Synthesis, properties and crystal structure of a heteropoly compound containing titanium

K4H2CoW12O40. 2Ti02 . 9H(2)O crystallizes from an aqueous solution of Na2WO4, Co(OAc)(2) and Ti(SO4)(2). The compound has very similar i.r. and u.v. spectra to those of [CoW12O40](6-) and [CoW11TiO40](8-) but its polarographic behaviour is different from that of [CoW11TiO40](8-) and exhibits only reduction of tungsten(VI). A single crystal structural analysis indicates that this compound consists of the heteropolyanion [CoW12O40](6-), titanium-oxygen chain, potassium ions and water molecules.

Fractal roughness characterization of super-ground Mn-Zn ferrite single crystals

The surface of superground Mn-Zn ferrite single crystal may be identified as a self-affine fractal in the stochastic sense. The rms roughness increased as a power of the scale from 10(2) nm to 10(6) nm with the roughness exponent alpha = 0.17 +/- 0.04, and 0.11 +/- 0.06, for grinding feed rate of 15 and 10 mu m/rev, respectively. The scaling behavior coincided with the theory prediction well used for growing self-affine surfaces in the interested region for magnetic heads performance. The rms roughnesses increased with increase in the feed rate, implying that the feed rate is a crucial grinding parameter affecting the supersmooth surface roughness in the machining process.

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.

SYNTHESIS AND X-RAY CRYSTAL-STRUCTURE CHARACTERIZATION OF ZN2(HPO4)(3).H3NCH2CH2NH3

A novel framework material, Zn-2(HPO4)(3).H3NCH2CH2NH3, has been synthesised and its crystal structure determined by single crystal X-ray diffraction.

SYNTHESIS AND CHARACTERIZATION OF BINUCLEAR ORGANOLANTHANIDE COMPLEXES INVOLVING CYCLOPENTADIENYL AND N-PROPYLOXIDE LIGANDS - X-RAY CRYSTAL-STRUCTURE OF [(C5H5)2YB(MU-OCH2CH2CH3)]2

By the reaction of Cp3Ln (Cp = C5H5; Ln = Dy, Ho, Yb) with equimolar n-propyl alcohol in THF (tetrahydrofuran) at room temperature three new binuclear organolanthanide complexes, [CP2Ln(mu-OCH2CH2CH3)]2 (Ln = Dy, Ho, Yb), have been synthesized, as shown by X-ray single-crystal structure analysis for the complex [Cp2Yb(mu-OCH2CH2CH3)]2. All the complexes were characterized by elemental analysis, IR and MS spectra. The Yb2O2 unit is planar, and the ytterbium atom is coordinated by two Cp ring centroids and two oxygen atoms of two n-propyloxide ligands to form a distorted tetrahedral geometry. The average Yb-C (Cp) bond distance is 2.589(17) angstrom. The average Yb-O distance is 2.199(5) angstrom. The Yb-Yb separation [3.521(1) angstrom] indicates that no metal-metal interaction is present.

THE SYNTHESIS AND CRYSTAL-STRUCTURE OF MOLYBDENUM-SILICON BLUE

The single crystal of heteropoly blue, HsSiMo12O40.12H2O, the reduced product of molybdenum-silicon heteropoly acid, was prepared by electrochemical reduction and evaporation in nitrogen atmosphere. The Crystal structure of the product was determined. The heteropoly blue H8SiMo12O40.12H2O, Crystallizes space group P1BAR a = 1.3769 (3) nm, b = 1.4346 (4) nm, c = 1.4134 (4) nm, alpha = 120.47 (2)-degrees, beta = 110.70 (2)-degrees, gamma = 66.11 (2)-degrees, Z = 2, R = 0.0608. The heteropoly blue anion was determined to have Keggin Structure and alpha-isomer and it remained the structure of the unreduced heteropoly acid anion. But the distortion of the structure and the changes of bond length and bond angle take place obviously. The four Mo5+ Positions were determined in the structure.

CRYSTAL-STRUCTURE OF 1, 10-DECANEDIAMMONIUM TETRACHLOROZINCATE

The crystal structure of the title compound has been determined from single crystal X-ray diffraction. The complex crystallizes in the triclinic space group P1 with Z=2. Lattice parameters are: a = 0.7296(1), b = 1.0110(3), c = 1.2814(4) nm; alpha = 90.84(2), beta = 101.17(2), gamma = 92.52(2)-degrees. Intensity data were collected on a Nicolet R3M/E four-circle diffractometer using MoK alpha (lambda = 0.071073 nm) radiation. The structure was solved by Patterson and Fourier techniques and refined by least-squares techniques to R = 0.065. The structure of the complex consists of tetrahedral ZnCl42- anions which form a two-dimensional sheets. Tetrahedral ZnCl42- anions are sandwiched between two hydrocarbon layers which consist of [NH3(CH2)10NH3]2+ cations. Each [NH3(CH2)10NH3]2+ group is in a gauche bond between C atoms near NH3 polar heads.

INFRARED SPECTRA AND CRYSTAL STRUCTURE OF BIS-(DIMETHOXYLPHOSPHATO) COPPER

The title complex has beep synthesized by the reaction of CaCl2, with trimethyl phosphate. Its Infrared spectra from 4000 to 100 cm(-1) measured. The assignment of acme absorption bands was discussed. It is found that the stretching vibrations of bridge groups O-P-O are divided into two groups according to their bond length. The crystal structure of the complex boa been determined from single crystal K-ray diffraction data. The crystals belong to monoclinic system, space group P2(1)/c with cell parameteras, a = 1,0704(4), b = 0.5093(2), c = 1.9737(6)nm, beta = 96.23(3)degrees, V = 1.0696(6)nm(2), Z = 4, final R = 0.044. Copper ion is coordinated to five Rimester oxygen atoms to form a distorted square pyramid. The adjacent copper ions are connected by symmetric and non-symmetric bridge groups of O-P-O, forming an infinite one-dimensional chain coordination polymer.

SYNTHESIS AND CRYSTAL-STRUCTURE OF K4H2[PMO9V3O40].10H2O

The crystal structure of the title compound was determined from single crystal X-ray diffraction at -90-degrees-C. The complex crystallizes in the tetragonal P4/mnc, Z = 2, a = 12.515(3), c = 17.636(7) angstrom. The structure was solved by Patterson and Fourier techniques and refined by least-squares to R = 0.061 for 788 reflections. The central PO4 is disordered, P-O = 1.54 angstrom, M(M = Mo or V) is 6-coordinate, M-O = 1.62-2.48 angstrom, K is 7-coordinate, K-O = 2.84-3.10 angstrom.

SYNTHESIS AND CRYSTAL-STRUCTURE OF A NEW LANTHANIDE CYCLOOCTATETRAENE COMPLEX (ETA-8-C8H8)ER(MU-ETA-8-C8H8)K(MU-ETA-8-C8H8)ER(MU-ETA-8-C8H8)K(THF)4

The tetranuclear nearly-linear complex (eta-8-C8H8)Er(mu-eta-8-C8H8)K(mu-eta-8-C8H8)Er(mu-eta-8-C8H8)K(THF)4 (THF = tetrahydrofuran) is first synthesised by the reaction of benzylcyclopentadienyl erbium dichloride (PhCH2C5H4)ErCl2.3THF with cyclooctatetraenyl potassium K2C8H8 in 1:1 molar ratio in THF; a single crystal X-ray study has shown that the complex has the tetralayer-sandwich structure and that the adjacent Er3+ and K+ ions are bridged by eta-8-cyclooctatetraenyl group.

STUDY OF BIMETALLIC COMPLEXES OF RARE-EARTH LITHIUM - SYNTHESIS AND CRYSTAL-STRUCTURE OF THE (LACL)DME(MU-2-CL)5(MU-3-CL) (LA.DME)LI(THF)2

The reaction between LaCl_3 and LiCl in THF at room temperature, with hexane as precipitant and glycol dimethyl ether as complexing agent, has been studied. A complex with the composition of (LaCl)DME(μ_2-Cl)_5(μ_3-Cl)(La·DME)Li(THF)_2 has been synthesized, its structure was studied by single crystal X-ray diffraction technique. The diffraction intensities were collected at about —100℃. The complex belongs to the triclinic space group P1 with α=11.123(3), 6=16.564(5), c=8.653(3)A, α=95.16(3), β=...

Synthesis, crystal structure and biological activities of N '-(4-methoxybenzylidene)-2-(1H-1,2,4-triazol-1-yl) acetohydrazide

The title compound, N'-(4-methoxybenzylidene)-2-(1H-1,2,4-triazol-1-yl)acetohydrazide, was synthesized and its structure was confirmed by means of IR, MS,H-1 NMR and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test shows that the synthesized compound has a low antifungal activity.

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.

Crystal structure and DFT studies of a triazole derivative: 4-(2-hydrobenzylideneamino)-3-(1,2,4-triazol-4-yl-methyl) 1H-1,2,4-triazole-5 (4H)-thione

A novel triazole derivative 4-(2-hydrobenzylideneamino)-3-(1, 2, 4-triazol-4-ylmethyl)-1H-1, 2, 4-triazole-5 (4H)-thione(1) was synthesized and characterized using elemental analysis, MR, and H-1 NMR, and its crystal structure was determined via X-ray single crystal diffraction analysis. Crystal data: monoclinic, P2 (1)/c, a = 0.83335 (9) nm, b = 1. 49777 (16) run, c = 1. 14724 (12) nm, beta = 107. 990 (2)degrees, D = 1. 470 Mg/m(3), and Z = 4. The geometries and the vibrational frequencies were determined using the density functional theory(DFT) method at the B3LYP/6-31G* level. To demonstrate the accuracy of the reaction route of compound 1, one of the important intermediates was also tested using the same method. The structural parameters of the two compounds calculated using the DFT study are close to those of the crystals, and the harmonic vibrations of the two compounds computed via the DFT method are in good agreement with those in the observed IR spectral data. The thermodynamic properties of the title compound were calculated, and the compound shows a good structural stability at normal temperature. The test results of biological activities show that it has a certain bactericidal ability.

Isolation, characterization and crystal structure of natural eremophilenolide from Ligularia sagitta

A new eremophilenolide 1beta, 10beta-epoxy-6beta-acetoxy-3beta-angeloyloxy-8beta-hydrox y-eremophil-7(11)-en-8, 12alpha-olide (1), together with liguhodgsonal (2), esculetin (3) and beta-sitosterol (4), was isolated from the aerial parts of Ligularia sagitta. The structure of the new constituent (1) was elucidated by spectroscopic methods and confirmed by single-crystal X-ray diffraction.