Samnium(Ⅲ)-bismuth(Ⅲ) heterobimetallic complexes, SmBi(edta)(NO3)2·7H2O (1) and SmBi(dtpa)(NO3)·3.5H2O(2) (edta=ethylenediaminetetraacetate, dtpa=diethylenetriaminepentaacetate), were syn...Samnium(Ⅲ)-bismuth(Ⅲ) heterobimetallic complexes, SmBi(edta)(NO3)2·7H2O (1) and SmBi(dtpa)(NO3)·3.5H2O(2) (edta=ethylenediaminetetraacetate, dtpa=diethylenetriaminepentaacetate), were synthesized and characterized by means of X-ray single crystal diffraction, X-ray powder diffraction, elemental analysis, ICP, FT-IR spectra and thermal analysis. The structure analysis revealed that 1 is in crystalline and 2 is in non-crystal state. Complex 1 crystallizes in monoclinic, space group P2(1)/n with a= 1.2622(2) nm, b=0.81157(15) nm, c=2.3634(5) nm, β= 105.340(2)°, V=2.3347(8) nm3, Z=4, Dc=2.563 gocm^-3,μ=10.125 mm-1. Bridging edta4 anions between Bi(Ⅲ) atoms and Sm(Ⅲ) atoms result into infinite 3D network structure. Thermal decomposition of the two complexes proceeds in similar stages, i.e., dehydration, pyrolysis of ligand, and decomposition of salt, and the final residue is oxide. In addition, the spectral properties have been studied through FL spectra and UV-Vis DRS. The two complexes exhibit one broad band Bi 6s6p-6s2 emission under UV excitation and the characteristic Sm3+ ion 4G5/2→6Hj/2 (J= 5, 7, 9, 11) transitions under visible light excitation, respectively.展开更多
The title complex K [Gd~Ⅲ(edta)(H_2O)_3]·5H_2O was synthesized, where edta denotes ethylenediamine- tetraacetic acid. The crystal and molecular structure of the complex were determined by single-crystal X-ray st...The title complex K [Gd~Ⅲ(edta)(H_2O)_3]·5H_2O was synthesized, where edta denotes ethylenediamine- tetraacetic acid. The crystal and molecular structure of the complex were determined by single-crystal X-ray structure analysis. The crystal belongs to an orthorhombic crystal system and an Fdd2 space group. The complex anion [Gd~Ⅲ(edta)(H_2O)_3] has a pseudo-monocapped square antiprismatic nine-coordinate structure in which six coordinate atoms (two N and four O) are from an edta ligand and three water molecules coordinate to Gd~Ⅲ ion directly. It can be predicted that Gd~Ⅲ ion can also form a nine-coordinate complex with ttha (triethylenetetraminehexaacetic acid) li- gand, so the GdⅢ complex anion [Gd~?é¨(r)(Httha)]~£¨2-£(c) can supply a free non-coordinate carboxyl group (-C-CH_2COOH) used for molecular embellishment in some biological molecules to form a contrast agent of Magnetic Resonance Imagine (MRI) with targeting function.展开更多
A novel binuclear Eu(Ⅲ) complex [Eu2(dpa dioxide)2(NO3)4(bpdioxide)-(EtOH)] (dpa dioxide = di-2-pyridylamine N,N'-dioxide, bpdioxide = 2,2'-bipyridine N,N'-dioxide) has been synthesized and it exhibits...A novel binuclear Eu(Ⅲ) complex [Eu2(dpa dioxide)2(NO3)4(bpdioxide)-(EtOH)] (dpa dioxide = di-2-pyridylamine N,N'-dioxide, bpdioxide = 2,2'-bipyridine N,N'-dioxide) has been synthesized and it exhibits strong and sharp fluorescent emission at 614 nm under UV radiation of 245 nm at room temperature. X-ray structural determination indicates two independent Eu(Ⅲ) ions in the structure with different EuO8N and EuOgN environments. The compound crystallizes in the triclinic system, space group P1, with a = 10.8089(7), b = 11.4670(8), c = 17.1440(12) A, α = 92.834(2), β = 93.854(3), γ = 95.433(2)°, Z = 2, Dc = 1.876 g/cm3, V= 2107.3(2) A3, F(000) = 1168.0, the final R = 0.032 and wR = 0.086 for 6331 observed reflections with I 〉 2σ(I).展开更多
The title complex was synthesised and its molecular and crystal structures were determined by single crystal X ray reflection structure analysis. The crystal data are as follows: K[In Ⅲ(EDTA)(H 2O)]·2H 2O (...The title complex was synthesised and its molecular and crystal structures were determined by single crystal X ray reflection structure analysis. The crystal data are as follows: K[In Ⅲ(EDTA)(H 2O)]·2H 2O (EDTA=ethylene diamine N, N, N′, N′ tetraacetate), Monoclinic, C c space group, a=0.9096(2) nm,b=1.1996(2) nm, c =1.5144(3) nm, β =99.40(3)°, V =1.6302(6) 3, Z =3, D c=1.498 g·cm -3 , μ =1.325 mm -1 , F (000)=726, R =0.0320 and R W=0.0903 for 2315 observed independent reflections. The complex anion [In Ⅲ(EDTA)(H 2O)] - has a seven coordinate pseudo pentagonal bipyramidal (PB D 5h ) structure, in which the EDTA serves as a hexadentate ligand with two N atoms and four O atoms and one water molecule (H 2O) directly coordinated to the central metal ion In Ⅲ as a seventh ligand. 〓〓展开更多
A new Bismuth(Ⅲ)-Lanthanum(Ⅲ) heterobimetallic polymer complex,{[(H2O)5La(μ4-edta)Bi(NO3)2]·3H2O}n(edta=diaminetetraacecarboxylate),has been hydrothermally synthesized and characterized by elemental analysis,F...A new Bismuth(Ⅲ)-Lanthanum(Ⅲ) heterobimetallic polymer complex,{[(H2O)5La(μ4-edta)Bi(NO3)2]·3H2O}n(edta=diaminetetraacecarboxylate),has been hydrothermally synthesized and characterized by elemental analysis,FT-IR,and X-ray diffraction single crystal structure analysis.It crystallizes in the monoclinic system,with space group P2(1)/n,a=1.27395(5)nm,b=0.82608(4) nm,c=2.38819(11) nm,β=104.9000(10)°,V=2.42879(19) nm3,Z=4,Dc=2.438 g·cm-3,μ=9.077mm-1,F(000)=1678,R1=0.0343,wR2=0.0906.In this complex,Bi atom is coordinated by four carboxyl O atoms from a single edta4-anion.La atom is bonded to four O atoms from four bridging carboxyl O atoms belonging to four different edta4-anions and five O atoms from five H2O molecules.Bi atoms and La atoms are linked by bridged edta4-anions,resulting into a novel infinite 3D network structure.TG-DSC and IR indicate that thermal decomposition proceeds in several stages,dehydration,pyrolysis of ligand,and finally decomposition of salt,and the residue is composite oxide based on δ-Bi2O3 at the temperature of 600℃.展开更多
文摘Samnium(Ⅲ)-bismuth(Ⅲ) heterobimetallic complexes, SmBi(edta)(NO3)2·7H2O (1) and SmBi(dtpa)(NO3)·3.5H2O(2) (edta=ethylenediaminetetraacetate, dtpa=diethylenetriaminepentaacetate), were synthesized and characterized by means of X-ray single crystal diffraction, X-ray powder diffraction, elemental analysis, ICP, FT-IR spectra and thermal analysis. The structure analysis revealed that 1 is in crystalline and 2 is in non-crystal state. Complex 1 crystallizes in monoclinic, space group P2(1)/n with a= 1.2622(2) nm, b=0.81157(15) nm, c=2.3634(5) nm, β= 105.340(2)°, V=2.3347(8) nm3, Z=4, Dc=2.563 gocm^-3,μ=10.125 mm-1. Bridging edta4 anions between Bi(Ⅲ) atoms and Sm(Ⅲ) atoms result into infinite 3D network structure. Thermal decomposition of the two complexes proceeds in similar stages, i.e., dehydration, pyrolysis of ligand, and decomposition of salt, and the final residue is oxide. In addition, the spectral properties have been studied through FL spectra and UV-Vis DRS. The two complexes exhibit one broad band Bi 6s6p-6s2 emission under UV excitation and the characteristic Sm3+ ion 4G5/2→6Hj/2 (J= 5, 7, 9, 11) transitions under visible light excitation, respectively.
文摘The title complex K [Gd~Ⅲ(edta)(H_2O)_3]·5H_2O was synthesized, where edta denotes ethylenediamine- tetraacetic acid. The crystal and molecular structure of the complex were determined by single-crystal X-ray structure analysis. The crystal belongs to an orthorhombic crystal system and an Fdd2 space group. The complex anion [Gd~Ⅲ(edta)(H_2O)_3] has a pseudo-monocapped square antiprismatic nine-coordinate structure in which six coordinate atoms (two N and four O) are from an edta ligand and three water molecules coordinate to Gd~Ⅲ ion directly. It can be predicted that Gd~Ⅲ ion can also form a nine-coordinate complex with ttha (triethylenetetraminehexaacetic acid) li- gand, so the GdⅢ complex anion [Gd~?é¨(r)(Httha)]~£¨2-£(c) can supply a free non-coordinate carboxyl group (-C-CH_2COOH) used for molecular embellishment in some biological molecules to form a contrast agent of Magnetic Resonance Imagine (MRI) with targeting function.
基金supported by the Natural Science Foundation of Jiangxi Province (No.0320026 and 0520036)the Natural Science Foundation of Jinggangshan University (No.JZ0815)
文摘A novel binuclear Eu(Ⅲ) complex [Eu2(dpa dioxide)2(NO3)4(bpdioxide)-(EtOH)] (dpa dioxide = di-2-pyridylamine N,N'-dioxide, bpdioxide = 2,2'-bipyridine N,N'-dioxide) has been synthesized and it exhibits strong and sharp fluorescent emission at 614 nm under UV radiation of 245 nm at room temperature. X-ray structural determination indicates two independent Eu(Ⅲ) ions in the structure with different EuO8N and EuOgN environments. The compound crystallizes in the triclinic system, space group P1, with a = 10.8089(7), b = 11.4670(8), c = 17.1440(12) A, α = 92.834(2), β = 93.854(3), γ = 95.433(2)°, Z = 2, Dc = 1.876 g/cm3, V= 2107.3(2) A3, F(000) = 1168.0, the final R = 0.032 and wR = 0.086 for 6331 observed reflections with I 〉 2σ(I).
文摘The title complex was synthesised and its molecular and crystal structures were determined by single crystal X ray reflection structure analysis. The crystal data are as follows: K[In Ⅲ(EDTA)(H 2O)]·2H 2O (EDTA=ethylene diamine N, N, N′, N′ tetraacetate), Monoclinic, C c space group, a=0.9096(2) nm,b=1.1996(2) nm, c =1.5144(3) nm, β =99.40(3)°, V =1.6302(6) 3, Z =3, D c=1.498 g·cm -3 , μ =1.325 mm -1 , F (000)=726, R =0.0320 and R W=0.0903 for 2315 observed independent reflections. The complex anion [In Ⅲ(EDTA)(H 2O)] - has a seven coordinate pseudo pentagonal bipyramidal (PB D 5h ) structure, in which the EDTA serves as a hexadentate ligand with two N atoms and four O atoms and one water molecule (H 2O) directly coordinated to the central metal ion In Ⅲ as a seventh ligand. 〓〓
文摘A new Bismuth(Ⅲ)-Lanthanum(Ⅲ) heterobimetallic polymer complex,{[(H2O)5La(μ4-edta)Bi(NO3)2]·3H2O}n(edta=diaminetetraacecarboxylate),has been hydrothermally synthesized and characterized by elemental analysis,FT-IR,and X-ray diffraction single crystal structure analysis.It crystallizes in the monoclinic system,with space group P2(1)/n,a=1.27395(5)nm,b=0.82608(4) nm,c=2.38819(11) nm,β=104.9000(10)°,V=2.42879(19) nm3,Z=4,Dc=2.438 g·cm-3,μ=9.077mm-1,F(000)=1678,R1=0.0343,wR2=0.0906.In this complex,Bi atom is coordinated by four carboxyl O atoms from a single edta4-anion.La atom is bonded to four O atoms from four bridging carboxyl O atoms belonging to four different edta4-anions and five O atoms from five H2O molecules.Bi atoms and La atoms are linked by bridged edta4-anions,resulting into a novel infinite 3D network structure.TG-DSC and IR indicate that thermal decomposition proceeds in several stages,dehydration,pyrolysis of ligand,and finally decomposition of salt,and the residue is composite oxide based on δ-Bi2O3 at the temperature of 600℃.