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1.
A Keggin-type tungstosilicate compound [CoII(2,2'-bipy)2(H2O)]2[SiWVI12O40]·2H2O1 (bipy = bipyridine) was prepared by a hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 (C4H40Co2N8O44SiW12) crystallizes in the triclinic system, space group P1 with a = 10.4979(6), b = 13.3946(7), c = 13.5756(8) (A°), α= 70.0769(18), β= 68.910(3), y = 74.186(4)°,V =1649.84(16) (A°)3, M, = 3688.95, Z =1, Dc= 3.713 mg.m-3,μ= 21.432 mm-1, F(000) = 1644, S =1.058, the final R = 0.0511 and wR = 0.1023 for 6523 observed reflections (I> 2σ(I)). Compound 1 consists of two coordinated cation fragments [CoII(2,2'-bipy)2(H2O)]2+, one normal Keggin polyanion unit [SiWVI12O40]4- and two lattice water molecules. To be noted, each polyanion unit is linked to two cation fragments by its two surface terminal oxygen atoms and two cobalt atoms of two cation fragments forming an organic-inorganic hybrid unit in 1. Furthermore, the compound shows strong photo-luminescence property in the solid state at room temperature.  相似文献   

2.
A novel compound [H-IDP]4[PMo12O40]·8H2O 1 based on Keggin-type phosphor- molybdate has been synthesized by hydrothermal method and characterized by IR spectroscopy, elemental analyses and single-crystal X-ray diffraction. The composite crystallizes in the mono- clinic system, space group C2/m with a = 13.937(5), b = 27.033(5), c = 10.857(5) A, β = 122.489(5)°, V = 3450(2)A^3, Mr = 2611.11, Z = 2, Dc = 2.498 g/cm^3, F(000) = 2486,μ = 2.243 mm^-1, the final R = 0.0568 and wR = 0.1216 for 2707 observed reflections with I 〉 2σ(I). X-ray structural study shows that 1 consists of a [PMo12O40]^4- polyanion, four protonated IDP cations and eight H2O molecules. In the structure of 1, a 3D network forms by hydrogen bond of [PMo12O40]^4- polyanion, HIDP^+ cation and H2O molecules. Upon excitation wavelength of 280 nrn in hydroxylic solvents at room temperature, 1 shows fluorescence property.  相似文献   

3.
A novel composite, [C16H36N][Cu(2,2-bipy)3][PW12O40]·CH3CN·H2O based on Keggin-type phosphotungstate, has been synthesized in acetonitrile at moderate temperature and then characterized by IR and single-crystal X-ray structural analysis. The crystal is of monoclinic system, space group P21/n with a = 20.489(4), b = 17.249(3), c = 23.723(4)A, β = 95.114(2)^o, V = 8350(3)A3, Mr = 3710.79, Z = 4, Dc = 2.952 g/cm^3, F(000) = 6676, μ = 16.808 mm^-1, the final R = 0.0551 and wR = 0.1269 for 9460 observed reflections with I 〉 20(I). Interestingly, it is found that the structure unit contains two different cations of [C16H36N]^+ and [Cu(2,2-bipy)3]^2+.  相似文献   

4.
The reaction of Co(OAc)2·4H2O with the Schiff base H2L in a methanol solution affords the red crystals of { [Co^ⅢL2]·[Co^Ⅱ(H2O)6]0.5·2.25H2O}4 1 (H2L = N-(2-hydroxyphenyl) salicylidenimine). The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n, C104Hi14Co6NaO37, Mr = 2421.61, a = 10.625(3), b = 16.335(4), c = 15.265(4)A^°, β = 102.990(4)°, V= 2581.6(11)A^°^3, Z = 1, Dc= 1.558 g/cm^3,μ = 1.034 mm^-1, F(000) = 1252, R = 0.0414 and wR = 0.1167 for 5889 reflections. The Co(HI) atom is six-coordinated by two nitrogen atoms and four oxygen atoms of two tridentate L ligands. The abundant hydrogen bonding interactions extend the complex into a one-dimensional supra- molecular framework. The uncoordinated water molecules act as space-fillers and consolidate the whole architecture through the hydrogen bonding interactions.  相似文献   

5.
The title compound, [Ni(tssb)(2,2-bipy)2].5(H2O) 1 (tssbH2 =2-[(E)-(2-oxido- phenyl)methyleneamino]ethanesulfonato, 2,2-bipy = 2,2'-bipyridinyl), belongs to orthorhombic, space group Pbcn with a = 20.3983(18), b = 17.6929(15), c = 17.0897(15) nm, V= 6167.8(9) nm^3, Mr= 688.38, Z = 8, De = 1.481 g.cm^-3, F(000) = 2880,μ = 0.758 mm-1 and S =1.099. Each NiIr atom is six-coordinated by one N and one O atoms from one tssb^2- anion and four N atoms from two 2,2-bipy ligands to give a distorted octahedral geometry. Noticeably, there exists a rare octa-mem- bered water ring which presents a 1D chain by sulfonic group.  相似文献   

6.
A new copper(II)-2,2'-biimidazole metal-organic POMs-supported compound [Cu(H2biim)2]{[Cu(H2biim)212[H10W12O44]}'8H2O (H2biim = 2,2'-biimidazole) has been success- fully synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and TG. The crystal adopts space group Pi with a = 11.800(2), b = 13.437(3), c = 13.685(3) A, V = 1922.5(7) A3, D,. = 3.507 g/cm3, C36H62Cu3N24W12O52, M,. = 4059.92, F(000) = 1837,μ = 18.796 mm-1, Z = 1, R = 0.0579 and wR = 0.1465 for 8734 observed reflections (I 〉 2σ(I)). X-ray crystallography analysis exhibits that the title compound consists of one [H10W12044]6- polyanion and three [Cu(H2biim)2] units. And significant π-π stacking interactions and intermolecular O-H-,.O or N-H.'-O hydrogen-bonding interactions lead to a three-dimensional supramolecular framework. Thermal stability and magnetic property of the complex have also been investigated.  相似文献   

7.
A new one-dimensional Mn(Ⅱ) complex, [MnL2(bipy)(H2O)2]n 1, has been obtained by the reaction of MnCl2·4H2O, 2,2'-bipyridine (bipy) and 1-(4-phenoxyacetate)-5-thioacetatetetrazole (H2L). The crystal crystallizes in the triclinic system, space group Pi with a = 7.6088(2), b = 12.2795(2), c = 13.6617(3)A, α = 75.416(2), β =79.264(2), γ = 74.271(2)°, V = 1179.48(4) A3, Z = 2, Mr = 555.43, F(000) = 570, Dc = 1.564 g/cm^3, μ = 0.704 mm^-1, the final R = 0.0454 and wR = 0.0849 for 3127 observed reflections (Ⅰ〉 2σ(Ⅰ)). The Mn(Ⅱ) is six-coordinated by two water molecules, two N atoms from bipy and two carboxylate O atoms from two L^2- to form a distorted octahedral geometry. Each L^2- ligand serves as a bridging ligand to link two Mn(Ⅱ) atoms, leading to a single-strand zigzag coordination polymer. Hydrogen-bonding interactions between adjacent chains as well as π-π stacking interactions extend the complex into a three-dimensional supramolecular architecture. Moreover, the title compound emits strong red fluorescent light (λem(max) = 610 nm) in EtOH solution.  相似文献   

8.
Three new inorganic-organic composite polyoxotungstates [Cu(2,2'-bpy)2]5[α-PW11.5Cu0.5O40]·2H2O 1, [Co(2,2'-bpy)2(N3)2]4H3[α-PW12O40]·3H2O 2 and [Cu(2,2'-bpy)2(4,4'-bpy)]2[α-GeW12O40]-4H2O 3 (2,2'-bpy = 2,2'-bipyridine, 4,4'-bpy = 4,4'-bipyridine) have been hydrothermally synthesized and structurally characterized. 1 crystallizes in the orthorhombic space group Pna21 with a = 27.847(3), b = 21.597(2), c = 20.1179(19)A, V= 12099(2)A^3, Z= 4, GOF= 1.038, R = 0.0427 and wR = 0.1035; 2 belongs to the triclinic space group P1^- with a = 12.31150(10), b = 16.1954(4), c = 19.36290(10)A, α = 99.366(11), β =105.168(8), γ = 111.836(8)°, V = 3309.98(9)A3, Z = l, GOF = 1.024, R = 0.0739 and wR = 0.2216; and 3 crystallizes in the monoclinic space group P21/n with a = 12.858(4), b = 20.943(6), c = 15.598(5)A, β = 102.338(5)°, V= 4103(2)A3, Z = 2, GOF = 1.026, R = 0.0557 and wR = 0.1316. The common structural features of 1-3 are that their molecular structures all consist of a saturated a-Keggin polyoxoanion and several discrete metal-organic moieties. Intriguingly, 2 and 3 are composed of metal-organic coordination moieties with two mixed ligands.  相似文献   

9.
A supramolecular compound, [ Co(2,2'-bipy) ( H2O)4 ] [ trans-1,4-chdc ] ( compound 1 ) ( 2,2'-bipy = 2,2'- bipyridine, 1,4-chdcH2 = 1,4-cyclohexanedicarboxylic acid), was synthesized and characterized by single-crystal Xray diffraction analysis, IR spectrometry, TG analysis, and elemental analyses. Single-crystal X-ray diffraction analysis revealed that [ Co( 2,2'-bipy) ( H2O)4 ]^2+ units and adjacent 1,4-chdc^2- formed a single layer by hydrogen bonding and electrostatic interactions along the ac-plane, and two symmetry-related single layers interacted with each other by hydrogen bonding, resulting in a double layer, which further formed a 3-D structure by π-π stacking. The most attractive structural feature of compound 1 is that 1,4-chdc2- possesses only tram-conformation although there are both c/s- and tram-conformations in the raw material.  相似文献   

10.
The title compound [Zn(btzb)2Cl2]·2H2O (1·2H2O, btzb = 1,2-bis(5-tetrazolyl)ben- zene) was synthesized in situ by the [2+3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence of ZnCl2 under refluxing conditions. 1·2H2O crystallizes in the monoclinic system, space group P2 1/c with a = 9.0119(18), b = 7.5566(15), c = 18.076(5)A, β= 114.67(2)°, V= 1118.6(4)A^3, Z = 2, Dc = 1.784 g/cm^3, T= 223(2) K, C16H16N16O2Cl2Zn, Mr = 600.74, F(000) = 608, μ(MoKα) = 1.393 mm^-1, S = 1.081, R = 0.0306 and wR = 0.0669 for 1896 observed reflections with I 〉 2σ(I). The Zn^2+ ion of 1 is coordinated by four N atoms from two btzb ligands and two Cl atoms, forming a distorted octahedral coordination geometry. A number of intermolecular hydrogen bon- ding interactions between molecules 1 and/or the solvated water molecules result in a 3D hydrogen-bonded structure. The luminescent property of 1·2H2O was also investigated.  相似文献   

11.
A new copper(II) complex Cu2(L)a(2,2'-bipy)2(H2O)2 (1) has been synthesized with 2-benzoylbenzoic acid (HL) and 2,2'-bipyridin as ligands. The crystal belongs to a monoclinic system with space group Cc, a = 13.9979(II), b = 15.9888(13), c = 30.306(3) A, β = 100.8700(10)°, V= 6661.1(10) A3, Dc= 1.372 g/cm3, Z = 8, F(000) = 2840, the final GOOF = 1.018, R= 0.0685, and wR= 0.1731. There are two mononuclear Cu(L)2(2,2'-bipy)(H20) units in the crystal of 1. Each Cu(II) cation is coordinated by five atoms. The magnetic and fluorescent properties of 1 were studied. The results show that 1 exhibits weak paramagnetism, and when the excitation wavelength is at 616 nm, it has an intense fluorescent emission band around 482 nm.  相似文献   

12.
赵丹  郑寿添  杨国昱 《结构化学》2009,28(4):503-508
One new arsenic-vanadium cluster, [Zn(dien)(Hdien)]2[As6V15O42(H2O)]·4H2O (1, dien = diethylenetriamine), has been hydrothermally synthesized and characterized by IR, elemental analysis, TGA, magnetic property and single-crystal X-ray diffraction analysis. Crystal data for 1: monoclinic, space group P21/n, a = 13.959(3), b = 22.428(5), c = 22.831(5) A^°, β = 90.733(4)°, Z = 4. X-ray crystallographic study showed that compound 1 is constructed from [As6V15O42(H2O)]^6- polyoxoanions linked together by novel [Zn(dien)(Hdien)]^3+ complex fragments via hydrogen bonds into a three-dimensional network. Variable temperature susceptibility measurement demonstrates the presence of antiferromagnetic interaction between V^IV cations in 1.  相似文献   

13.
A metal-organic coordination compound formulated as [Cd(pzdc)(2,2'-bipy)]n·nH2O 1 (Hzpzdc = pyrazine-2,3-dicarboxylic acid, 2,2'-bipy = 2,2'-bipyridine) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P2 1/c with a = 10.8081(13), b = 14.4328(17), c = 10.2530(12) A, β = 98.504(2)°, V= 1581.8(3) ]A3, C16H14CdN4O5, Mr= 454.71, Dc = 1.909 g/cm^3, μ(MoKa) = 1.420 mm^-1, F(000) = 904, Z = 4, the final R = 0.0230 and wR = 0.0554 for 2901 observed reflections (I 〉 2σ(I)). It exhibits an interesting two-dimensional network structure and shows yellow photoluminescent property at room temperature.  相似文献   

14.
A new compound has been synthesized under hydrothermal conditions and characterized by IR, elemental analysis, XPS and single-crystal X-ray diffraction analysis. The title compound [Mn(en)3]2en0.5[HV8VV8IVO38(CI)]·4.5H2O crystallizes in monoclinic, space group C2/c, with a = 17.016(4), b = 18.858(4), c = 18.872(4) A, β = 93.667(4)°, V = 6043(2)A3, Z = 4, Dc = 2.242 g/cm3, Mr = 2040.12, F(000) = 4020,μ = 2.895 mm-1, Rint = 0.0921, R = 0.0649 and wR = 0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38(CI)]4- cage, two [Mn(en)3]2^2+ cations, four and a half lattice waters and a half ethylenediamine. In addition, intermolecular O-H...N, O-H...O, N-H...O and C-H...O hydrogen bonds link the molecules together to form a three-dimensional structure.  相似文献   

15.
An organic-inorganic hybrid based on a-Keggin-typed [BWI2040]5- anionic cluster, [Co(BIIM)3]2H[BWx2040]'7H20 (BIIM = 2,2"-biimidazole), was hydrothermally synthesized and structurally characterized by thermogravimetric analysis, IR and UV spectra. The title compound crystallizes in monoclinic, space group P21/n with a = 12.3490(10), b = 33.270(3), c = 18.9660(16) A, β = 105.9950(10)°, V= 7490.5(11) A3, C36HsoBCo2N24047W12, Mr = 3905.80, Dc = 3.45 l g/cm3, μ(MoKa) = 18.886 rnm-1, F(000) = 6972, Z = 4, S = 1.004, the final R = 0.0404 and wR = 0.0914 for 14683 observed reflections (1 〉 2tr(/)). The compound consists of two isolated [Co(BIIM)3]2+ cations and one [BW12040]5 anion, in which each Co2+ ion is coordinated by six N atoms from three BIIM ligands displaying a regular CoN6 octahedron. These components are finally linked together via N-H...O(polyoxometalate and wate) hydrogen bonds into a two-dimensional framework. Full investigation of the intermolecular interactions by Hirshfeld surface and fingerprint plots clearly indicates that there are rare W--Oterminal···πimidazole ring interactions which cooperate with the classical N-H···O hydrogen bonds to stabilize the structural packing.  相似文献   

16.
谢学群  杨春龙  李前进 《结构化学》2007,26(9):1009-1012
The title compound [Mn(DPMT)2Cl2(H2O)2] (DPMT = 1-[[2-(2,4-dichlorophenyl)- 1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole) was synthesized by the reaction of MnCl2·4H2O and DPMT in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 23.913(4), b = 7.8883(13), c = 8.6291(14) , β = 95.816(3)o, V = 1619.4(5) 3, Z = 2, C24H26Cl6MnN6O6, Mr = 762.15, Dc = 1.563 g/cm3, μ = 0.950 mm-1, S = 1.045, F(000) = 774, R = 0.0462 and wR = 0.0981. The molecular structure is a centrosymmetric conformation, and two ligands are symmetrically located on both sides of the Mn atom. The manganese atom is surrounded by two nitrogen atoms from ligands, two chlorine atoms and two oxygen atoms from water molecules to form a slightly distorted octahedral geometry.  相似文献   

17.
A supramolecular compound(H2en)2[Cu(en)2(H3O)2][Mo8O28](en=ethylenediamine) was hydrothermally prepared and confirmed by elemental analysis and TG analysis.Single-crystal X-ray analysis reveals that the crystal crystallizes in the triclinic system,space group P1 with a=9.4635(4),b=9.8645(5),c=10.9794(5),α=69.2050(10),β=72.3730(10),γ=78.4510(10)o,Mr=1559.55,V=908.24(7)3,Z=1,Dc=2.851 g/m3,F(000)=749,μ=3.350 mm-1,S=1.000,the final R=0.0217 and wR=0.0567.The compound consists of(H2en)2+,[Mo8O28]8-anion and [Cu(en)2(H3O)2]2+ cations and constructs a 3D supramolecular structure through hydrogen bonds between the nitrogen atoms from en of [Cu(en)2(H3O)2]4+ fragments and the terminal oxygen atoms from the [Mo8O28]8-polyoxoanions.The electrochemical behavior of this compound has been studied in detail based on a solid bulk modified carbon paste electrode of compound(CPE).  相似文献   

18.
A novel zinc(H) metal phosphonate compound [Zn(phen)(m-OOCC6H4PO3H)] 1 (phen = phenanthroline) has been synthesized under hydrothermal conditions. Single-crystal X-ray structure analysis reveals that compound 1 belongs to the triclinic system, space group P1 with a = 9.3356(19), b = 10.203(2),c = 10.743(2)A,α = 76.3030(70), β= 69.2317(51), y = 84.3833(74)°,V = 929.4(3) ,A3, Z = 2, C2OH15N2O5PZn, Mr = 459.68, Dc = 1.643 g/cm^3,μ= 1.444, mm^-1, F(000) = 468, the final R = 0.0330 and wR = 0.0848. In the structure, the central ion Zn(H) is five-coordinated, linking three O atoms with one from carboxyl and the other two from phosphonyl group. The remained two coordinate sites were occupied by two N atoms from one phen molecule to form the asymmetric unit. Then every two adjacent asymmetric units are bridged by the O atoms from phosphonate group and carboxyl to give rise to a 1D chain along the b axis. These chains are constructed by weak π-π stacking interactions and C-H…π interactions to generate a 3D supramolecular framework.  相似文献   

19.
Two new cobalt(II) supramolecular complexes [Co(4,4'-bipy)2(H2O)4]·[Co2(4,4'-bipy)3(H2O)8]·2TST·2(4,4'-bipy)·4H2O 1 and [Co(4,4'-bipy)2(H2O)4]DSNT·4,4'-bipy 2 based upon the assembly of Co(II), 4,4'-bipyridine (4,4'-bipy) and two new multifunctional organic ligands, 2,4,6-tris(4-sulfophenyl- amino)-1,3,5-triazine (H3TST) and 2,4-bis(p-sulfanilato)-6-diethylamino-1,3,5-triazine (H2DSNT), have been prepared by hydrothermal method and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal structure of 1 is of monoclinic, space group P21/n with a = 13.599(4), b = 18.988(6), c = 22.995(7) A, β = 90.273(6)°, V = 5938(3)A^3, Z = 4, C56H59Co1.5N13O17S3, Mr = 1370.74, Dc = 1.533 g/cm^3, μ = 0.613 mm^-1, F(000) = 2842, GOOF = 1.018, the final R = 0.0796 and wR = 0.1498 for 9019 observed reflections with I 〉 2σ(I). The crystal structure of 2 belongs to the monoclinic system, space group C2/c with a = 18.864(6), b = 14.283(5), c = 20.246(7)A, β = 107.799(6)°, V = 5194(3)A^3, Z = 4, C49H52CoN12O10S2, Mr = 1092.08, Dc = 1.397 g/cm^3, μ = 0.480 mm^-1, F(000) = 2276, GOOF = 1.059, the final R = 0.0665 and wR = 0.1900 for 4887 observed reflections with I 〉 2σ(I). The results of X-ray crystal structure analysis revealed that complexes 1 and 2 exhibit layered supramolecular frameworks stabilized by electrostatic interactions, π-π interactions and hydrogen bonds.  相似文献   

20.
[Co^11(phen)3]2[{(ZnW12O40)Co^11(phen)2(H2O)}2Co^11(trien)2(NaH2O)2]·3H2O was synthesized via hydrothermal technique and characterized with elemental analyses, IR spectroscopy, TGA-DTA, and variable temperature magnetic susceptibility. The compound crystallized in the monoclinic system with the space group P21/n, a=1.8210 nm, b=2.3592 nm, c=2.2932 nm, β=110.31°, V=9.239 nm^3, Z=2, R1=0.0827. The compound consists of two coordination cations, three lattice water molecules, and a macroanion [{(ZnW12O40)Co(phen)2(H2O)}2Co(C6H18N4)2·(NaH2O)2]^4- in which each supported Keggin anion [(ZnW12O40Co^11(phen)2(H2O)]^4- acts as a ligand to coordinate to central bridging Co^2+ ion via a terminal oxygen atom. Hydrogen bonds are responsible for the construction of 3D architecture of the compound. The compound is paramagnetic with a weak antiferromagnetic interaction(0=-46.796 K).  相似文献   

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