A novel coordination ploymer [Cd(HO-BDC)(phen)·H2O]n (where HO-BDC is 5-Hydroxyisophthalic acid and phen is 1,10-phenanthroline) has been synthesized and characterized by elemental analysis, IR spectra and single...A novel coordination ploymer [Cd(HO-BDC)(phen)·H2O]n (where HO-BDC is 5-Hydroxyisophthalic acid and phen is 1,10-phenanthroline) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2/c, with a=0.876 4(2) nm, b=1.233 0(3) nm, c=1.761 2(4) nm, β=109.152(9)°, V=1.797 8(7) nm3, Z=4, Mr=490.73, Dc=1.813 g·cm-3, F(000)=976, μ=1.258 mm-1, the final R=0.043 8 and wR=0.098 9 for 2 880 observed reflections with I>2σ(I). The structural analysis shows that the complex has a one-dimensional chain structure. CCDC: 609770.展开更多
A novel 1D coordination ploymer [{Cd(hmbdc)2(2,2′-bipy)2}·H2O]n (hmbdc=5-hydroxybenzene-1,3-dioic acid) was synthesized by the hydrothermal reaction of hmbdc, CdSO4·8H2O and 2,2′-bipy. The structure was ch...A novel 1D coordination ploymer [{Cd(hmbdc)2(2,2′-bipy)2}·H2O]n (hmbdc=5-hydroxybenzene-1,3-dioic acid) was synthesized by the hydrothermal reaction of hmbdc, CdSO4·8H2O and 2,2′-bipy. The structure was characterized by elemental analysis, IR and single crystal X-ray diffraction. The title coordination ploymer crystallized in monoclinic with space group P2/c, a=0.857 96(19) nm, b=1.113 8(3) nm, c=1.858 8(4) nm, β=104.259(9)°. The coordination polymer has an infinite chain structure and its luminescent property has also been studied. CCDC: 294519.展开更多
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
This paper reports the features and regularities of the infrared spectra for two kinds of complexes containing R 2dtc ligand. The cubane like clusters containing R 2dtc ligand possess weak and wide peaks at 400—500 c...This paper reports the features and regularities of the infrared spectra for two kinds of complexes containing R 2dtc ligand. The cubane like clusters containing R 2dtc ligand possess weak and wide peaks at 400—500 cm -1 assigned to M μ 3S vibration,while the peaks at 330—380 cm -1 and 1 470—1 510 cm -1 can be assigned to M S dtc and C—N vibrations,respectively.The ν ( C—N ) and ν (C=S) vibrations for Me 2dtc cubane cluster exhibit blue shift and red shift,respectively,when compared with those of other R 2dtc ones.This would be attributed to the strong super conjugation of the methly group. The M μ 3S vibrations for both types of complexes [V 2Cu 2S 4(R 2dtc) 2(PhS) 2] 2- and [VCu 4S 4(R 2dtc) n(PhS) 4-n ] 3- ( n =0,1,2) occur at 480 and 465 cm -1 ,respectively.This small difference becomes a useful indication to distinguish the two types of clusters. Cluster complexes containing (R 2dtc) 2V 2O 2(μ S) 2 structural unit show the V=O vibration in the range of 844—970 cm -1 .It is noted that (Et 4N)[V 3S 2O 3(Et 2dtc) 3] contains two sets of the V=O bonds corresponding to two sets of V=O vibrations at 970 and 844 cm -1 .An additional coordination of the V=O bond to another metal atom obviously weakens the V=O bond to give rise to the red shift of the infrared frequency.Similar red shifts were also observed for other complexes and were discussed.展开更多
文摘A novel coordination ploymer [Cd(HO-BDC)(phen)·H2O]n (where HO-BDC is 5-Hydroxyisophthalic acid and phen is 1,10-phenanthroline) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2/c, with a=0.876 4(2) nm, b=1.233 0(3) nm, c=1.761 2(4) nm, β=109.152(9)°, V=1.797 8(7) nm3, Z=4, Mr=490.73, Dc=1.813 g·cm-3, F(000)=976, μ=1.258 mm-1, the final R=0.043 8 and wR=0.098 9 for 2 880 observed reflections with I>2σ(I). The structural analysis shows that the complex has a one-dimensional chain structure. CCDC: 609770.
基金the Natural Science Foundation of China(21003020)the National Science Foundation for Fostering Talents in Basic Research of the National Natural Science Foundation of China(J1103303)+1 种基金the Natural Science Fund of Fujian Province(2013J01041)the Foundation of State Key Laboratory of Structural Chemistry(20130012)
文摘A novel 1D coordination ploymer [{Cd(hmbdc)2(2,2′-bipy)2}·H2O]n (hmbdc=5-hydroxybenzene-1,3-dioic acid) was synthesized by the hydrothermal reaction of hmbdc, CdSO4·8H2O and 2,2′-bipy. The structure was characterized by elemental analysis, IR and single crystal X-ray diffraction. The title coordination ploymer crystallized in monoclinic with space group P2/c, a=0.857 96(19) nm, b=1.113 8(3) nm, c=1.858 8(4) nm, β=104.259(9)°. The coordination polymer has an infinite chain structure and its luminescent property has also been studied. CCDC: 294519.
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.
文摘This paper reports the features and regularities of the infrared spectra for two kinds of complexes containing R 2dtc ligand. The cubane like clusters containing R 2dtc ligand possess weak and wide peaks at 400—500 cm -1 assigned to M μ 3S vibration,while the peaks at 330—380 cm -1 and 1 470—1 510 cm -1 can be assigned to M S dtc and C—N vibrations,respectively.The ν ( C—N ) and ν (C=S) vibrations for Me 2dtc cubane cluster exhibit blue shift and red shift,respectively,when compared with those of other R 2dtc ones.This would be attributed to the strong super conjugation of the methly group. The M μ 3S vibrations for both types of complexes [V 2Cu 2S 4(R 2dtc) 2(PhS) 2] 2- and [VCu 4S 4(R 2dtc) n(PhS) 4-n ] 3- ( n =0,1,2) occur at 480 and 465 cm -1 ,respectively.This small difference becomes a useful indication to distinguish the two types of clusters. Cluster complexes containing (R 2dtc) 2V 2O 2(μ S) 2 structural unit show the V=O vibration in the range of 844—970 cm -1 .It is noted that (Et 4N)[V 3S 2O 3(Et 2dtc) 3] contains two sets of the V=O bonds corresponding to two sets of V=O vibrations at 970 and 844 cm -1 .An additional coordination of the V=O bond to another metal atom obviously weakens the V=O bond to give rise to the red shift of the infrared frequency.Similar red shifts were also observed for other complexes and were discussed.
