Hydrothermal synthesis and crystal structure of a novel compound: [Ni(phen)(3)](2)[(SiMo10V2O40)-O-IV((VO)-O-IV)2]center dot 2H(2)O

A novel compound [Ni(phen)(3)](2)[(SiMo10V1/2O40)-O-V((VO)-O-IV)(2)] . 2H(2)O has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the triclinic, system, space group P-1, a = 12.378(4) Angstrom, b = 14.148(5) Angstrom, c = 14.316(2) Angstrom, alpha = 105.91(2)degrees, beta = 95.31(2)degrees, gamma = 96.89(3)degrees, V = 2373.0(12) Angstrom(3), Z = 1, (lambdaMo(Kalpha)) = 0.71073 Angstrom, R1 (wR2) = 0.0869(0.2174). Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range of 1.51 < theta < 22.50degrees using the omega-scan technique. Empirical absorption correction (psi scan) was applied. The structure was solved by the direct method and refined by the Full-matrix least-squares on F-2 using the SHELXL-97 software. X-ray crystallographic study showed that the title compound contained a bi-capped alpha-Kegin-type [(SiMo10V2O40)-O-IV((VO)-O-IV)(2)](4-) polyoxoanion.

The AFM characterization of Ni(phen)(3)(2+) fixing effects on DNA

In this paper, the fixing and stretching effect of Ni(phen)(2+)(3) with different concentrations on DNA had been studied by Tapping mode AFM. Under an ambient condition, the high-resolution DNA images were obtained, the average height, width and length of well spread DNA molecules were measured. The results showed that because of the variations of ionic concentration, the density and topography of DNA molecules on substrate had a great difference. The AFM and gel electrophoresis results also showed that, under our experimental condition, DNA molecules kept intact, Ni(phen)(2+)(3) did not catalyze the cleavage activity of EcoRI, therefore, Ni (phen)(2+)(3) would be used to make high-resolution physical mapping of DNA by AFM.

Single-crystal X-ray structure and properties of K-10[Ni-4(H2O)(2)(AsW9O34)(2)]center dot 4H(2)O

The rational synthesis and the structural and magnetic characterization of a nickel cluster are presented. The compound comprises a rhomblike Ni4O16 group encapsulated between two-heptadentate tungstoarsenate ligands [AsW9O34](9-). The crystal structure of K-10[Ni-4(H2O)(2)(AsW9O34)(2)](.)4H(2)O was solved in monoclinic, P2(1)/n symmetry, with a = 12.258(3) Angstrom, b = 21.232(4) Angstrom, c = 15.837(3) Angstrom, beta = 92.05(3)degrees, V = 4119.1(14) Angstrom(3), Z = 2, and R = 0.0862. The crystal structure of the Ni(II) derivative was compared with that of the Cu(II), Zn(II), Co(II) and Mn(II) derivatives. The Ni4O14(H2O)(2) unit in the compound shows no Jahn-Teller distortion. On the other hand, the Ni(II) derivative shows ferromagnetic exchange interactions within the Ni4O16 group (J = 7.8 cm(-1), J' = 13.7 cm(-1)) and an S = 4 ground state, the highest spin state reported in a heteropoly complex. Its redox electrochemistry has been studied in acid buffer solutions using cyclic voltammetry. It exhibited two steps of one-electron redox waves attributed to redox processes of the tungsten-oxo framework. The new catalyst showed an electrocatalytic effect on the reduction of NO2-.

Hydrothermal synthesis and crystal structure of a novel layered compound [Ni(C10H8N2)(2)V3O8.5]

A novel layered compound, [Ni(C10H8N2)(2)V3O8.5], was hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. The compound crystallizes in monoclinic system, space group P21/c with a = 1.551 8(3) nm, b = 1.476 1(3) nm, c = 1.048 3(2) nm, beta = 92.02(3), V = 2.399 8(8) nm(3), Z = 4, R = 0. 046 7, wR(2) = 0. 085 9.

Hydrothermal synthesis and structural characterization of a mixed-valence molybdenum (IV,VI) arsenate (III): Ni(H2NCH2CH2NH2)(3)[((MoO6)-O-IV)(Mo6O18)-O-VI((As3O3)-O-III)(2)]H2O

A novel mixed-valence molybdenum(IV, VI) arsenate(III), Ni(H2NCH2CH2NH2)(3)[((MoO6)-O-IV)(Mo6O18)-O-VI((As3O3)-O-III)(2)]H2O, hydrothermally synthesized and characterized by single-crystal X-ray diffraction and thermogravimetric analysis. The polyanion cage derives from the Anderson structure, in which the central octahedron was filled up by molybdenum(IV) and it was capped on both sides by a novel As3O63- cyclo-triarsenate(III). The title compound had a high catalytic activity for the oxidation of benzaldehyde to benzoic acid using H2O2 as oxidant in a liquid-solid biphase system. (C) 1999 Elsevier Science B.V. All rights reserved.

Metal-oxo cluster-supported transition metal complexes: hydrothermal synthesis and characterization of [{M(phen)(2)}(2)(Mo8O26)] (M = Ni or Co)

Two new metal-ore supported transition metal complexes, E{M(phen)(2)}(2)(Mo8O26) (M = Ni or CO; phen = 1,10-phenanthroline) are synthesized by a hydrothermal method and characterized by X-ray crystallography, showing that the octamolybdate possesses a novel unprecedented structure and that [M(phen)(2)](2+) units are covalently bonded to the [Mo8O26](4-) cluster.

[Ni(C10H8N2)(3)](2)[V4O12].11H(2)O

The crystal structure of the title compound, bis[tris(2,2'-bipyridyl-N,N')nickel(II)] cyclo-tetravanadate undecahydrate, contains a centrosymmetric [V4O12](4-) anion, which has an eight-membered ring structure formed by four VO4 tetrahedra sharing vertices, and two complex cations containing octahedrally-coordinated Ni-II ions. The anion and coordinated Ni-II ions are isolated and make up anion and cation layers, respectively. The Ni-N distances range from 2.077(3) to 2.112(2)Angstrom and the V-O distances range from 1.621(2) to 1.803(2)Angstrom.

Comparative study on the doping effect of 3d elements in Bi(1.5)Pb(0.2)Sr(2)Ca(2)Cu(2.8)M(0.2)O(y) (M=Sc,Ti,V,Cr,Mn,Fe,Co,Ni, or Zn)

With XRD, R-T, and ac chi measurements a comparative study on the doping effects of 3d elements in Bi(1.5)Pb(0.2)Sr(2)Ca(2)Cu(2.8)M(0.2)O(y) (M = Sc, Ti, V, Cr, Mn, Fe, Co, Ni, or Zn) has been carried out. The effects of the former five members are significantly different, both on phase formed and on T-c, from the latter four. It seems that the effect on phase stabilization correlates with the valency of the doped cation. In connection with the instability of the 2223 phase, the correlation has been discussed.

Studies on the adsorption property of NO on the Ni-based mixed oxide catalysts with Perovskite-like (ABO(3) and A(2)BO(4)) structure

The mixed oxides LaNiO3, La0.1Sr0.9NiO3, La2NiO4 and LaSrNiO4 with perovskite (ABO(3)) and related(A(2)BO(4)) structures were prepared and the adsorption property for NO and the catalytic activity for NO decomposition over these oxidse were also tested. The catalysts were characterized by means of BET surface measurement, chemical analysis, NO-TPD etc.. It was shown that the adsorption amount of NO is correlated with the concentration of oxygen vacancy formed and the adsorption type and strength of NO are related to the valence of metallic ion. Generally there are three kinds of adsorption species, NO-, NO+ and NO on the mixed oxides, among them the negative adsorpion species (NO-) are active for NO decomposition. The weaker the adsorption of oxygen on the catalyst is, the faster the mobility of oxygen is and the easier the redox process takes place in reproducing the active sites in which the oxygen species (O-, O2-) would participate.

SYNTHESIS AND X-RAY STRUCTURE OF A SEMICONDUCTING ORGANOMETALLIC SALT [FECP(TOL)](2)[NI(MNT)(2)]

The compound [FeCp(Tol)](2)[Ni(mnt)(2)] has been prepared from [FeCp(Tol)]AlCl4 and Na-2[Ni(mnt)(2)]. This new organometallic radical ionic salt has been characterized by elemental analysis, IR, H-1 NMR and mass spectroscopy. The X-ray structure of the compound shows there are segregated cation and anion stacks in the perpendicular directions, The molecular anions form a zig-zag stacking along the b axis, and between every two neighbouring anion planes a methyl group of the cation is inserted. This gives rise to a long spacing of 6.87 Angstrom, between the anion planes. The cations stack along the c axis, with the closest spacing of 3.457 Angstrom between the cyclopentadienyl plane and the neighbouring toluene plane, which is shorter than the sum of Van der Wall's radii. Conductivity measurements showed the compound as a semiconductor with a room temperature conductivity of 1.6 X 10(-4) Scm(-1).

A BINUCLEAR NICKEL(II) COMPLEX CONTAINING AN OXAMIDO-BRIDGE - SYNTHESIS, PROPERTIES AND X-RAY CRYSTAL-STRUCTURE OF [NI(OXAE)NI(PHEN)(2)](CLO4)(2)CENTER-DOT-3H2O

The binuclear complex [Ni(oxae)Ni(phen)2](ClO4)(2) . H2O (oxae=N,N'bis(2-aminoethyl) oxamido dianion, phen = 1, 10-phenanthroline) was prepared from the planar monomeric complex Ni(oxae) and characterized through analytical and spectroscopic measurements. The structure of [Ni(oxae)Ni(phen)(2)] (ClO4)2 . 3H(2)O was investigated by single-crystal X-ray analysis. The complex has an extended oxamido-bridged structure and consists of two nickel(II) ions, one of them in a square planar environment and another in a distorted octahedral environment. The Ni-Ni distance is 5.267 Angstrom.

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Hydrothermal synthesis and crystal structure of cluster compound {[Ni(enMe)(2)][SiW12O40]}[Ni(enMe)(2)(H2O)(2)](2) center dot 3H(2)O

the novel One-dimensional chain structure of the title cluster compound was synthesized and characterized by elemental analysis, IR spectra, TGA and X-ray single-crystal diffraction. The title cluster compound crystallized in a monochnic system with space group C2/c, a = 1.2656 nm, b = 2.20656 (4) nm, c =2.26763 (4) nm, beta = 92.078 degrees, V = 6.32852 (16) nm(3), Z = 4, D-c = 3.801 g/cm(3), A = 2.271 mm(-1), F(000) = 6512, R-1= 0.0549, wR(2) = 0.1087. The structure building block of the structure is the polyanion [SiW12O40](6-) with alpha-Keggin structure. The clusters were linked together with one-dimensional infinite chain through [ Ni ( enMe) (2)] (2+) cations. The [ Ni ( enMe) (2) ( H2O) (2)] (2+) cations and water molecules were filled in the structure. The cluster compound was expanded to three-dimensional framework by hydrogen bond interactions among molecules.