A novel binucleus mixed-ligand[Cd2(phen)4(bmal)2]·3H2O (phen=phenanthroline; bmal=benzylmalonic acid radical) has been synthesized by the reaction of phen and bmal with cadmium(Ⅱ) salt. X-ray crystal structure a...A novel binucleus mixed-ligand[Cd2(phen)4(bmal)2]·3H2O (phen=phenanthroline; bmal=benzylmalonic acid radical) has been synthesized by the reaction of phen and bmal with cadmium(Ⅱ) salt. X-ray crystal structure analysis was carried out to determine the crystal structure of the title complex. The crystal of the title complex belongs to monoclinic system with space group P21/c, a=1.119 1(8) nm, b=2.480 5(17) nm, c=1.063 4(8) nm, β=142.042(12)°, Z=4, V=2.887(3) nm3, Dc=1.613 g·cm-3, R1=0.046 2, wR2=0.115 6, F(000)=1 424. One carboxyl of bmal is coordinated to Cd(1) with monodentate form, the others are coordinated to Cd(2) with bidentate form. The complexes form a 1-D chain structure bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in bmal, the 2-D network structure was formed by π-π interaction of neighbouring phen. CCDC: 257080.展开更多
Binuclear mixed valent manganese complex [(Phen) 2Mn( μ O) 2Mn(Phen) 2] (ClO 4) 3·CH 2ClCOOH·2H 2O was synthesized by the reaction of [Mn 3O(O 2CCH 2Cl) 6(C 5H 5N) 2(H 2O)] ·CH 2ClCOO·H 2O with Ph...Binuclear mixed valent manganese complex [(Phen) 2Mn( μ O) 2Mn(Phen) 2] (ClO 4) 3·CH 2ClCOOH·2H 2O was synthesized by the reaction of [Mn 3O(O 2CCH 2Cl) 6(C 5H 5N) 2(H 2O)] ·CH 2ClCOO·H 2O with Phen and NaClO 4 in the CH 2ClCOOH CH 2ClCOONa buffer (pH=4.0). X ray diffraction result for the single crystal shows that the crystal is triclinic, space group P 1, with a =\{1.182 64(7)\} nm, b =1.449 32(8) nm, c =1.664 99(9) nm, α =104.585 0(10)°, β =97.123 0(10)°, \{ γ =\}106.921 0(10)°, V =2.581 6(3) nm 3, Z =2, D c=1.660 g·cm -3 , R =0.052 2. A peak at 640 nm in UV Vis spectrum is designed to the electronic transition of bridge legend O 2- to Mn(Ⅲ). Cyclic voltammogram shows that the complex in CH 3CN undergoes two quasi reversible one electron redox reactions at E 1/2 =1.25 V and E 1/2 =0.33 V, respectively.展开更多
EPR spectra of three new quaternary gadolinium complexes(I： [Gd(C6H5COO)2(NO3)(bipy)]2,Ⅱ： [Gd(m- CH3C6H4COO)2(NO3)(phen)]2 andⅢ： [Gd(p- CH3C6H4COO)(NO3)(phen)]2) with mixed anion ligands in polycrystalline powder...EPR spectra of three new quaternary gadolinium complexes(I： [Gd(C6H5COO)2(NO3)(bipy)]2,Ⅱ： [Gd(m- CH3C6H4COO)2(NO3)(phen)]2 andⅢ： [Gd(p- CH3C6H4COO)(NO3)(phen)]2) with mixed anion ligands in polycrystalline powders and solutions have been investigated at different temperatures and solvents.New behavior of EPR spectra of complexⅢ was first observed in polycrystalline powder at 77K and three types of EPR spectra for three complexes,symmetry resonance spectrum for the complexⅡ ,U spectrum for the complexⅢ ,and asymmetry resonance spectrum for the complex I.The relationship of EPR features between the crystal- field strength in the complexes and local symmetry around Gd(Ⅲ ) was discussed.The crystal- field parameters b20 and asymmetry parametersλ′ of the complexes I andⅢ were estimated.展开更多
A new mixed-valence trinuclear oxo-centered manganese complex Mn3O(O2CCC l3)6(py)2(H2O) was prepared by the reaction of NnBu4MnO4 with Mn(OAc)2·4H2O, t richloroacetic acid and pyridine in absolute EtOH. The cryst...A new mixed-valence trinuclear oxo-centered manganese complex Mn3O(O2CCC l3)6(py)2(H2O) was prepared by the reaction of NnBu4MnO4 with Mn(OAc)2·4H2O, t richloroacetic acid and pyridine in absolute EtOH. The crystal structure was det ermined. The complex crystallizes in monoclinic, space group P21/c, unit cell pa rameters, a=14.951(1), b=20.791(2), c=17.882(1),á=?=90a=102.67(1)展开更多
Complex [Tb(2-FC6H4COO)3·C10H8N2]2 was synthesized from TbCl3·nH2O,2-fluorobenzoic acid,and 2,2′-bipyridine(C10H8N2).The crystals are monoclinic with space group P21/n,and the crystal parameters are:a=1.21...Complex [Tb(2-FC6H4COO)3·C10H8N2]2 was synthesized from TbCl3·nH2O,2-fluorobenzoic acid,and 2,2′-bipyridine(C10H8N2).The crystals are monoclinic with space group P21/n,and the crystal parameters are:a=1.219 1（4） nm,b=1.777 4（6） nm,c=1.371 5（4） nm,β=111.400（5）,（M=）732.41,V=2.767（15） nm3,Z=4,Dcalc=1.758 g/cm3,T=293（2） K.The final R=0.030 2,（wR=）0.054 7.The two Tb3+ ions are linked together by four 2-fluorobenzoate groups in a bridging mode to form a dimeric unit.Each Tb3+ ion is also chelated by one 2-fluorobenzoate group and one 2,2′-bipy ligand,making a coordination number of eight.There are four emission peaks in the luminescence spectrum at 490,545,584,and 618 nm,corresponding to the transitions of the Tb3+ ion:5D4→7F6,5D4→7F5,5D4→7F4,and(5D4→)7F3,respectively.展开更多
The complex \ 2 Complex LI Xia *, JIN Qiong Hua (Department of Chemistry,Capital Normal University,Beijing 100037) Abstract The complex \[Nd(C 4 H 3 OCOO) 2 ·NO 3 ·C 10 H 8 N 2 \] 2 was synthesized from Nd(N...The complex \ 2 Complex LI Xia *, JIN Qiong Hua (Department of Chemistry,Capital Normal University,Beijing 100037) Abstract The complex \[Nd(C 4 H 3 OCOO) 2 ·NO 3 ·C 10 H 8 N 2 \] 2 was synthesized from Nd(NO 3 ) 3 · n H 2 O, 2 furancarboxylic acid(C 4 H 3 OCOOH), and 2,2′ bipyridine(C 10 H 8 N 2 ). The unit cell is triclinic and of Pī symmetry. Unit cell parameters are:Pī, a =0 992 18(17) nm, b =1 023 05(17) nm, c = 1 114 4(3) nm , α =86 778(8)°, β =76 153(5)°, γ =70 363(14)°, M =584 58, V = 1 037 3(4) nm 3 , Z =1 , D calc = 1 877 Mg/m 3 , T =293(2) K. The final R =0 061 8, w R =0 164 4. Each Nd 3+ ion is coordinated by five O atoms of four furancarboxylate groups, two O atoms of nitrate and two N atoms of 2,2′ bipyridine molecule, with a coordination number of 9. The four carboxylate groups coordinate in two modes:bridging and bridging chelating . The two Nd 3+ ions in the dimer are held together by four carboxylate groups of furancarboxylic acid.展开更多
A new cyano-bridged Gadolinium^(Ⅲ)-Iron^(Ⅲ)complex{[Gd(DMF)_(3)(DMSO)(H_(2)O)_(3)]2H_(2)0(DMF=N,N·-dimethylformamide;DMSO=dimethylsulfoxidel}was synthesized by the grinding reaction method,.It crysta-]llizes in...A new cyano-bridged Gadolinium^(Ⅲ)-Iron^(Ⅲ)complex{[Gd(DMF)_(3)(DMSO)(H_(2)O)_(3)]2H_(2)0(DMF=N,N·-dimethylformamide;DMSO=dimethylsulfoxidel}was synthesized by the grinding reaction method,.It crysta-]llizes in the triclinic.,space group P1 with ceIl parameters:a=O.90363(2)nm,b=1.25078(3)nm,c=1.41303(1)nm,穋m^(-3),Z=2,Mr=756.72,F(000)=760,Ⅲ)and the approxi-mately oriented octahedrally sixfold-coordinated Fe(Ⅲ)are linked by a cyano-bridge group to construct a dinuclear compound.The{[Gd(DMF)_(3)(DMSO)(H_(2)O)_(3)](Ⅲ)-Fe(Ⅲ)interaction is antiferromagnetic.CCDC:223430.展开更多
文摘A novel binucleus mixed-ligand[Cd2(phen)4(bmal)2]·3H2O (phen=phenanthroline; bmal=benzylmalonic acid radical) has been synthesized by the reaction of phen and bmal with cadmium(Ⅱ) salt. X-ray crystal structure analysis was carried out to determine the crystal structure of the title complex. The crystal of the title complex belongs to monoclinic system with space group P21/c, a=1.119 1(8) nm, b=2.480 5(17) nm, c=1.063 4(8) nm, β=142.042(12)°, Z=4, V=2.887(3) nm3, Dc=1.613 g·cm-3, R1=0.046 2, wR2=0.115 6, F(000)=1 424. One carboxyl of bmal is coordinated to Cd(1) with monodentate form, the others are coordinated to Cd(2) with bidentate form. The complexes form a 1-D chain structure bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in bmal, the 2-D network structure was formed by π-π interaction of neighbouring phen. CCDC: 257080.
文摘Binuclear mixed valent manganese complex [(Phen) 2Mn( μ O) 2Mn(Phen) 2] (ClO 4) 3·CH 2ClCOOH·2H 2O was synthesized by the reaction of [Mn 3O(O 2CCH 2Cl) 6(C 5H 5N) 2(H 2O)] ·CH 2ClCOO·H 2O with Phen and NaClO 4 in the CH 2ClCOOH CH 2ClCOONa buffer (pH=4.0). X ray diffraction result for the single crystal shows that the crystal is triclinic, space group P 1, with a =\{1.182 64(7)\} nm, b =1.449 32(8) nm, c =1.664 99(9) nm, α =104.585 0(10)°, β =97.123 0(10)°, \{ γ =\}106.921 0(10)°, V =2.581 6(3) nm 3, Z =2, D c=1.660 g·cm -3 , R =0.052 2. A peak at 640 nm in UV Vis spectrum is designed to the electronic transition of bridge legend O 2- to Mn(Ⅲ). Cyclic voltammogram shows that the complex in CH 3CN undergoes two quasi reversible one electron redox reactions at E 1/2 =1.25 V and E 1/2 =0.33 V, respectively.
文摘EPR spectra of three new quaternary gadolinium complexes(I： [Gd(C6H5COO)2(NO3)(bipy)]2,Ⅱ： [Gd(m- CH3C6H4COO)2(NO3)(phen)]2 andⅢ： [Gd(p- CH3C6H4COO)(NO3)(phen)]2) with mixed anion ligands in polycrystalline powders and solutions have been investigated at different temperatures and solvents.New behavior of EPR spectra of complexⅢ was first observed in polycrystalline powder at 77K and three types of EPR spectra for three complexes,symmetry resonance spectrum for the complexⅡ ,U spectrum for the complexⅢ ,and asymmetry resonance spectrum for the complex I.The relationship of EPR features between the crystal- field strength in the complexes and local symmetry around Gd(Ⅲ ) was discussed.The crystal- field parameters b20 and asymmetry parametersλ′ of the complexes I andⅢ were estimated.
文摘A new mixed-valence trinuclear oxo-centered manganese complex Mn3O(O2CCC l3)6(py)2(H2O) was prepared by the reaction of NnBu4MnO4 with Mn(OAc)2·4H2O, t richloroacetic acid and pyridine in absolute EtOH. The crystal structure was det ermined. The complex crystallizes in monoclinic, space group P21/c, unit cell pa rameters, a=14.951(1), b=20.791(2), c=17.882(1),á=?=90a=102.67(1)
文摘Complex [Tb(2-FC6H4COO)3·C10H8N2]2 was synthesized from TbCl3·nH2O,2-fluorobenzoic acid,and 2,2′-bipyridine(C10H8N2).The crystals are monoclinic with space group P21/n,and the crystal parameters are:a=1.219 1（4） nm,b=1.777 4（6） nm,c=1.371 5（4） nm,β=111.400（5）,（M=）732.41,V=2.767（15） nm3,Z=4,Dcalc=1.758 g/cm3,T=293（2） K.The final R=0.030 2,（wR=）0.054 7.The two Tb3+ ions are linked together by four 2-fluorobenzoate groups in a bridging mode to form a dimeric unit.Each Tb3+ ion is also chelated by one 2-fluorobenzoate group and one 2,2′-bipy ligand,making a coordination number of eight.There are four emission peaks in the luminescence spectrum at 490,545,584,and 618 nm,corresponding to the transitions of the Tb3+ ion:5D4→7F6,5D4→7F5,5D4→7F4,and(5D4→)7F3,respectively.
文摘The complex \ 2 Complex LI Xia *, JIN Qiong Hua (Department of Chemistry,Capital Normal University,Beijing 100037) Abstract The complex \[Nd(C 4 H 3 OCOO) 2 ·NO 3 ·C 10 H 8 N 2 \] 2 was synthesized from Nd(NO 3 ) 3 · n H 2 O, 2 furancarboxylic acid(C 4 H 3 OCOOH), and 2,2′ bipyridine(C 10 H 8 N 2 ). The unit cell is triclinic and of Pī symmetry. Unit cell parameters are:Pī, a =0 992 18(17) nm, b =1 023 05(17) nm, c = 1 114 4(3) nm , α =86 778(8)°, β =76 153(5)°, γ =70 363(14)°, M =584 58, V = 1 037 3(4) nm 3 , Z =1 , D calc = 1 877 Mg/m 3 , T =293(2) K. The final R =0 061 8, w R =0 164 4. Each Nd 3+ ion is coordinated by five O atoms of four furancarboxylate groups, two O atoms of nitrate and two N atoms of 2,2′ bipyridine molecule, with a coordination number of 9. The four carboxylate groups coordinate in two modes:bridging and bridging chelating . The two Nd 3+ ions in the dimer are held together by four carboxylate groups of furancarboxylic acid.
文摘A new cyano-bridged Gadolinium^(Ⅲ)-Iron^(Ⅲ)complex{[Gd(DMF)_(3)(DMSO)(H_(2)O)_(3)]2H_(2)0(DMF=N,N·-dimethylformamide;DMSO=dimethylsulfoxidel}was synthesized by the grinding reaction method,.It crysta-]llizes in the triclinic.,space group P1 with ceIl parameters:a=O.90363(2)nm,b=1.25078(3)nm,c=1.41303(1)nm,穋m^(-3),Z=2,Mr=756.72,F(000)=760,Ⅲ)and the approxi-mately oriented octahedrally sixfold-coordinated Fe(Ⅲ)are linked by a cyano-bridge group to construct a dinuclear compound.The{[Gd(DMF)_(3)(DMSO)(H_(2)O)_(3)](Ⅲ)-Fe(Ⅲ)interaction is antiferromagnetic.CCDC:223430.
