The crystal and molecular structures of Schiff base bis(salicylidene)-p-diaminobenzene were determined by X-ray crystallography. It crystallized in a monoclinic system with space group P2(1)/c, lattice parameters a=1....The crystal and molecular structures of Schiff base bis(salicylidene)-p-diaminobenzene were determined by X-ray crystallography. It crystallized in a monoclinic system with space group P2(1)/c, lattice parameters a=1.4649(3) nm, b=0.45770(9) nm, c=1.2241(2) nm, α=γ=90.00°, β=112.07(3)°, V=(0.7606(3) nm^3,) and Z=4. The crystal structure of the title compound is composed of discrete monomeric molecule of ((C_6H_4)(NCC_6H_4OH)_2) which is planar. The intermolecular hydrogen bonds make the compound steady.展开更多
A novel compound PMPP-SAL (1-phenyl-3-methyl-4-(salicylidene hydrazide)- propenylidene-pyrazolone-5) has been synthesized and characterized by elemental analysis, IR,^1H NMR and single-crystal X-ray diffraction. T...A novel compound PMPP-SAL (1-phenyl-3-methyl-4-(salicylidene hydrazide)- propenylidene-pyrazolone-5) has been synthesized and characterized by elemental analysis, IR,^1H NMR and single-crystal X-ray diffraction. The X-ray diffraction reveals that the compound is of orthorhombic, space group Pbca with a=16.132(5), b=10.113(3), c=23.143(7) A, V=3776(2)A°^3, Z=8, C20H20N4O3, Mr=364.40, Dc =1.282 g/cm^3, F(000)=1536,μ(MoKa)=0.089 mm^-1, S=0.992, R=0.0578 and wR=0.1362 for 1871 observed reflections with I〉2σ(I). In the crystal, the compound possesses two C=O bonds and exists in the NH-form' other than NH-form.展开更多
Dye sensitized solar cell represents a promising method for the conversion of solar energy to electric energy. In the present work free N,N'-bis(salicyli-dene)ethylenediamine and its copper (II) complex were synth...Dye sensitized solar cell represents a promising method for the conversion of solar energy to electric energy. In the present work free N,N'-bis(salicyli-dene)ethylenediamine and its copper (II) complex were synthesized, characterized, and investigated for use as dye sensitizers in the fabrication of dye sensitized solar cells. The dyes were characterized using UV-Vis, Steady State Florescence, and Fluorescence Lifetime, Thermogravimetric Analysis, Differential Scanning Calorimetry, and Cyclic Voltammetry. The thermogravimetric analyses of the ligand and the ligand Copper complex demonstrate the stabilizing effect of the copper ion on the ligand complex. Additionally, the copper ion is shown to stabilize the structure, as evidenced by the 150oC increase in the extrapolated onset temperature of the decomposition event. The ligand copper complex is further stabilized by the presence of the copper, which is determined by the 6.34% residue that remained at the end of the thermogravimetric analysis, compared with 0% residue when applying the same condition for the ligand without copper. The current-voltage characteristics of the cells and the electrochemical impedance were determined. The photovoltaic performance of the solar cell devices fabricated using N,N'-bis(salicylidene) ethylenediamine dye was found to be slightly better than those produced from the copper complex. The solar to electric power efficiency of the ligand-based dye sensitized solar cell was 0.14% and that of the copper complex was found to 0.12%. Although the difference in the cell efficiency is quite small, it is obvious that the insertion of Copper into the ligand did not enhance the performance of the solar cells. The photocurrent-photovoltage results are consistent with the absorption spectra that showed a more prominent band for the ligand. The free hydroxyl groups, present in the ligand but absent from the copper complex owing to their coordination with the copper metal, could be responsible for the difference in the performance of the devices. The hydroxyl groups get attached to the TiO2 and facilitate the transfer of electrons.展开更多
Positive electrospray ionization tandem mass spectrometry was applied to study four newly synthesized(12-aminodehydroabietylamine)acetamide-substituted salicylidene Schiff bases(ADASSSB).The results showed that the MS...Positive electrospray ionization tandem mass spectrometry was applied to study four newly synthesized(12-aminodehydroabietylamine)acetamide-substituted salicylidene Schiff bases(ADASSSB).The results showed that the MSn characteristics of ADASSSB can be used for their qualitative and quantitative analysis.展开更多
The Co(II) complex I and ammonium salt II were synthesized from the direct reaction of 1,2-ethylenediamine and cobaltous acetate tetrahydrate and manganese acetate tetrahydrate in anhydrous ethanol. Treatment of N,N...The Co(II) complex I and ammonium salt II were synthesized from the direct reaction of 1,2-ethylenediamine and cobaltous acetate tetrahydrate and manganese acetate tetrahydrate in anhydrous ethanol. Treatment of N,N'-bis(salicylidene)ethylenediamine with Cu(OAc)2·H2O results in the formation of Cu(II) complex III. C14H37CoNaO8 (I): triclinic, space group P1, a = 8.6296(12), b = 12.0291(17), c = 12.1108(17) A, α = 75.335(2), β = 69.991(2), γ = 72.248(2)°, V= 1109.4(3) A3, Z = 2, ρcaloa = 1.342 g/cm3, the final R= 0.0342 for 4817 observed reflections with I 〉 2σ(I) and Rw = 0.1263 for all data. C6H16N204 (II): space group P1, a = 5.5513(10), b = 5.5589(11), c = 7.4437(14) A, α = 94.332(4), β = 104.497(4), γ = 103.487(4)°,V= 214.06(7) A3, Z = 1, ρcalcd = 1.398 g/cm3, the final R = 0.0431 for 829 observed reflections with I〉 2σ(I) and Rw = 0.1263 for all data. C14H37CuN40 (III), space group P21/n, a = 9.050(9), b = 18.434(17), c = 11.659(11) A, β = 107.134(19)°, V= 1859(3) A3, Z = 4, ρcalcd =1.443 g/cm3, the final R = 0.0616 for 3308 observed reflections (O 〉 2σ(I)) and Rw = 0.1229 for all data. Their structures were all determined by X-ray diffraction, elemental analysis and IR.展开更多
Ultrasound-assisted emulsification–microextraction followed by inductively coupled plasma–optical emission spectrometry was utilized for simultaneous pre-concentration and trace detection of lead,bismuth,and iron in...Ultrasound-assisted emulsification–microextraction followed by inductively coupled plasma–optical emission spectrometry was utilized for simultaneous pre-concentration and trace detection of lead,bismuth,and iron in water samples.Disodium N,N-bis(salicylidene)ethylenediamine and trichloroethylene were used as chelating agent and extraction solvent,respectively.The parameters of interest were volume of extraction solvent,temperature,and concentrations of salt and chelating agent.A fractional factorial design was developed to identify these parameters and how they vary with one another.The results demonstrated that the concentrations of salt and chelating agent affected extraction efficiency.Subsequently,a central-composite design was used to acquire optimum levels of effective parameters.The optimal conditions were 160.7 mg L^(−1) and 1.77%(w/v)for concentration of chelating agent and salt,respectively.The linear dynamic ranges were determined to be 1–1000μg L^(−1) for Pb and Bi,and 10–1000μg L^(−1) for Fe.The correlation coefficient(R2)was 0.990–0.995.The limits of detection were 0.54–0.78μg L^(−1).The relative standard deviation(concentration=200μg L^(−1),n=8)was in the range of 2.0–4.3%.This method was successfully applied for the trace detection of Pb,Bi,and Fe in freshwater samples of waterfall and spring and satisfactory relative recoveries(96.2–99.6%)were obtained.展开更多
基金Supported by the National Natural Science Foundation of China(No.2 0 2 75 0 2 0 ) the Natural Science Foundation ofShandong Province(No.Z2 0 0 2 B0 2 ) and the Outstanding Adult- young Scientific Research Encouraging Foundation of Shan-dong Provinc
文摘The crystal and molecular structures of Schiff base bis(salicylidene)-p-diaminobenzene were determined by X-ray crystallography. It crystallized in a monoclinic system with space group P2(1)/c, lattice parameters a=1.4649(3) nm, b=0.45770(9) nm, c=1.2241(2) nm, α=γ=90.00°, β=112.07(3)°, V=(0.7606(3) nm^3,) and Z=4. The crystal structure of the title compound is composed of discrete monomeric molecule of ((C_6H_4)(NCC_6H_4OH)_2) which is planar. The intermolecular hydrogen bonds make the compound steady.
基金This work was supported by the National Natural Science Foundation of China (20262005 and 20366005)
文摘A novel compound PMPP-SAL (1-phenyl-3-methyl-4-(salicylidene hydrazide)- propenylidene-pyrazolone-5) has been synthesized and characterized by elemental analysis, IR,^1H NMR and single-crystal X-ray diffraction. The X-ray diffraction reveals that the compound is of orthorhombic, space group Pbca with a=16.132(5), b=10.113(3), c=23.143(7) A, V=3776(2)A°^3, Z=8, C20H20N4O3, Mr=364.40, Dc =1.282 g/cm^3, F(000)=1536,μ(MoKa)=0.089 mm^-1, S=0.992, R=0.0578 and wR=0.1362 for 1871 observed reflections with I〉2σ(I). In the crystal, the compound possesses two C=O bonds and exists in the NH-form' other than NH-form.
文摘Dye sensitized solar cell represents a promising method for the conversion of solar energy to electric energy. In the present work free N,N'-bis(salicyli-dene)ethylenediamine and its copper (II) complex were synthesized, characterized, and investigated for use as dye sensitizers in the fabrication of dye sensitized solar cells. The dyes were characterized using UV-Vis, Steady State Florescence, and Fluorescence Lifetime, Thermogravimetric Analysis, Differential Scanning Calorimetry, and Cyclic Voltammetry. The thermogravimetric analyses of the ligand and the ligand Copper complex demonstrate the stabilizing effect of the copper ion on the ligand complex. Additionally, the copper ion is shown to stabilize the structure, as evidenced by the 150oC increase in the extrapolated onset temperature of the decomposition event. The ligand copper complex is further stabilized by the presence of the copper, which is determined by the 6.34% residue that remained at the end of the thermogravimetric analysis, compared with 0% residue when applying the same condition for the ligand without copper. The current-voltage characteristics of the cells and the electrochemical impedance were determined. The photovoltaic performance of the solar cell devices fabricated using N,N'-bis(salicylidene) ethylenediamine dye was found to be slightly better than those produced from the copper complex. The solar to electric power efficiency of the ligand-based dye sensitized solar cell was 0.14% and that of the copper complex was found to 0.12%. Although the difference in the cell efficiency is quite small, it is obvious that the insertion of Copper into the ligand did not enhance the performance of the solar cells. The photocurrent-photovoltage results are consistent with the absorption spectra that showed a more prominent band for the ligand. The free hydroxyl groups, present in the ligand but absent from the copper complex owing to their coordination with the copper metal, could be responsible for the difference in the performance of the devices. The hydroxyl groups get attached to the TiO2 and facilitate the transfer of electrons.
文摘Positive electrospray ionization tandem mass spectrometry was applied to study four newly synthesized(12-aminodehydroabietylamine)acetamide-substituted salicylidene Schiff bases(ADASSSB).The results showed that the MSn characteristics of ADASSSB can be used for their qualitative and quantitative analysis.
文摘The Co(II) complex I and ammonium salt II were synthesized from the direct reaction of 1,2-ethylenediamine and cobaltous acetate tetrahydrate and manganese acetate tetrahydrate in anhydrous ethanol. Treatment of N,N'-bis(salicylidene)ethylenediamine with Cu(OAc)2·H2O results in the formation of Cu(II) complex III. C14H37CoNaO8 (I): triclinic, space group P1, a = 8.6296(12), b = 12.0291(17), c = 12.1108(17) A, α = 75.335(2), β = 69.991(2), γ = 72.248(2)°, V= 1109.4(3) A3, Z = 2, ρcaloa = 1.342 g/cm3, the final R= 0.0342 for 4817 observed reflections with I 〉 2σ(I) and Rw = 0.1263 for all data. C6H16N204 (II): space group P1, a = 5.5513(10), b = 5.5589(11), c = 7.4437(14) A, α = 94.332(4), β = 104.497(4), γ = 103.487(4)°,V= 214.06(7) A3, Z = 1, ρcalcd = 1.398 g/cm3, the final R = 0.0431 for 829 observed reflections with I〉 2σ(I) and Rw = 0.1263 for all data. C14H37CuN40 (III), space group P21/n, a = 9.050(9), b = 18.434(17), c = 11.659(11) A, β = 107.134(19)°, V= 1859(3) A3, Z = 4, ρcalcd =1.443 g/cm3, the final R = 0.0616 for 3308 observed reflections (O 〉 2σ(I)) and Rw = 0.1229 for all data. Their structures were all determined by X-ray diffraction, elemental analysis and IR.
文摘Ultrasound-assisted emulsification–microextraction followed by inductively coupled plasma–optical emission spectrometry was utilized for simultaneous pre-concentration and trace detection of lead,bismuth,and iron in water samples.Disodium N,N-bis(salicylidene)ethylenediamine and trichloroethylene were used as chelating agent and extraction solvent,respectively.The parameters of interest were volume of extraction solvent,temperature,and concentrations of salt and chelating agent.A fractional factorial design was developed to identify these parameters and how they vary with one another.The results demonstrated that the concentrations of salt and chelating agent affected extraction efficiency.Subsequently,a central-composite design was used to acquire optimum levels of effective parameters.The optimal conditions were 160.7 mg L^(−1) and 1.77%(w/v)for concentration of chelating agent and salt,respectively.The linear dynamic ranges were determined to be 1–1000μg L^(−1) for Pb and Bi,and 10–1000μg L^(−1) for Fe.The correlation coefficient(R2)was 0.990–0.995.The limits of detection were 0.54–0.78μg L^(−1).The relative standard deviation(concentration=200μg L^(−1),n=8)was in the range of 2.0–4.3%.This method was successfully applied for the trace detection of Pb,Bi,and Fe in freshwater samples of waterfall and spring and satisfactory relative recoveries(96.2–99.6%)were obtained.