Ni(Ⅱ),Cu(Ⅰ) complexes bearing mono(2-chlorobenzaldehyde)-thiosemicarbazone(HL) were synthesized in non-aqueous solvent containing ligand(HL) by the electrochemical oxidation of anodic metal with Ti,Ni and Cu,respectively.The complexes were characterized by elemental analysis,IR,UV,magnetic susceptibility and molar conductivity etc.展开更多
文摘Metal (Me=Fe(III), Mo(VI), Mn(II), Co(II), Ni(II), Zn(II) and Cu(II)) 2-hydroxy-1-naphthaldehyde thiosemicarbazone complexes (MeHNT) were synthesized and used as mimic-enzyme catalysts to mimic the active group of horseradish peroxidase (HRP). The results showed that Fe-HNT, Mo-HNT are effective catalysts, which have similar catalytic activity as HRP. The sequence of catalytic activities of tested biomimic peroxidas is Mo-HNT > Fe-HNT > Zn-HNT > Ni-HNT > Mn-HNT. Among them, Fe-HNT is used as a mimic-enzyme catalyst in determination of ascorbic acid and glucose by coupling the catalytic reaction of glucose oxidase.
基金the Scientific Research Projects (BAP) of Selcuk University, Turkey (2003/151).
文摘The ion transfer reaction of 2-benzoylpyridine-thiosemicarbazone (HL), which has antimicrobial and antifungal properties and anticancer activity, has been studied to determine its lipophilicity by cyclic voltammetry at the water/1,2-dichloroethane (1,2-DCE) interface. The physicochemical parameters such as standard partition coefficient (lgPI)andthestandardGibbsenergyoftransfer("G0tr,,wI "o)oftheprotonatedformoftheligandwere measured asa function of pH in aqueous phase. The protonated form of the ligand exhibited reversible or quasi-reversible voltammograms at the1,2-DCEintherangeofpH1-5.Theprotonationconstantsoftheligand,pKa1andpKa2,weredeterminedspectrophotometrically and were found to be 12.14 and 3.24, respectively. The standard Gibbs energy of transfer ("G0tr,,wN" o) and the partition coefficient of neutral species (lgPN) were also determined by the shake-flask method. The standard Gibbs energy of transfer of this compound across the water/1,2-DCE interface was evaluated as the quantitative measure of its lipophilicity. The difference between lgPI and lgPN was related to the degree of charge delocalization and was used to evaluate qualitatively the lipophilicity of the ligand.
文摘Acetylthiophene thiosemicarbazone(C4H4S) C (CH3)=NNHC-SNH2-·1/2H2O has been prepared by the condensation of 2-acetylthiophene with thiosemicarbazide. This compound crystallized in monoclinic space group P21/c with unit cell parameters: a = 15. 909 (2) , b = 5 .424 (3)A,β=108. 59 (1)°,V=1989 (1)A 3, Z=8, Dc= 1.391g/cm3, F(000)= 872, λ=0.71073 A,μ(MoKα) = 4. 7 cm-1, final RO= 0.36 for 2852 observed reflections. Analysis of molecular structure reveals that this Schiff base possesses the E-form configuration. Each asymmetric unit contains two thiosemicarbazones and one water molecule which form hydrogen bonds statistically.
文摘The title compound crystallized in space goups P2(1)/c with Z=4, in a unit cell of dimensions, a=12.964(4), b=5.131(5), c=14.970(1)Angstrom; V=9331(1) Angstrom(3) Dc=1.429gcm(-3), mu=0.541mm(-1), R=0.045, Rw=0.059. The equilibrium constant of the ligand with CdBr2 was obtained by polarographic method. Crystal structure determination revealed that the molecule is in transconformation and non-hydrogen atoms of the molecule are in one plane except N(3) atom.
文摘Nickel(II) reacts with 2-acetylpyridine-4-methyl-3-thiosemicarbazone (APMT) and forms a yellow colored complex, which was extracted into n-hexanol from sodium acetate and acetic acid buffer at pH 6.0. The absorbance value of the Ni(II)-APMT complex was measured at different intervals of time at 375 nm to ascertain the time stability of the complex. The extraction of the complex into the solvent was instantaneous and stable for more than 72 hrs. The system obeyed Beer’s law in the concentration range of 0.235 - 2.43 μg·ml–1 of nickel(II), with an excellent linearity and a correlation coefficient of 0.999. The molar absorptivity and Sandell’s sensitivity of the extracted species were found to be 2.16 × 104 L mol–1 ·cm–1 and 0.003 μg·cm–2 at 375 nm, respectively. Hence a detailed study of the extraction of nickel(II) with APMT has been undertaken with a view to developing a rapid and sensitive extractive spectrophotometric method for the determination of nickel(II) when present alone or in the presence of diverse ions which are usually associated with nickel(II) in environmental matrices like soil and industrial effluents. Various standard alloy samples (CM 247 LC, IN 718, BCS 233, 266, 253 and 251) have been tested for the determination of nickel for the purpose of validation of the present method. The results of the proposed method are comparable with those from atomic absorption spectrometry and were found to be in good agreement.
文摘Ti(Ⅳ),Ni(Ⅱ),Cu(Ⅰ) complexes bearing mono(2-chlorobenzaldehyde)-thiosemicarbazone(HL) were synthesized in non-aqueous solvent containing ligand(HL) by the electrochemical oxidation of anodic metal with Ti,Ni and Cu,respectively.The complexes were characterized by elemental analysis,IR,UV,magnetic susceptibility and molar conductivity etc.