Small angle X-ray scattering study of structural parameters of the aggregated state in polyamide 1010+BMI

The structural parameters of the aggregated state in the polyamide PA1010 and N,N'-bismaleimide-4,4'-diphenyl methane (BMI) system were computed by means of the desmearing intensity from SAXS and using the concept of the distance distribution function. The results revealed that the parameters Q, I(0), l(c) and L decreased with the increase BMI component, whereas O-s increased. The particle dimension Z for different BMI contents was less than 13.2 nm, and the maximum value of the distance distribution function P(Z) was found to be in the range Z = 6.5-7.0 nm.

APPLICATION OF THE MOMENT METHODS TO ANALYSIS OF X-RAY-DIFFRACTION LINE-PROFILE FOR PA1010-BMI SYSTEM

Pure X-ray diffraction profiles have been analysed for polyamide 1010 and PA1O1O-BMI system by means of multipeak fitting resolution of X-ray diffraction. The methods of variance and fourth moment have been applied to determine the particle size and strain values for the paracrystalline materials. The results indicated that both variance and fourth moment of X-ray diffraction line profile yielded approximately the same values of the particle size and the strain. The particle sizes of (100) reflection have been found to decrease with increasing BMI content, whereas the strain values increased.

COMPARATIVE-STUDIES ON PERIODATOCUPRATE(II, III) AND TELLURATOCUPRATE(II, III)

The crystal structures, electronic spectra, and Cu2p XPS of Cu(III) complexes Na4H[Cu(H2TeO6)(2)]. 17H(2)O and Na4K[Cu(HlO(6))(2)]. 12H(2)O have been described. The characterizations of a Cu(III) atom in a complex are as follows: (i) In a square-planar coordination, the average bond length of Cu-O is 0.183 nm, shorter than the 0.190-0.200 nm found for a Cu(II) complex. (2) The ''blue shift'' occurs for d-d transitions in the electronic spectrum of the Cu(III) complex compared to those of its related Cu(II) complex, resulting from the higher valence state. (3) Cu(III) compounds with CuO4 square-planar coordination are expected to be diamagnetic whereas Cu(II) compounds to be paramagnetic. (4) Comprehensive investigations on Cu2p XPS show that the binding energy of Cu2p(3/2) of a pure Cu(III) compound is about 2.0 eV higher than that of its corresponding Cu(II) compound: the shake-up satellites do not appear in the Cu2p XPS for a pure diamagnetic Cu(III) compound, the same as found for a diamagnetic Ni(II) compound: the FWHM of the signal of Cu2p XPS may become broader for Cu(III) compound because its core hole's lifetime shortens due to the higher valence state of copper. (C) 1995 Academic Press, Inc.

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.

SYNTHESIS, SOLUTION DYNAMICS AND X-RAY CRYSTAL-STRUCTURES OF NEODYMIUM-YLIDE COMPLEXES, [(C(5)H(4)R)(3)NDCH2P(ME)PH(2)] (R=H, BU(T))

The interaction of [(C(5)H(4)R)(2)NdCl.2LiCl] (R = H, Bu(t)) with one equivalent of Li[(CH2)(CH2)PPh(2)] in refluxing tetrahydrofuran gave the purplish-blue complex [(C(5)H(4)R)(3)NdCH2P(Me)Ph(2)] in 50% yield. The compounds have been fully characterized by analytical, spectroscopic and X-ray diffraction methods. Variable temperature P-31{H-1} NMR spectroscopy indicated the existence of the following equilibrium: [(C(5)H(4)R)(3)NdCH2P(Me)Ph(2)] + THF reversible arrow (C(5)H(4)R)(3)Nd(THF) + CH2=P(Me)Ph(2). At room temperature, the exchange between the coordinated and free ylide ligand is slow on the NMR time scale.

SYNTHESIS AND X-RAY STRUCTURE OF AN ORGANOLANTHANUM COMPLEX [(BUTCP)3LACLLI(THF)3]

LaCl3.2LiCl reacts with two equivalents of Bu(t)CpNa in THF to give the complex [(Bu(t)Cp)3LaClLi(THF)3]. The crystal structure was determined by X-ray diffraction at room temperature. Two units, (Bu(t)Cp)3La and Li(THF)3, are connected by a single chlo

SMALL-ANGLE X-RAY-SCATTERING STUDY ON THE INTERFACE IN BLOCK-COPOLYMERS WITH FRACTAL PROPERTIES

The interface thickness in two triblock copolymers were determined using small-angle x-ray scattering in the context of the theory proposed by Ruland. The thickness was found to be nonexistent for the samples at three different temperatures. By viewing th

A NEW METHOD FOR THE SYNTHESIS OF LN(ETA-6-C6ME6)(ALCL4)3 (LN=ND, SM, GD, YB), AND THE X-RAY CRYSTAL-STRUCTURE OF YB(ETA-6-C6ME6)(ALCL4)3.MEC6H5

A series of neutral eta6-C6Me6 complexes of lanthanide elements Ln(176-C6Me6)(AlCl4)3 . MeC6H5(Ln = Nd, Sm, Gd, Yb) has been prepared directly in good yields from the reaction of LnCl3, AlCl3 and C6Me6 in toluene. The complexes have been characte

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 X-RAY CRYSTAL-STRUCTURE OF THE SM-YLIDE COMPLEX, [(C5H5)3SMCH2P(ME)PH2]

The interaction of (C5H5)2SmCl.LiCl with one equivalent of Li[(CH2)(CH2) PPh2] in refluxing tetrahydrofuran gives the yellow complex [(C5H5)3SmCH2P (Me)Ph2] in 30% yield. The compound has been fully characterized by analytical, spectroscopic and X-ray diffraction methods.

DEHYDROGENATION OF ORGANOLANTHANIDE ALKOXIDES AND X-RAY CRYSTAL-STRUCTURE OF REACTION-PRODUCT [(C5H-5)2YB(MU-OCH=C=CH2)]2

[Cp3Yb] reacts with HOR (Cp = C5H5; R = CH2CH=CH2, CH2CH2Me) in thf (thf = tetrahydrofuran)at room temperature to give complexes [{Cp2Yb(mu-OR)}2], which are dehydrogenated to yield the new complex [{Cp2Yb(mu-OCH=C=CH2)}2] in refluxing thf solution; the X-ray crystal structure shows that the new complex is dimeric with oxygen atoms as bridging groups.

HIGH-TEMPERATURE SUPERCONDUCTOR, YBA2CU3O7-X AS ALL-SOLID-STATE LITHIUM CELL

The utility of the high-temperature superconductor, YBa2Cu3O7-x as the cathode material for an all-solid-state lithium cell has been examined. The capacity of YBa2Cu3O7-x is 223 mA h g-1 and the discharge efficiency is > 92%. Measurements of a.c. impedance show that the charge-transfer resistance at the interface of the electrolyte/cathode is very low and increases with the depth-of-discharge of the battery. Studies using X-ray photoelectron spectroscopy (XPS) reveal that the cathode becomes doped with Li+ ions as the cell discharges.

SYNTHESES AND X-RAY STRUCTURES OF BIS(T-BUTYLCYCLOPENTADIENYL)LANTHANIDE CHLORIDE COMPLEXES [(BU(T)CP)2LNCL]2 (LN = PR, GD, ER)

Reaction of lanthanide trichlorides with two equivalents of sodium t-butylcyclopentadienide in THF gave rise to the bis(t-butylcyclopentadienyl)lanthanide chloride complexes [(Bu(t)Cp)2LnCl]2 (Ln = Pr, Gd, Er), which were characterized by elemental analysis, IR and H-1 NMR spectroscopy. In addition, the crystal structures of [(ButCp)2PrCl]2 (1) and [(ButCp)2GdCl]2 (2) were determined by single crystal X-ray diffraction at room temperature. The coordination number for Pr3+ and Gd3+ is 8 and the bond lengths Pr-Cl and Gd-Cl are 2.864(2) and 2.771(3) angstrom, respectively. The structural studies showed the complexes to have C2h symmetry.