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1.
A new reduced molybdenum(V) phosphate (H3dien)2(H2dien)2[NaMo12O24 (OH)6 (HEPO4)(HPO4)5(PO4)2]·nH2O (n= 10.92, dien = diethylenetriamine) has been synthesized under hydrothermal conditions and characterized by elemental analyses, IR and X-ray diffraction. C16H96.84MO12N12NaO72.92P8 (Mr = 3046.73) crystallizes in the monoclinic system, space group P21/c with a = 13.3575(18), b = 21.907(3), c = 15.654(2)A, β= 110.22(2)°, V= 4298.4(10) A^3 Dc = 2.354 g/cm^3, Z = 2,μ(MoKcr) = 1.966 mm^-1, F(000) = 2990.4, the final R = 0.0357 and wR = 0.1086 for 8739 observed reflections with I 〉 2σ(I). It consists of sandwich-shaped cluster anions [Na{Mo6P4}2]^10- held together into a three-dimensional supramolecular framework through intermolecular hydrogen-bonding contacts. A probe reaction of the oxidation of acetaldehyde with H2O2 showed that this compound has high catalytic activity in the reaction.  相似文献   

2.
A new sandwich transition metal substituted polyoxotungstate, [NH3(CH2)4NH3]6[Co4(H2O)2(B-α-GeW9O34)2]}·7H2O 1, was hydrothermaUy synthesized and characterized by IR spectra and single-crystal X-ray diffraction. The single-crystal X-ray analysis reveals that the crystal crystallizes in monoclinic system, space group P21/c with a = 16.6073(6), b = 15.3333(5), c = 19.9869(7) A, β = 103.41(1)°, Mr = 5481.38, V = 4950.8(3) A3, Z = 2, Dc = 3.677 g/cm^3, F(000) = 4900, μ(MoKa) = 22.165 mm^-1, GOOF = 1.005, the final R = 0.0228 and wR = 0.0527. The crystal structure indicates that the [Co4(H2O)2(B-α-GeW9O34)2]^12- polyoxoanion contains two trivacant Keggin [B-α-GeW9O34]^10- fragments in a staggered fashion linked via a rhomb-like Co4O16 group in a centrosymmetric arrangement (C2h symmetry) leading to a sandwich-type structure.  相似文献   

3.
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   

4.
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   

5.
One new polyoxometalate compound connected via cobalt/potassium cations,namely H5K{[Co(H2O)5]2(H2Mo3.24W8.76O42)}·19H2O 1,was prepared and characterized by ele- mental analysis and IR spectroscopy. Single-crystal X-ray diffraction analysis result reveals that anions of {[Co(H2O)5]2(H2Mo3.24W8.76O42)}6- in compound 1 are linked by potassium cations to form one- dimensional chain,based on which a three-dimensional network is further constructed with the help of hydrogen bonds. Crystal data: H67Co2KMo3.24O72W8.76,Mr = 3297.87,monoclinic,C2/c,a = 19.0126(10),b = 16.6025(5),c = 19.1908(10)A,β = 106.713(1)°,V = 5801.8(5) A^3,Z = 4,Dc = 3.755 g/cm^3,F(000) = 5961,μ = 18.730 mm^-1,R = 0.0569 and wR = 0.1437 (I 〉 2σ(I)).  相似文献   

6.
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   

7.
DANG Zhen-Hua  ;MOU Si  ;XU Li 《结构化学》2009,28(12):1575-1578
The new binuclear molybdenum(V) complex Na4[Mo2O4(HNTA)2]2·19H2O (NTA = nitrilotriacetate) has been prepared and characterized by single-crystal X-ray diffraction analysis and IR. The crystal has space group Pnma with a = 10.2239(2),b = 23.8174(3),c = 23.1845(4) A,V = 5645.58(16)A^3,Z = 4,C24H66Mo4N4Na4O51,Mr = 1702.50,Dc = 1.958 g/cm^3,μ = 1.027 mm^-1,F(000) = 3280,T = 293(2) K,the final R = 0.0609 and wR = 0.1449 for 5512 observed reflections (I 〉 2σ(I)). Each MoV atom has a distorted octahedral coordination geometry,and the two coordination octahedra share a common edge to form a dioxo-bridged Mo2O4 unit which is coordinated by NTA ligands. The dianionic binuclear units [Mo2O4(HNTA)2]^2- are interconnected by Na^+ into a layered structure.  相似文献   

8.
蔡成翔  何坤欢  蒋毅民 《结构化学》2009,28(10):1275-1280
The title complex [Cu2(Sams)2(H2O)2(bipy)]·(H2O) 1 (H2Sams = N-(2-hydroxybenzy) aminomethanesulfonic acid, bipy = 4,4′-bipyridine) has been synthesized by the reaction of Cu- (CH3COO)2·H2O, nESams and 4,4′-bipyridine in aqueous methanol. It was characterized by IR, elemental analysis, thermogravimetric analysis (TGA) and X-ray diffraction analysis. Complex 1 crystallizes in monoclinic, space group P21/n with a= 10.9533(17), b = 8.3408(13), c = 16.714(3) A^°, β = 101.295(4)°, V = 1494.3(4) A^°3 and Z = 2. The asymmetric unit is comprised of a tridentate Schiff base Sams^2- anionic ligand, a 4,4′-bipyddine and two coordinated water molecules, thus forming a binuclear copper(Ⅱ) complex. The coordination environment at Cu^Ⅱ center is described as a slightly distorted square pyramidal geometry. Via intermolecular hydrogen bonds C(10)-H(10)…O(3) and C(13)- H(13)…O(3), an infinite supramolecular chain is yielded. A number of intermolecular hydrogen bonds greatly contribute to the stabilization of the solid-state structure for 1.  相似文献   

9.
A transition metal substituted polyoxotungstate, [Cu(en)2(H2O)]2{PW11.5Cu0.5O40[Cu(en)2] }·2H2O
1 based on Keggin frameworks, has bccn hydrothcrmally synthesized and characterized by IR, TGA and single-crystal X-ray structural analysis. It is interesting to find that the structure unit contains two different valence cations, narncly, one [Cu(1)(en)2(H2O)]^+ and one [Cu(2)(en)2(H2O)]^2+. Data for the crystal: orthorhombic system, space group Pbca, a = 21.585(2), b = 20.695(2), c = 26.137(3)A, V = 11675(2)A^3, Z = 8, Mr = 3428.23, Dc = 3.901 g/cm^3, F(000) = 12156,μ(MoKα) = 23.932 mm^-1, the final R = 0.0468 and wR = 0.0969 for 6927 observed reflections (I 〉 2σ(I)).  相似文献   

10.
Two new nonmetal borates, [(C2H10N2)]2[B14O20(OH)6] 1 and [C8H22N4][B5O6(OH)4]2 2, have been synthesized under mild conditions and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis and thermogravimetric analysis. Crystal data for compound 1: triclinic, space group P^-1, a = 8.4979(17), b = 8.8498(18), c = 10.065(2)A^°, α = 95.01(3), β = 96.99(3), γ = 116.82(3)°, V= 661.8(3)A^°^3, Z= 1, Mr = 697.63, Dc = 1.751 g/cm^3,μ = 0.163 mm^-1, F(000) = 356, the final R = 0.0372 and wR = 0.0968 (I 〉 2σ(I)); and those for compound 2: monoclinic, space group P21/c, a = 9.1867(18), b= 14.118(3), c = 10.334(2)A^°, β = 91.48(3)°, V = 1339.8(5)A^°^3, Z = 2, Mr = 610.46, Dc = 1.513 g/cm^3,μ = 0.135 mm^-1, F(000) = 632, the final R = 0.0350 and wR = 0.0912 (I 〉 2σ(I)). For both 1 and 2, the anionic units are interlinked via O-H…O hydrogen bonds to form a 3D supramolecular network, while the protonated cations are located in the free space of the inorganic borate framework and interact with the anions by electrostatic attraction and extensive N-H…O hydrogen bonds.  相似文献   

11.
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   

12.
The title complex [bis(dien)zinc(Ⅱ)] zinc(Ⅱ) tetrachloride was synthesized and characterized by X-ray single-crystal diffraction, elemental analysis, electric conductivity, IR and electronic spectra. The compound crystallizes in the tetragonal system, space group I^-4 with a = 10.250(3), b = 10.250(3), c = 9.054(2) V = 951.2(5)A^3, Mr = 486.95, Z = 2, F(000) = 504, Dc = 1.700 g/cm&3,μ = 3.083 mm^-1, λ. = 0.71073A, the final R = 0.0226 and wR = 0.0642. The symmetric crystal smacture consists of a zinc complex cation [Zn(dien)2]^2+ and a zinc tetrachloride aniOn [ZnC14]^2-, forming a three, dimensional framework through intrmnolecular and intermolecular hydrogen bonds.  相似文献   

13.
A three-dimensional supramolecular architecture, {[Co(proH)(H2O)3]2[P2Mo5O23]}·7H2O (1, pro = praline), has been synthesized and characterized by IR, elemental analysis, thermogravimetric analysis, and single-crystal X-ray diffraction. 1 crystallizes in monoclinic, space group C2 with a = 20.600(3), b = 11.6980(11), c = 9.2944(10)A, β = 107.837(4)°, V = 2132.1(4) A^3, Z = 2, C10H46Co2Mo5N2O40P2, Mr = 1493.99, Dc = 2.327 g/cm^3, F(000) = 1468, μ(MoKα) = 2.375 mm^-1, the final R = 0.0339 and wR = 0.0844 for 4169 observed reflections with I 〉 2σ(I). Singlecrystal X-ray crystallographic analysis reveals that the helical water chains and {[Co(proH)- (H2O)3]2[P2Mo5O23]}n chains are perpendicular to each other and extend into an overall three-dimensional supramolecular architecture by hydrogen-bonding interactions. The magnetic investigation indicates weak antiferromagnetic interactions in the compound.  相似文献   

14.
A new borate [H2EG][B7O10(OH)3] (1) based on [B14O20(OH)6]4- polyborate anions has been solvothermally synthesized in the presence of H2EG as a template (EG = ethylene glycol). The structure was determined by single-crystal X-ray diffraction and further characterized by FFIR, elemental analysis and thermogravimetric analysis. Compound 1 crystallizes in the triclinic system, space group Pi, with a = 8.5095(4), b = 8.8694(4), c = 10.0756(4) A, a = 95.094(2), β = 96.936(2), γ = 116.844(2)°, V = 664.66(5) A3. The structure of 1 consists of [B14O20(OH)6]4- moiety, which could be regarded as the largest isolated polyborate anion so far. The anions are interlinked via hydrogen bonding to form a 3D supramolecular network, whereas the diprotonated [H2EG]2+ are filled in the free space of inorganic borate network and interact with the inorganic framework by extensive hydrogen bonds. It is noteworthy that the EG acts not only as a solvent, but also as a template.  相似文献   

15.
A novel ionic compound [Fe(CN)6·(PhCHeNC9H7)4]·12H2O
(C70H80FeN10O12, Mr = 1309.29) has been synthesized and its structure was characterized by I-R, elemental analysis and X-ray diffraction. The compound crystaUizes in triclinic, space group P1, with a = 10.968(7), b = 11.466(7), c = 14.077(8)A, α= 87.014(7), β= 78.124(7), γ = 72.708(7)°, V = 1654.1(17)A3, Z = 1, Dc = 1.314 g·cm^-3, F(000) = 692, p = 0.298 mm^-1, the final R = 0.0519 and wR = 0.1355. The building unit of the title compound consists of four (PhCH2N+C9H7) ions, one [Fe(CN)6]4- anion, and a dozen water molecules. According to the structural analysis, [Fe(CN)6]4- ions are linked together by O-H…O and O-H…N hydrogen bonds, while (PhCH2N+C9HT) and [Fe(CN)6]4- ions interact with each other by electrostatic force to form an ionic compound.  相似文献   

16.
The title complex [CoL(H20)3]2·H2O (C26H46N4O21S4CO2), where L = taurine-5- methyl-2-hydroxyisophthalaldehydes, has been synthesized and characterized by IR and X-ray diffraction analysis. The crystal of the complex belongs to the triclinic system, space group P1, with a = 11.197(4), b = 13.309(5), c = 14.486(5) ]A, a = 78.827(13),β = 70.547(11), γ = 81.058(13)°, Mr = 996.77, S = 1.08, V= 1987.2(13) A3, Z = 2, Dc = 1.666 g/cm3, F(000) = 1032,μ = 1.131 mm^-1, R = 0.0633 and wR = 0.1293. According to the structural analysis, the Co( Ⅱ ) ion adopts a slightly distorted six-coordinated octahedral geometry. One N atom of the Schiff base of each molecule was hydrogenated to form hydrogen bond with O atom. Two coterminous molecules packed in one crystal water molecule are linked by intermolecular hydrogen bonds, thus generating an infinite chain constructed by hydrogen bonds.  相似文献   

17.
The hydrothermal reaction of copper chloride dihydrate and 5,5-dimethyl-imidazolidine,-2,4-dione with a mole ratio of 1:1 in acetonitrile resulted in the formation of a new acetate-bridged dinuclear copper complex, [C2H6ON]2[Cu2Cl2(μ-CH3COO)4]. Protonated acetamide in eaolie form and acetic acid were yielded by the hydrolysis of acetonitrile under hydrothennal condition. The rifle complex (C12H24Cl2Cu2N2O10) was characterized by X-ray single-crystal diffraction, IR spectrum, elemental and electrochemical analysis. It crystallizes in the monoclinic system, space group P21/c with a = 8.298004), b = 14.358(2), c = 12.0010(2) A^°, β= 130.620(3)°, V = 1085.3(2) A^°^3, Dc = 1.696 g/cm^3, 34, = 554.31, Z = 2, F(000) = 564 and μ = 2.254 mm^-1. The crystal structure consists of a tetraacetate-bridging dinulcear copper complex anion [Cu2Cl2(μ-CH3COO)4]^2-, with the chlorine anions in the axial positions, and two protonated acetamide cations [C2H6ON]^+, which were connected through hydrogen bonds to form a three-dimensional infinite network.  相似文献   

18.
A Keggin-type tungstosilicate compound [Co^Ⅱ(2,2′-bipy)2(H2O)]2[SiW^Ⅵ12O40]·2H2O 1 (bipy = bipyridine) was prepared by a hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 (C40H40Co2N8O44SiW12) 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), γ = 74.186(4)°, V = 1649.84(16)A^3, Mr = 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 [Co^Ⅱ(2,2′-bipy)2(H2O)]^2+, one normal Keggin polyanion unit [SiW^Ⅵ12O40]^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 photoluminescence property in the solid state at room temperature.  相似文献   

19.
A novel inorganic-organic hybrid compound, {[Co(dien)]4[0aO4)MoV8(wV10.56MoV10.44)4- O33(OH)3]}'nH20 (1, n = 1, dien = diethylenetriamine), has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the triclinic system with a = 11.927(2), b = 13.328(3), c = 19.306(4)A, a = 93.76(3), β = 94.14(3), γ = 109.99(3)°, V= 2863.2(12) A3, space group P1 and Z = 2 at 173 K. The final full-matrix least-squares refinement converged to R = 0.049 for 9621 observed reflections with 1 〉 2σ(I) and wR = 0.139 for all data (9871) and S = 1.073. Crystal structure analysis shows that 1 contains a kind of the first reported mixed-valence and molybdenum-tungsten mixed-distributed e-Keggin structural polyanion capped by four Co(dien) fragments with the main group element P occupying the center site. These results were further confirmed by energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Thermogravimetry (TG) and X-ray photoelectron spectroscopy (XPS) analyses.  相似文献   

20.
Under hydrothermal condition, the reaction of 2-naphthoxyacetic acid with ZnCl2 and 4,4′-bipyridine (4,4′-bipy) has afforded a new Zn(Ⅱ) compound, [Zn(C12H9O3)2(C10H8N2)]n·nH2O1, which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of monoclinic, space group P21/c with a = 7.7335(2), b = 19.3834(4), c = 20.1707(4) A, β = 104.9830(10)°, V = 2920.82(11) A^3, C34H28ZnN2O7, Mr = 641.95, Z = 4, Dc = 1.460 g/cm^3,μ = 0.895 mm^-1, F(000) = 1328, R = 0.0406 and wR = 0.0876 for 4417 observed reflections (I〉 2σ(I)) Complex 1 consists of one-dimensional zigzag chains deriving from Zn(C12H9O3)2 units linked by 4,4′-bipy ligands, and lattice water molecules decorate between the chains. Non-covalent interactions, such as hydrogen-bonding and aromatic π-π interactions, lead to the formation of a 3D network structure. The thermogravimetric analysis (TGA) and luminescent property for 1 have also been studied in this paper.  相似文献   

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