A dinuclear complex [DyFe(CN)6(DMF)4(H2O)3]·1.25H2O (DMF=N, N dimethylformamide) 1 based on the cyanide as linkage was prepared and structurally characterized by X ray single crystal structure analysis. The Dy?io...A dinuclear complex [DyFe(CN)6(DMF)4(H2O)3]·1.25H2O (DMF=N, N dimethylformamide) 1 based on the cyanide as linkage was prepared and structurally characterized by X ray single crystal structure analysis. The Dy?ion is eight coordinations in a square antiprism arrangement and the Fe?ion is six coordinations oriented octahedrally. The neutral units [DyFe(CN)6(DMF)4(H2O)3] are held together by hydrogen bonds formed by lattice water molecules, coordinated water molecules and nitrogen atoms of cyanide coming from other distinct complex units to afford a three dimensional framework. CCDC: 192314.展开更多
GThe title compound was synthesized by reaction of Cu(ClO4)2, picolinic acid and carbamide in C2H5OH/CH3CN solution, and characterized by single crystal X ray diffraction. It crystallizes in the orthorhombic system, s...GThe title compound was synthesized by reaction of Cu(ClO4)2, picolinic acid and carbamide in C2H5OH/CH3CN solution, and characterized by single crystal X ray diffraction. It crystallizes in the orthorhombic system, space group Pbcawith a=14.0481(8), b=9.0130(5), c=18.626(1)?, V=2358.3(2)?3, Z=4, Dx=1.771g·cm-3, μ=1.235mm-1 and F(000)=1276. The final R factor is 0.0440 for 1434 observed reflections. The X ray analysis revealed that the copper?atom iscoordinated by two picolinic ligands in the equatorial plane, while the two oxygen atoms of perchlorate occupy the axial positions of octahedron with lengthened Cu O distances, resulting in a 4+2 elongated octahedral environment. In the compound, there also exist two protonated carbamide cations for charge balance. CCDC: 195354.展开更多
The two complexes [Cu(C5H2N2O4)(H2O)3]·2H2O (1) and [Ni(C5H2N2O4)(H2O)4]·H2O (2) were synthesized by self assembly reactions of Cu(NO3)2·3H2O or Ni(CH3COO)2·4H2O with orotic acid (2,6 dioxo 1,2,3,6...The two complexes [Cu(C5H2N2O4)(H2O)3]·2H2O (1) and [Ni(C5H2N2O4)(H2O)4]·H2O (2) were synthesized by self assembly reactions of Cu(NO3)2·3H2O or Ni(CH3COO)2·4H2O with orotic acid (2,6 dioxo 1,2,3,6 tetrahydro 4 pyrimidinecarboxylic acid), respectively. Their crystal structures were determined by single crystal X ray diffraction analyses. Crystallographic data for complex 1: C5H8N2CuO7·2H2O, Mr=307.7, monoclinic P21/n, a=0.57710(1)nm, b=1.76863(6)nm, c=1.09955(4)nm, β=98.600(2)°, V=1.109.63(6)nm3, Z=4 , Dc=1.842g·cm-3, μ(MoKα)=2.010mm-1, F(000)=628, R=0.0436, wR=0.1015, And for complex 2: C5H10N2NiO8·H2O, Mr=302.88, orthorhombic Pbcn, a=2.0763(1)nm, b=1.69355(9)nm, c=0.73478(4)nm, V=2.5837(2)nm3, Z=8, Dc=1.557g·cm-3, μ(MoKα)=1.538 mm-1, F(000)=1248, R=0.0545, wR=0.1305. The X ray analyses revealed that the Cu? and Ni? atoms are both coordinated by carboxylic O atom and contiguous N atom of the pyrimidine ring. In complex 1 the Cu? atom has a slightly distorted square pyramid coordination environment with additional three water molecules, while in complex 2 the Ni? atom adopts a slightly distorted octahedral geometry with additional four water molecules. The three dimensional frameworks of the two complexes are formed by intermolecular hydrogen bonding interactions. CCDC: 1, 204881; 2, 204882.展开更多
A new lanthanide complex [Sm（C2O4）（H2O）5]nCln·2nH2O has been obtained by hydrothermal synthetic method. The crystal belongs to monoclinic, space group P21/n, with a = 7.5438（6）, b = 14.3201（11）, c = 10.8...A new lanthanide complex [Sm（C2O4）（H2O）5]nCln·2nH2O has been obtained by hydrothermal synthetic method. The crystal belongs to monoclinic, space group P21/n, with a = 7.5438（6）, b = 14.3201（11）, c = 10.8608（9）A, β = 94.565（4）°, V = 1169.55（16）A^3, C2H14ClO11Sm, Mr = 399.93, Z = 4, Dc = 2.271 g/cm^3, μ = 5.290 cm^-1, F（000） = 772, the final R = 0.0271 and wR = 0.0632 for 1880 observed reflections with I 〉 2σ（I）. X-ray crystal analysis reveals that each Sm（III） atom is nine-coordinated by four oxygen atoms from two oxalate ligands and five coordinated water molecules in a distorted tricapped trigonal prism. The chain-like structure of lanthanide oxalate is reported for the first time. The fluorescent property and magnetic behavior of the title compound were investigated. The θ of –14.3（2）° and J of –0.26 cm^-1 indicate antiferromagnetic interaction in the molecule.展开更多
The zinc 3-hydroxy-2-mercaptopyridine complex was prepared by self-assemby reaction of Zn(NO3)2 and 3-hydroxy-2-mercaptopyridine (hmp). Single-crystal X-ray diffraction analysis indicates that it crystallizes in a tet...The zinc 3-hydroxy-2-mercaptopyridine complex was prepared by self-assemby reaction of Zn(NO3)2 and 3-hydroxy-2-mercaptopyridine (hmp). Single-crystal X-ray diffraction analysis indicates that it crystallizes in a tetragonal system, space group (No. 122) with a = 13.4562(6), c = 13.6860(8) , V = 2478.1(2) 3, Z = 8, Mr = 317.67, Dc = 1.703 g/cm3, m(Mo-Ka) = 2.308 mm-1 and F(000) = 1280. R = 0.0289 and wR = 0.0676 for 1040 observed reflections (I > 2s(I)). The crystal structure consists of a neutral molecule with a distorted tetrahedral cis-ZnS2O2 core, in which the mononuclear Zn2+ ion is coordinated by two O and two S atoms from two hmp ligands with the average bond distances of 2.301(1) ?for ZnS and 1.986(3) ?for ZnO. The 1H . NMR and IR spectra of the compound are discussed.展开更多
文摘A dinuclear complex [DyFe(CN)6(DMF)4(H2O)3]·1.25H2O (DMF=N, N dimethylformamide) 1 based on the cyanide as linkage was prepared and structurally characterized by X ray single crystal structure analysis. The Dy?ion is eight coordinations in a square antiprism arrangement and the Fe?ion is six coordinations oriented octahedrally. The neutral units [DyFe(CN)6(DMF)4(H2O)3] are held together by hydrogen bonds formed by lattice water molecules, coordinated water molecules and nitrogen atoms of cyanide coming from other distinct complex units to afford a three dimensional framework. CCDC: 192314.
文摘GThe title compound was synthesized by reaction of Cu(ClO4)2, picolinic acid and carbamide in C2H5OH/CH3CN solution, and characterized by single crystal X ray diffraction. It crystallizes in the orthorhombic system, space group Pbcawith a=14.0481(8), b=9.0130(5), c=18.626(1)?, V=2358.3(2)?3, Z=4, Dx=1.771g·cm-3, μ=1.235mm-1 and F(000)=1276. The final R factor is 0.0440 for 1434 observed reflections. The X ray analysis revealed that the copper?atom iscoordinated by two picolinic ligands in the equatorial plane, while the two oxygen atoms of perchlorate occupy the axial positions of octahedron with lengthened Cu O distances, resulting in a 4+2 elongated octahedral environment. In the compound, there also exist two protonated carbamide cations for charge balance. CCDC: 195354.
文摘The two complexes [Cu(C5H2N2O4)(H2O)3]·2H2O (1) and [Ni(C5H2N2O4)(H2O)4]·H2O (2) were synthesized by self assembly reactions of Cu(NO3)2·3H2O or Ni(CH3COO)2·4H2O with orotic acid (2,6 dioxo 1,2,3,6 tetrahydro 4 pyrimidinecarboxylic acid), respectively. Their crystal structures were determined by single crystal X ray diffraction analyses. Crystallographic data for complex 1: C5H8N2CuO7·2H2O, Mr=307.7, monoclinic P21/n, a=0.57710(1)nm, b=1.76863(6)nm, c=1.09955(4)nm, β=98.600(2)°, V=1.109.63(6)nm3, Z=4 , Dc=1.842g·cm-3, μ(MoKα)=2.010mm-1, F(000)=628, R=0.0436, wR=0.1015, And for complex 2: C5H10N2NiO8·H2O, Mr=302.88, orthorhombic Pbcn, a=2.0763(1)nm, b=1.69355(9)nm, c=0.73478(4)nm, V=2.5837(2)nm3, Z=8, Dc=1.557g·cm-3, μ(MoKα)=1.538 mm-1, F(000)=1248, R=0.0545, wR=0.1305. The X ray analyses revealed that the Cu? and Ni? atoms are both coordinated by carboxylic O atom and contiguous N atom of the pyrimidine ring. In complex 1 the Cu? atom has a slightly distorted square pyramid coordination environment with additional three water molecules, while in complex 2 the Ni? atom adopts a slightly distorted octahedral geometry with additional four water molecules. The three dimensional frameworks of the two complexes are formed by intermolecular hydrogen bonding interactions. CCDC: 1, 204881; 2, 204882.
基金financially supported by the National Natural Science Foundation of China (Grants No. 91545201,21601185)the Key Research Program of Frontier Sciences,CAS (Grants No.XDB20010000,QYZDBSSW-SLH020)+1 种基金the Youth Innovation Promotion Association of CASthe Natural Science Foundation of Fujian Province (Grants No.2017J01033,2018J01028)~~
基金This work was supported by the NNSFC (20131020)the NSF for Distinguished Yong Scientist of China (20425104)the NSF of Fujian Province (E0510028)
文摘A new lanthanide complex [Sm（C2O4）（H2O）5]nCln·2nH2O has been obtained by hydrothermal synthetic method. The crystal belongs to monoclinic, space group P21/n, with a = 7.5438（6）, b = 14.3201（11）, c = 10.8608（9）A, β = 94.565（4）°, V = 1169.55（16）A^3, C2H14ClO11Sm, Mr = 399.93, Z = 4, Dc = 2.271 g/cm^3, μ = 5.290 cm^-1, F（000） = 772, the final R = 0.0271 and wR = 0.0632 for 1880 observed reflections with I 〉 2σ（I）. X-ray crystal analysis reveals that each Sm（III） atom is nine-coordinated by four oxygen atoms from two oxalate ligands and five coordinated water molecules in a distorted tricapped trigonal prism. The chain-like structure of lanthanide oxalate is reported for the first time. The fluorescent property and magnetic behavior of the title compound were investigated. The θ of –14.3（2）° and J of –0.26 cm^-1 indicate antiferromagnetic interaction in the molecule.
基金the Innovative Project (No. IP01007)the Introduction of Overseas Elitists Program (No. IB990168) of the Chinese Academy of Sciences
文摘The zinc 3-hydroxy-2-mercaptopyridine complex was prepared by self-assemby reaction of Zn(NO3)2 and 3-hydroxy-2-mercaptopyridine (hmp). Single-crystal X-ray diffraction analysis indicates that it crystallizes in a tetragonal system, space group (No. 122) with a = 13.4562(6), c = 13.6860(8) , V = 2478.1(2) 3, Z = 8, Mr = 317.67, Dc = 1.703 g/cm3, m(Mo-Ka) = 2.308 mm-1 and F(000) = 1280. R = 0.0289 and wR = 0.0676 for 1040 observed reflections (I > 2s(I)). The crystal structure consists of a neutral molecule with a distorted tetrahedral cis-ZnS2O2 core, in which the mononuclear Zn2+ ion is coordinated by two O and two S atoms from two hmp ligands with the average bond distances of 2.301(1) ?for ZnS and 1.986(3) ?for ZnO. The 1H . NMR and IR spectra of the compound are discussed.
