X-ray crystal structure of the dye 2-bromo-4-cyano-4′-N,N-diethylaminoazobenzene

The crystal structure of 2-bromo-4-cyano-4′-N,N-diethylaminoazobenzene has been determined from X-ray diffraction data: C₁₇H₁₇N₄Br, mol. wt = 357·1. Triclinic, Pī (No. 2), α = 13·162(5) Å, b = 7·516(3) Å, c = 8·496(4) Å, α = 101·63(4)°, β = 95·79(4)°, γ = 91·49(4)°, V = 818·10 ų, Z = 2, D_c = 1·45 g cm^?3, F(000) = 378, λ(Mo_Kz) = 0·7107 Å, μ(Mo_Kα) = 26·70 cm^?1. The structure was solved by direct methods and refined by full-matrix least-squares to R = 0·053 for 2081 independent reflexions. The molecule possesses an essentially planar azobenzene skeleton. The effects of substituents on the geometry of the azo group are discussed. Significant molecular parameters are: NN, 1·264(6) Å; ₁BrC, 1·904(5) Å; mean NC, 1·410(7) Å; NNC, 115·7(2)° and 113·0(2)°; NCC (cis relative to NN), 125·4(3)° and 123·1(2)°; CC(Br)C, 123·0(2)°.     

Relationships between crystal structure and microwave dielectric properties of (Zn1/3B2/3)xTi1 − xO2 (B = Nb, Ta) ceramics

Dependence of microwave dielectric properties on the crystal structure of (Zn_1/3B_2/3⁵⁺)_xTi_1 − xO₂ (B⁵⁺ = Nb, Ta) ceramics was investigated as a function of Zn_1/3B_2/3⁵⁺O₂ (B⁵⁺ = Nb, Ta) content (0.4 ≤ x ≤ 0.7). Dielectric constant (K) and the temperature coefficient of resonant frequency (TCF) of sintered specimens were strongly dependent on the structural characteristics of oxygen octahedra in rutile structure. Cation rattling and the distortion of oxygen octahedra were dependent on the bond length ratio of apical (d_apical)/equatorial (d_equatorial) of oxygen octahedra. The quality factor (Qf) was dependent on the reduction of Ti ion as well as the microstructure of the sintered specimens.     

Film models for multicomponent mass transfer; computational methods: the exact solution of the maxwell-stefan equations

Computational difficulties which have been encountered in using the Krishna—Standart method for calculation of interphase mass transfer rates in multicomponent mixtures are discussed. Consideration is given to various alternative methods of performing the matrix calculations involved and to the stability of such methods. On this basis a computer algorithm is developed which is faster and more reliable than that published previously.     

The structure of the [Et2In(μ,λ-O2C)–C6H4–2–NH2]∞ coordination polymer: Competition of intramolecular hydrogen bonding with metal–ligand coordination preferences in determining the molecular and crystal structure

The X-ray structure analysis of [Et₂In(μ,λ-O₂C)–C₆H₄–2–NH₂]_n (1) reveals an extended one-dimensional chain comprised of an array of five-coordinate indium centers. The chain unit repeated along two-fold screw axis is defined by the diethylindium moiety chelated asymmetrically by the carboxylate group with one of the two carboxylate oxygens acting as bridge to the next indium center in the chain. The NH₂ group does not participate in the coordination of the metal center but is involved in an intermolecular hydrogen bond.     

Synthesis and crystal structure of Zn[O3PCH(NH2)CH3] · 2H2O, the first zinc α-aminoethylphosphonate with a layer structure

A novel tetrahedrally coordinated zinc phosphonate, Zn[O₃PCH(NH₂)CH₃] · 2H₂O, has been synthesized using hydrothermal techniques. X-ray diffraction indicates that this material is a two-dimensional layered structure with the organic part of the phosphonate anion being directed into the interlayer region. The zinc atoms are coordinated by three oxygens of three different phosphonate groups, and by the nitrogen of an additional phosphonate unit.     

Influence of sintering temperature and holding time on the densification, phase transformation, microstructure and properties of hot pressing WC-40 vol.%Al2O3 composites

WC-40 vol.%Al₂O₃ composites were prepared by high energy ball milling followed by hot pressing. The tungsten carbide (WC) and commercial alumina (Al₂O₃) powders composed of amorphous Al₂O₃, boehmite (AlOOH) and χ-Al₂O₃ were used as the starting materials. The phase transformation during sintering, the influence of sintering temperature and holding time on the densification, microstructure, Vickers hardness and fracture toughness and the toughening effects of WC-40 vol.%Al₂O₃ composites were investigated. The results showed that the amorphous Al₂O₃, AlOOH and χ-Al₂O₃ were transformed to α-Al₂O₃ completely during the sintering process. With the increasing sintering temperature and holding time, the relative density increased and both the Vickers hardness and fracture toughness increased initially to the maximum values and then decreased. When the as milled powders were hot pressed at 1540 °C for 90 min, a relative density of 97.98% and a maximum hardness of 18.65 GPa with an excellent fracture toughness of 10.43 MPa m^1/2 of WC-40 vol.%Al₂O₃ composites were obtained.     

Effect of strontium and phosphorus source on the structure,morphology and luminescence of Sr5(PO4)2SiO4:Euphosphor prepared by solid-state reaction

Sr₅(PO₄)₂SiO₄:Eu²⁺ phosphosilicate phosphor was prepared by high temperature solid-state reaction. Effects of strontium sources (strontium oxide, strontium nitrate and strontium carbonate) and of phosphorus sources (diammonium phosphate, strontium monophosphate) on the reactivity of their mixture during heating and on phase composition, morphology and photoluminescence excitation and emission properties of the phosphors were investigated by TG–DTG–DSC, XRD, SEM and photoluminescence spectroscopy. The sequence of the solid-state reactions when using the different starting reagents was discussed based on the TG–DTG–DSC results. It was found that it is hard to prepare pure Sr₅(PO₄)₂SiO₄:Eu²⁺ phosphor with either of strontium sources studied when stoichiometric (NH₄)₂HPO₄ was used as a phosphorus source. Minor Sr₂SiO₄ impurity phase was present in the phosphors. The content of impurity phase, the morphology and resultant photoluminescence properties of the phosphors were markedly influenced by the strontium source employed. When SrCO₃ was used as the strontium source, the phase purity of the phosphor was improved with the addition of excess (NH₄)₂HPO₄. When (NH₄)₂HPO₄with 5% excess or SrHPO₄ in stoichiometric ratio was used as the phosphorus source a pure phase phosphor was obtained. In addition, the morphology and photoluminescence of the phosphor were also influenced by phosphorus source. The possible reasons causing different properties of the phosphors prepared using different raw materials were discussed based on reaction schemes.     

Dynamic “operando” observation of 1 wt% Pd-based TWCs: Simultaneous XAS/DRIFTS/mass spectrometry analysis of the effects of Ce0.5Zr0.5O2 loading on structure, reactivity and performance

The behavior of 1 wt% Pd-TWCs (three-way catalysts), containing up to 33 wt% Ce_0.5Zr_0.5O₂ is followed under reducing (CO) and oxidizing (NO) cycling conditions. The dynamic behavior of these systems is analyzed using a synchronous, time-resolved energy dispersive X-ray absorption spectroscopy (XAS), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and mass spectrometry (MS) set-up with subsecond time resolution. Two main physico-chemical phenomena corresponding to noble metal morphological (size/shape) changes and the redox behavior of the noble metal–promoter interface are shown to control the TWC response to NO/CO cycling conditions. Metal-only aspects strongly influence N–O dissociation and N–N coupling steps while the metal–promoter interface has a global influence on both N₂ and CO₂ formation via oxygen handling (storage/release) properties. The relative importance of these two phenomena is studied as a function of the Ce_0.5Zr_0.5O₂ promoter content of the catalysts.     

A novel disubstituted Lindqvist-type polyoxomolybdate [Te2Mo4O19] supporting two organic vanadyl moieties: Synthesis, characterization, and crystal structure of {[V(2,2-bipy)2]2(4,4-bipy)[Te2Mo4O19]}

The first example of disubstituted Lindqvist-type polyoxomolybdate {[V(2,2-bipy)₂]₂(4,4-bipy)[Te₂Mo₄O₁₉]} has been synthesized hydrothermally and characterized by elemental analyses, XPS, IR, TG-DTA and X-ray single crystal diffraction. The structural analysis shows that the neutral molecular unit [V(2,2-bipy)₂]₂[Te₂Mo₄O₁₉] consists of a novel Lindqvist-type polyanion [Te₂Mo₄O₁₉]⁶⁻ supporting two vanadyl moieties [V(2,2-bipy)₂]³⁺, and such neutral molecules are joined together by π − π stacking interactions between the pyridine groups to form a two-dimensional grid-like network with non-coordinating “guest” 4,4-bipys encapsulated.