Four ternary lanthanide complexes with unsaturated acid and 1,10-phenanthroline are prepared in methanol and characterized by elemental analysis, molar conductance, UV, IR, (()~1H) NMR and XPS. The results from this p...Four ternary lanthanide complexes with unsaturated acid and 1,10-phenanthroline are prepared in methanol and characterized by elemental analysis, molar conductance, UV, IR, (()~1H) NMR and XPS. The results from this paper show that the complexes Ln(phen)(SA)_3·2H_2O or Ln(phen)(CA)_3·H_2O (Ln=Ce(Ⅲ), Sm(Ⅲ) and Eu(Ⅲ), (phen=1,10-)phenanthroline, SA=Sorbate and CA=Cinnamate) has better anti-inflammatory effect than cerium nitrate and their gremores are steadier than cerium nitrate gremor. And there is a kind of medicament which can replace the cerium nitrate gremor completely in treating burn.展开更多
Two ternary complexes of RE(ClO_4)_3-DPSO-phen and two binary complexes of RE(ClO_4)_3-phen have been synthesized (RE=Eu, Tb; DPSO=diphenyl sulfoxide, phen=1,10-phenanthroline). Elemental analysis and TG-DTA studies s...Two ternary complexes of RE(ClO_4)_3-DPSO-phen and two binary complexes of RE(ClO_4)_3-phen have been synthesized (RE=Eu, Tb; DPSO=diphenyl sulfoxide, phen=1,10-phenanthroline). Elemental analysis and TG-DTA studies suggest that the ternary complexes consist of RE(ClO_4)_3(DPSO)(phen)_3·nH_2O (n=1, 3) and binary complexes consist of RE(phen)_4(ClO_4)_3. IR spectra studies indicate that the DPSO ligand is bonded with RE(Ⅲ) through oxygen atom in sulfinyl group and phen ligand is bonded to RE(Ⅲ) through nitrogen atom. The molar conductivities measured in the acetonitrile solution indicate that two inorganic anions ClO_4^- are coordinated and binary complexes are nonelectrolyte. In the fluorescent spectra it was found that the fluorescence emission intensity of the ternary complexes more intensive than that of the binary complexes.展开更多
Eight new complexes with the general formula of RE(Gly)(NO_3)_3(phen)_2·3H_2O (RE=La, Ce, Pr, Nd, Gd, Sm, Er, Y) were synthesized and characterized by elemental analysis, molar conductivity, IR spectra, UV spectr...Eight new complexes with the general formula of RE(Gly)(NO_3)_3(phen)_2·3H_2O (RE=La, Ce, Pr, Nd, Gd, Sm, Er, Y) were synthesized and characterized by elemental analysis, molar conductivity, IR spectra, UV spectra and thermal analysis. All the complexes are stable in air and their conductance values in acetonitrile lie in the range of 204.1~239.4 S·cm2·mol -1, indicating 1∶2 type electrolytes. The IR shows that all the COO of glycine and oxygen atom of NO_3- take part in the coordination to the RE ions. The thermal behavior of La complex shows that the weight losses at 75~120 ℃ and 145~170 ℃ correspond to the loss of two lattice water molecules and one coordinated water molecules, respectively.展开更多
The title complex M (mnt) (phen), M=Fe11, Co11. Ni11, Cu11. Zn11. was respectivelysynthesized by reaction of disodium maleionitriledithiolate (Na2 (mnt) ) with corresponding metalcomplex M (phen) Cl2. Charge transfer ...The title complex M (mnt) (phen), M=Fe11, Co11. Ni11, Cu11. Zn11. was respectivelysynthesized by reaction of disodium maleionitriledithiolate (Na2 (mnt) ) with corresponding metalcomplex M (phen) Cl2. Charge transfer transitions in the absorption and emission spectra have beenstuded.展开更多
The electrochemical properties of eight new divalent transition metal benzenesulphonate complexes with 1,10-phenanthroline in different solvents and supporting electrolytes were investigated by means of cyclic voltamm...The electrochemical properties of eight new divalent transition metal benzenesulphonate complexes with 1,10-phenanthroline in different solvents and supporting electrolytes were investigated by means of cyclic voltammetry(CV). Based on the CV data the influences of various coordination modes on the electrochemical behavior of the complexes were discussed. The diffusion coefficient D c and rate constant k s of those complexes in DMF systems were estimated according to CV and the results show that these processes were all quasi-reversible.展开更多
Two multidentate ligands 2,9-di[6'-(2″-hydroxyl-3″-methoxyphenyl)-n-2',5'-diazahexyl]-1,10-phenanthroline(LA)and 2,9-di(6'-α-phenol-n-2',5'-diazahexyl)-1,10-phenanthroline(LB)were synthesized and full...Two multidentate ligands 2,9-di[6'-(2″-hydroxyl-3″-methoxyphenyl)-n-2',5'-diazahexyl]-1,10-phenanthroline(LA)and 2,9-di(6'-α-phenol-n-2',5'-diazahexyl)-1,10-phenanthroline(LB)were synthesized and fully characterized.Protonation of the ligands and the stability of the complexes of the ligands with divalent metal ions were investigated.The trinuclear metal complexes [Cu(Ⅱ)and Zn(Ⅱ)] of the ligands were studied,as catalysts,for the transphosphorylation of the RNA-model substrate 2-hydroxypropyl-p-nitrophenyl phosphate(HPNP).The second-order rate constants of HPNP-hydrolysis catalyzed by M3L and M3LH-1 were obtained,which indicated that Zn3LBH-1 was the most efficient catalyst among them.The proposed mechanisms included the activation of the substrate via binding to the metal ions and intramolecular nucleophilic attack by the deprotonated C2-hydroxyl of HPNP.展开更多
1,10-phenanthroline and its derivatives can form charge-transfer complexes with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone(DDQ).The absorption spectra and conditions of complex formation,such as the reaction time,the q...1,10-phenanthroline and its derivatives can form charge-transfer complexes with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone(DDQ).The absorption spectra and conditions of complex formation,such as the reaction time,the quantity of DDQ, and the solvents, have been studied.After the HMO calculation of phenanthrolines,the molar absorptivities were found to depend on the substituents on the phenanthroline rings.展开更多
A series of ternary lanthanide complexes Ln(C6H5CHOHCOO)3(phen)(H2O)(Ln=La,Ce,Pr,Nd,Sm,Eu)were synthesized with α-hydroxyl-phenyl-acetic acid and 1,10-phenanthroline(phen)as ligands.The structure and property of comp...A series of ternary lanthanide complexes Ln(C6H5CHOHCOO)3(phen)(H2O)(Ln=La,Ce,Pr,Nd,Sm,Eu)were synthesized with α-hydroxyl-phenyl-acetic acid and 1,10-phenanthroline(phen)as ligands.The structure and property of complexes were characterized by elemental analysis,IR,1H-NMR,UV and TGA,and the co-ordinate mode of both ligands was discussed.It was shown that the co-ordinate mode of 1,10-phenanthroline was chelated,while α-hydroxyl-phenyl-acetate ion was monodentate or bridging.The mechanism of thermal determined by thermogravimetry was indicated that the degree of co-ordinate ability of ligand was:α-hydroxyl-phenyl-acetate ion > 1,10-phenanthroline(phen).展开更多
The thermal behavior of [Tb_2( m -MBA)_6(phen)_2](H_2O)_2( m -MBA=C_8H_7O_2, methoxybenzoate; phen=C_ 12 H_8N_2, 1,10-phenanthroline) in static air atmosphere was investigated by means of TG-DTG and DTA methods. The...The thermal behavior of [Tb_2( m -MBA)_6(phen)_2](H_2O)_2( m -MBA=C_8H_7O_2, methoxybenzoate; phen=C_ 12 H_8N_2, 1,10-phenanthroline) in static air atmosphere was investigated by means of TG-DTG and DTA methods. The thermal decomposition of the title compound takes place mainly in two steps. The intermediate and the residue for each decomposition were identified by the TG curve. By the kinetic method of processing thermal analysis data put forward by Malek et al ., it is defined that the kinetics model for the first-step thermal decomposition is SB( m,n ).展开更多
A terbium o-methylbenzoate complex with 1,10-phenanthroline, Tb(o-MBA)_3phen(where o-MBA = o-methylbenzoate and phen = 1,10-phenanthroline) was prepared from ethanol solutionand its crystal structure was determined by...A terbium o-methylbenzoate complex with 1,10-phenanthroline, Tb(o-MBA)_3phen(where o-MBA = o-methylbenzoate and phen = 1,10-phenanthroline) was prepared from ethanol solutionand its crystal structure was determined by X-ray diffraction. The crystal of the complexTb(o-MBA)_3phen belongs to triclinic crystal system and P1 (#2) space group. The crystal data are asfollows: a = 1.4371(4) nm, b = 1.7387(2) nm, c = 1.3109(2) nm, α = 96.37(1)°, β = 107.21(2)°,γ= 82.78(2)°, Ⅴ= 3.094(1) nm^3, Z= 2, M_r = 1489.12, D_c= 1.598 g·cm^(-3), μ = 2.330 mm^(-1)and F(000) = 1488.00. The final R and R_w are 0.038 and 0.047 for 8668 [Ⅰ > 2σ(Ⅰ)] uniquereflections, respectively. In the complex each Tb^(3+) ion is eight-coordinated by one1,10-phenanthroline molecule, one bidentate carboxylate group and four bridging carboxylate groups.The carboxylate groups are bonded to the terbium ion in two modes: the chelating bidentate and thebridging bidentate. Excitation and luminescence data observed at room temperature show that thetitle complex emits strong green fluorescence under ultraviolet light. The results of thermalanalysis indicate that the complex Tb(o-MBA)_3phen is quite stable to heat.展开更多
A dinuclear dysprosium(III) complex with benzoic acid and 1,10-phenanthroline, [Dy(BA)3phen]2 (BA = benzoate, PHEN = 1,10-phenanthroline) (C66H46Dy2NaO12, Mr = 1412.07) was synthesized and characterized by ele...A dinuclear dysprosium(III) complex with benzoic acid and 1,10-phenanthroline, [Dy(BA)3phen]2 (BA = benzoate, PHEN = 1,10-phenanthroline) (C66H46Dy2NaO12, Mr = 1412.07) was synthesized and characterized by elemental analysis, UV, IR, X-ray diffraction, molar conductance and TG-DTG techniques. It crystallizes in triclinic, space group P1 with a = 10.773(2), b = 11.933(3), c = 12.417(5) A, α= 105.226(3),β= 93.470(3), γ= 113.475(2)°, V= 1388.0(7), Z = 1, Dc = 1.689 g/cm3, μ(MoKa) = 2.742 mm-1 and F(000) = 698. R = 0.0210, wR = 0.0538. In the crystal, each Dy(III) ion is eight-coordinated by one bidentate chelating carboxylate group, four bidentate bridging carboxylate groups and one 1,10-phenanthroline molecule. The thermal decomposition process of [Dy(BA)3phen]2 has been determined by thermal analysis.展开更多
The complex of [Sm(p-MOBA)3phen]2 (p-MOBA, p-methoxybenzoate; phen,1 10-phenanthroline) was prepared and characterized by elemental analysis, IR, and UV spectroscopy. The thermal decomposition of the [Sm(p-MOBA)...The complex of [Sm(p-MOBA)3phen]2 (p-MOBA, p-methoxybenzoate; phen,1 10-phenanthroline) was prepared and characterized by elemental analysis, IR, and UV spectroscopy. The thermal decomposition of the [Sm(p-MOBA)sphen]2 complex and its kinetics were studied under a static air atmosphere by TG-DTG methods. The intermediate and residue for each decomposition stage were identified from the TG curve. The kinetic parameters and mecha- nisms of the first decomposition stage were obtained from the analysis of the TG-DTG curves by a new method of processing the data of thermal analysis kinetics. The lifetime equation at a mass loss of 10% was deduced as lnr= - 30.6795 + 21034.56/Tby isothermal thermogravimelric analysis.展开更多
A new ternary complex of nickel(II) with L-aspartate (L-Asp) and 1, 10-phenan- throline(Phen), [Ni3(L-Asp)(Phen)5(H2O)3](ClO4)4?4.75H2O, has been synthesized in a mixed sol- vent of H2OC2H5OH at the pH value of 3. I...A new ternary complex of nickel(II) with L-aspartate (L-Asp) and 1, 10-phenan- throline(Phen), [Ni3(L-Asp)(Phen)5(H2O)3](ClO4)4?4.75H2O, has been synthesized in a mixed sol- vent of H2OC2H5OH at the pH value of 3. It crystallizes in triclinic, space group P1 with a = 11.861(2), b = 18.384(4), c = 19.746(3) ?, α = 107.68(1), β = 105.94(1), γ = 103.41(2)°, V = 3703.6(11) ?3, Mr = 1745.66, Z = 2, Dc =1.565 g/cm3, μ = 0.989 mm-1, F(000) = 1791, R = 0.0643 and wR = 0.1611. The complex contains two cations, binuclear [Ni2(L-Asp)(Phen)3(H2O)]2+ and mononu- clear [Ni(Phen)2(H2O)2]2+. All the nickel ions in the complex are six-coordinated with a distorted octahedral geometry, but the coordination environments for them are different. There exist hydrogen bonds and π-π stacking interactions in the complex.展开更多
Some rare earth chelates of(1'-phenyl-3'-methyl-5'-phrazolone-4')-carbonylmethanoic acid and 1, 10-phenanthroline have been synthesized.The composition of the complexes were confirmed by elemental anal...Some rare earth chelates of(1'-phenyl-3'-methyl-5'-phrazolone-4')-carbonylmethanoic acid and 1, 10-phenanthroline have been synthesized.The composition of the complexes were confirmed by elemental analy. sis.The molar conductance,IR,~4H-NMR,electronic spectra and thermogravimetric analysis of the chelates have been measured and discussed.展开更多
2,9-Diformyl-l, 10-phenanthrolinebis(2,6-dimethylanil)cobalt(Ⅱ) perchlorate was synthesized and demonstrated to be [COL2][ClO4]2 by X-ray diffraction analysis. It crystallizes in the monoclinic system, space grou...2,9-Diformyl-l, 10-phenanthrolinebis(2,6-dimethylanil)cobalt(Ⅱ) perchlorate was synthesized and demonstrated to be [COL2][ClO4]2 by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group C2/c with a = 22.294(4), b = 15.122(3), c = 20.640(4) A, β = 119.618(4)°, V = 6048.9(19) A^3, C63H52Cl2CoN9O9, Mr= 1208.97, F(000) = 2504, De= 1.328g/cm^3, Z = 4, μ= 0.436, the final R = 0.0712 and wR = 0.1718 for 1734 observed reflections (I 〉 2σ(I)). In its solid state the helical polymeric chains are supramolecularly associated through intermolecular and interionic hydrogen bonding interactions.展开更多
Three new coordination polymers,namely [Zn(FDA)(phen)(H2O)·H2O]n(1),[Cd(HFDA)(phen)2(NO3)](2) and [Cd(FDA)(phen)]n(3)(H2FDA = 2,5-furandicarboxylic acid,phen = 1,10-phenanthroline) have be...Three new coordination polymers,namely [Zn(FDA)(phen)(H2O)·H2O]n(1),[Cd(HFDA)(phen)2(NO3)](2) and [Cd(FDA)(phen)]n(3)(H2FDA = 2,5-furandicarboxylic acid,phen = 1,10-phenanthroline) have been synthesized by the solvothermal method and characterized by elemental analysis,IR,powder X-ray diffraction,thermogravimetric analysis and X-ray single-crystal diffraction analysis.For 1,the neighboring Zn^2+ ions are bridged by FDA2-as linkers to form one-dimensional(1D) chains,and phen ligands are as the terminal ligands.Furthermore,the 1D chains are packed into a three-dimensional(3D) supramolecular structure through hydrogen bonds and π-π interactions.For 2,the H2FDA ligand is partial deprotonation,which is a rare phenomenon among other coordination polymers based on H2FDA.Under the synergetic effect of phen ligands and the partial deprotonation of H2FDA,the structure of 2 is discrete.For 3,the Cd^2+ ions are linked by two carboxylates of FDA^2-ligand to give rise to 1 D zig-zag chains,and phen ligands chelate the Cd^2+ ions like 1.In addition,solid-state luminescent spectra of three coordination polymers were also studied at room temperature.展开更多
The complex [Cu(phen)2py](ClO4)2 was obtained by the reaction of 1,10-phenanthroline with Cu(ClO4)2·6H2O in water and by recrystallization from pyridine. A single-crystal X-ray study shows that the complex is a ...The complex [Cu(phen)2py](ClO4)2 was obtained by the reaction of 1,10-phenanthroline with Cu(ClO4)2·6H2O in water and by recrystallization from pyridine. A single-crystal X-ray study shows that the complex is a square pyramidal arrangement of five nitrogen atoms from the two 1,10-phenanthroline ligands and one pyridine ligand, respectively. The compound is orthorhombic, C29H21N5Cl2O8Cu, Mr = 701.958, with space group Pbcn, a = 29.9593(3), b = 16.1240(3), c = 11.9183(6) ?, V = 5757.3(3) ?3, Z = 8, Dc = 1.409g/cm3, μ =1.121 mm-1, F(000) = 2465, R = 0.0539, Rw = 0.1380 for 4293 reflections with I >2σ(I). The bond lengths of Cu(1)-N(1), Cu(1)-N(2), Cu(1)-N(3) and Cu(1)-N(4) are 2.223(3), 2.017(3), 2.013(3) and 2.038(3) ?, respectively. The distance from copper to pyridine N(5) is 2.012(3) ?. The angles N(2)-Cu(1)-N(3) and N(4)-Cu(1)-N(5) are 176.1(1) ° and 160.9(1)°, respectively. The angles between axial position nitrogen atom N (1) and four square position nitrogen atoms N(2), N(3), N(4), N(5) are 79.3(1), 98.3(1), 90.7(1), 108.4(1)°, respectively.展开更多
文摘Four ternary lanthanide complexes with unsaturated acid and 1,10-phenanthroline are prepared in methanol and characterized by elemental analysis, molar conductance, UV, IR, (()~1H) NMR and XPS. The results from this paper show that the complexes Ln(phen)(SA)_3·2H_2O or Ln(phen)(CA)_3·H_2O (Ln=Ce(Ⅲ), Sm(Ⅲ) and Eu(Ⅲ), (phen=1,10-)phenanthroline, SA=Sorbate and CA=Cinnamate) has better anti-inflammatory effect than cerium nitrate and their gremores are steadier than cerium nitrate gremor. And there is a kind of medicament which can replace the cerium nitrate gremor completely in treating burn.
文摘Two ternary complexes of RE(ClO_4)_3-DPSO-phen and two binary complexes of RE(ClO_4)_3-phen have been synthesized (RE=Eu, Tb; DPSO=diphenyl sulfoxide, phen=1,10-phenanthroline). Elemental analysis and TG-DTA studies suggest that the ternary complexes consist of RE(ClO_4)_3(DPSO)(phen)_3·nH_2O (n=1, 3) and binary complexes consist of RE(phen)_4(ClO_4)_3. IR spectra studies indicate that the DPSO ligand is bonded with RE(Ⅲ) through oxygen atom in sulfinyl group and phen ligand is bonded to RE(Ⅲ) through nitrogen atom. The molar conductivities measured in the acetonitrile solution indicate that two inorganic anions ClO_4^- are coordinated and binary complexes are nonelectrolyte. In the fluorescent spectra it was found that the fluorescence emission intensity of the ternary complexes more intensive than that of the binary complexes.
文摘Eight new complexes with the general formula of RE(Gly)(NO_3)_3(phen)_2·3H_2O (RE=La, Ce, Pr, Nd, Gd, Sm, Er, Y) were synthesized and characterized by elemental analysis, molar conductivity, IR spectra, UV spectra and thermal analysis. All the complexes are stable in air and their conductance values in acetonitrile lie in the range of 204.1~239.4 S·cm2·mol -1, indicating 1∶2 type electrolytes. The IR shows that all the COO of glycine and oxygen atom of NO_3- take part in the coordination to the RE ions. The thermal behavior of La complex shows that the weight losses at 75~120 ℃ and 145~170 ℃ correspond to the loss of two lattice water molecules and one coordinated water molecules, respectively.
文摘The title complex M (mnt) (phen), M=Fe11, Co11. Ni11, Cu11. Zn11. was respectivelysynthesized by reaction of disodium maleionitriledithiolate (Na2 (mnt) ) with corresponding metalcomplex M (phen) Cl2. Charge transfer transitions in the absorption and emission spectra have beenstuded.
基金Supported by the National Natural Science Foundation of China(No.21576112)Natural Science Foundation Project of Jilin Province(No.20130521019JH and 20150623024TC-19)+1 种基金Natural Science Foundation Project of the Education Department of Jilin Province(No.[2014]152)the Science and Technology Development Plan of Siping City(2015049)
文摘Three lanthanide(III) complexes [Ln(4-NCP)(1,4-BDC)]n·xn H2O(Ln = Pr(1), Sm(2), Nd(3). 4-HNCP = 2-(4-carboxyphenyl)imidazo(4,5-f)(1,10)phenanthroline, 1,4-H2 BDC = benzene-1,4-dicarboxylic acid) have been hydrothermally synthesized and characterized via elemental analysis, infrared spectrometry and single-crystal X-ray diffraction. Structural analyses revealed that complexes 1~3 possess similar porous three-dimensional frameworks with the point symbol {4^(12)·6~3}. Meanwhile, complexes 1~3 exhibit excellent thermal stabilities and complex 2 exhibits characteristic luminescent property.
文摘The electrochemical properties of eight new divalent transition metal benzenesulphonate complexes with 1,10-phenanthroline in different solvents and supporting electrolytes were investigated by means of cyclic voltammetry(CV). Based on the CV data the influences of various coordination modes on the electrochemical behavior of the complexes were discussed. The diffusion coefficient D c and rate constant k s of those complexes in DMF systems were estimated according to CV and the results show that these processes were all quasi-reversible.
基金Supported by the National Natural Science Foundation of China(Nos.20371028and20671052).
文摘Two multidentate ligands 2,9-di[6'-(2″-hydroxyl-3″-methoxyphenyl)-n-2',5'-diazahexyl]-1,10-phenanthroline(LA)and 2,9-di(6'-α-phenol-n-2',5'-diazahexyl)-1,10-phenanthroline(LB)were synthesized and fully characterized.Protonation of the ligands and the stability of the complexes of the ligands with divalent metal ions were investigated.The trinuclear metal complexes [Cu(Ⅱ)and Zn(Ⅱ)] of the ligands were studied,as catalysts,for the transphosphorylation of the RNA-model substrate 2-hydroxypropyl-p-nitrophenyl phosphate(HPNP).The second-order rate constants of HPNP-hydrolysis catalyzed by M3L and M3LH-1 were obtained,which indicated that Zn3LBH-1 was the most efficient catalyst among them.The proposed mechanisms included the activation of the substrate via binding to the metal ions and intramolecular nucleophilic attack by the deprotonated C2-hydroxyl of HPNP.
基金Supported by the National Natural Science Funds.
文摘1,10-phenanthroline and its derivatives can form charge-transfer complexes with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone(DDQ).The absorption spectra and conditions of complex formation,such as the reaction time,the quantity of DDQ, and the solvents, have been studied.After the HMO calculation of phenanthrolines,the molar absorptivities were found to depend on the substituents on the phenanthroline rings.
文摘A series of ternary lanthanide complexes Ln(C6H5CHOHCOO)3(phen)(H2O)(Ln=La,Ce,Pr,Nd,Sm,Eu)were synthesized with α-hydroxyl-phenyl-acetic acid and 1,10-phenanthroline(phen)as ligands.The structure and property of complexes were characterized by elemental analysis,IR,1H-NMR,UV and TGA,and the co-ordinate mode of both ligands was discussed.It was shown that the co-ordinate mode of 1,10-phenanthroline was chelated,while α-hydroxyl-phenyl-acetate ion was monodentate or bridging.The mechanism of thermal determined by thermogravimetry was indicated that the degree of co-ordinate ability of ligand was:α-hydroxyl-phenyl-acetate ion > 1,10-phenanthroline(phen).
基金Supported by the Natural Science Foundation of Hebei Province(No.2 0 2 140 ) and Hebei Education Departm ent(No.2 0 0 112 1)
文摘The thermal behavior of [Tb_2( m -MBA)_6(phen)_2](H_2O)_2( m -MBA=C_8H_7O_2, methoxybenzoate; phen=C_ 12 H_8N_2, 1,10-phenanthroline) in static air atmosphere was investigated by means of TG-DTG and DTA methods. The thermal decomposition of the title compound takes place mainly in two steps. The intermediate and the residue for each decomposition were identified by the TG curve. By the kinetic method of processing thermal analysis data put forward by Malek et al ., it is defined that the kinetics model for the first-step thermal decomposition is SB( m,n ).
基金The project is financially supported by the Natural Science Foundation of Hebei Province (No. 202140 and No. 203148)
文摘A terbium o-methylbenzoate complex with 1,10-phenanthroline, Tb(o-MBA)_3phen(where o-MBA = o-methylbenzoate and phen = 1,10-phenanthroline) was prepared from ethanol solutionand its crystal structure was determined by X-ray diffraction. The crystal of the complexTb(o-MBA)_3phen belongs to triclinic crystal system and P1 (#2) space group. The crystal data are asfollows: a = 1.4371(4) nm, b = 1.7387(2) nm, c = 1.3109(2) nm, α = 96.37(1)°, β = 107.21(2)°,γ= 82.78(2)°, Ⅴ= 3.094(1) nm^3, Z= 2, M_r = 1489.12, D_c= 1.598 g·cm^(-3), μ = 2.330 mm^(-1)and F(000) = 1488.00. The final R and R_w are 0.038 and 0.047 for 8668 [Ⅰ > 2σ(Ⅰ)] uniquereflections, respectively. In the complex each Tb^(3+) ion is eight-coordinated by one1,10-phenanthroline molecule, one bidentate carboxylate group and four bridging carboxylate groups.The carboxylate groups are bonded to the terbium ion in two modes: the chelating bidentate and thebridging bidentate. Excitation and luminescence data observed at room temperature show that thetitle complex emits strong green fluorescence under ultraviolet light. The results of thermalanalysis indicate that the complex Tb(o-MBA)_3phen is quite stable to heat.
基金Supported by NNSFC, NSF of Hebei Province (No. B2007000237)Hebei Education Department (No. 2004325)Hebei Normal University (No. L2006Z06 and L2005Y12)
文摘A dinuclear dysprosium(III) complex with benzoic acid and 1,10-phenanthroline, [Dy(BA)3phen]2 (BA = benzoate, PHEN = 1,10-phenanthroline) (C66H46Dy2NaO12, Mr = 1412.07) was synthesized and characterized by elemental analysis, UV, IR, X-ray diffraction, molar conductance and TG-DTG techniques. It crystallizes in triclinic, space group P1 with a = 10.773(2), b = 11.933(3), c = 12.417(5) A, α= 105.226(3),β= 93.470(3), γ= 113.475(2)°, V= 1388.0(7), Z = 1, Dc = 1.689 g/cm3, μ(MoKa) = 2.742 mm-1 and F(000) = 698. R = 0.0210, wR = 0.0538. In the crystal, each Dy(III) ion is eight-coordinated by one bidentate chelating carboxylate group, four bidentate bridging carboxylate groups and one 1,10-phenanthroline molecule. The thermal decomposition process of [Dy(BA)3phen]2 has been determined by thermal analysis.
基金the Natural Science Foundation of Hebei Province (No. B2007000237)Hebei Education Department (No. 2004325)Hebei Normal University (No. L2006Z06, No. L2005Y12).
文摘The complex of [Sm(p-MOBA)3phen]2 (p-MOBA, p-methoxybenzoate; phen,1 10-phenanthroline) was prepared and characterized by elemental analysis, IR, and UV spectroscopy. The thermal decomposition of the [Sm(p-MOBA)sphen]2 complex and its kinetics were studied under a static air atmosphere by TG-DTG methods. The intermediate and residue for each decomposition stage were identified from the TG curve. The kinetic parameters and mecha- nisms of the first decomposition stage were obtained from the analysis of the TG-DTG curves by a new method of processing the data of thermal analysis kinetics. The lifetime equation at a mass loss of 10% was deduced as lnr= - 30.6795 + 21034.56/Tby isothermal thermogravimelric analysis.
基金This work was supported by the Natural Science Foundation of Guangxi Province (No. 9912044)
文摘A new ternary complex of nickel(II) with L-aspartate (L-Asp) and 1, 10-phenan- throline(Phen), [Ni3(L-Asp)(Phen)5(H2O)3](ClO4)4?4.75H2O, has been synthesized in a mixed sol- vent of H2OC2H5OH at the pH value of 3. It crystallizes in triclinic, space group P1 with a = 11.861(2), b = 18.384(4), c = 19.746(3) ?, α = 107.68(1), β = 105.94(1), γ = 103.41(2)°, V = 3703.6(11) ?3, Mr = 1745.66, Z = 2, Dc =1.565 g/cm3, μ = 0.989 mm-1, F(000) = 1791, R = 0.0643 and wR = 0.1611. The complex contains two cations, binuclear [Ni2(L-Asp)(Phen)3(H2O)]2+ and mononu- clear [Ni(Phen)2(H2O)2]2+. All the nickel ions in the complex are six-coordinated with a distorted octahedral geometry, but the coordination environments for them are different. There exist hydrogen bonds and π-π stacking interactions in the complex.
文摘Some rare earth chelates of(1'-phenyl-3'-methyl-5'-phrazolone-4')-carbonylmethanoic acid and 1, 10-phenanthroline have been synthesized.The composition of the complexes were confirmed by elemental analy. sis.The molar conductance,IR,~4H-NMR,electronic spectra and thermogravimetric analysis of the chelates have been measured and discussed.
文摘2,9-Diformyl-l, 10-phenanthrolinebis(2,6-dimethylanil)cobalt(Ⅱ) perchlorate was synthesized and demonstrated to be [COL2][ClO4]2 by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group C2/c with a = 22.294(4), b = 15.122(3), c = 20.640(4) A, β = 119.618(4)°, V = 6048.9(19) A^3, C63H52Cl2CoN9O9, Mr= 1208.97, F(000) = 2504, De= 1.328g/cm^3, Z = 4, μ= 0.436, the final R = 0.0712 and wR = 0.1718 for 1734 observed reflections (I 〉 2σ(I)). In its solid state the helical polymeric chains are supramolecularly associated through intermolecular and interionic hydrogen bonding interactions.
基金supported by the National Natural Science Foundation of China(21501012)
文摘Three new coordination polymers,namely [Zn(FDA)(phen)(H2O)·H2O]n(1),[Cd(HFDA)(phen)2(NO3)](2) and [Cd(FDA)(phen)]n(3)(H2FDA = 2,5-furandicarboxylic acid,phen = 1,10-phenanthroline) have been synthesized by the solvothermal method and characterized by elemental analysis,IR,powder X-ray diffraction,thermogravimetric analysis and X-ray single-crystal diffraction analysis.For 1,the neighboring Zn^2+ ions are bridged by FDA2-as linkers to form one-dimensional(1D) chains,and phen ligands are as the terminal ligands.Furthermore,the 1D chains are packed into a three-dimensional(3D) supramolecular structure through hydrogen bonds and π-π interactions.For 2,the H2FDA ligand is partial deprotonation,which is a rare phenomenon among other coordination polymers based on H2FDA.Under the synergetic effect of phen ligands and the partial deprotonation of H2FDA,the structure of 2 is discrete.For 3,the Cd^2+ ions are linked by two carboxylates of FDA^2-ligand to give rise to 1 D zig-zag chains,and phen ligands chelate the Cd^2+ ions like 1.In addition,solid-state luminescent spectra of three coordination polymers were also studied at room temperature.
文摘The complex [Cu(phen)2py](ClO4)2 was obtained by the reaction of 1,10-phenanthroline with Cu(ClO4)2·6H2O in water and by recrystallization from pyridine. A single-crystal X-ray study shows that the complex is a square pyramidal arrangement of five nitrogen atoms from the two 1,10-phenanthroline ligands and one pyridine ligand, respectively. The compound is orthorhombic, C29H21N5Cl2O8Cu, Mr = 701.958, with space group Pbcn, a = 29.9593(3), b = 16.1240(3), c = 11.9183(6) ?, V = 5757.3(3) ?3, Z = 8, Dc = 1.409g/cm3, μ =1.121 mm-1, F(000) = 2465, R = 0.0539, Rw = 0.1380 for 4293 reflections with I >2σ(I). The bond lengths of Cu(1)-N(1), Cu(1)-N(2), Cu(1)-N(3) and Cu(1)-N(4) are 2.223(3), 2.017(3), 2.013(3) and 2.038(3) ?, respectively. The distance from copper to pyridine N(5) is 2.012(3) ?. The angles N(2)-Cu(1)-N(3) and N(4)-Cu(1)-N(5) are 176.1(1) ° and 160.9(1)°, respectively. The angles between axial position nitrogen atom N (1) and four square position nitrogen atoms N(2), N(3), N(4), N(5) are 79.3(1), 98.3(1), 90.7(1), 108.4(1)°, respectively.