Isolation and X-ray crystallographic structure of cyclic tetramer based on bisphenol A and o-phthaloyl dichloride

The polycrystalline powder of the cyclic tetramer based on bisphenol A and o-phthaloyldichloride has been prepared by recrystallization from nitrobenzene and its crystal structure has been determined by Wide-Angle X-ray Diffraction (WAXD). The unit cell is orthorhombic and its dimensions a = 0.967 6 nm, b = 0.869 9 nm, c = 2.085 9 nm, Space group belongs to Pmmm, With two tetramers per unit cell,the crystal density is 1.36 g . cm(-3), Indices of crystal diffraction peaks are also detailed in the present work.

X-ray crystallographic structure of cyclic tetramer ester based on bisphenol-A and o-phthaloyldichloride

The polycrystalline powder of the cyclic tetramer ester based on bisphenol-A and o-phthaloyldichloride has been prepared by recrystallization from nitrobenzene and its crystal structure determined by wide-angle X-ray diffraction. The unit cell is orthorhombic and has dimensions a=0.967 nm, b=0.8699 nm, c = 2.0859 nm. With two tetramers per unit cell, the crystal density is 1.36 g cm(-3). Indices of crystal diffraction peaks are also detailed in the present work. Copyright (C) 1996 Elsevier Science Ltd.

Studies on organolanthanide complexes .58. Syntheses of 1,1'-(3-oxa-pentamethylene)dicyclopentadienyl divalent organolanthanides (Ln=Sm, Yb) and X-ray molecular structure of O(CH2CH2C5H4)(2)Yb(DME)

The compounds O(CH2CH2C5H4)(2)Ln(THF)(2) [Ln = Sm(1), Yb(2)] were synthesized by the reduction of O(CH2CH2C5H4)(2)LnCl with sodium metal in tetrahydrofuran (THF) at room temperature. Recrystallization of 2 from dimethoxyethane (DME) produced the single-crystal O(CH2CH2C5H4)(2)Yb(DME) (3) whose structure has been determined by an X-ray diffraction study. The crystals are orthorhombic, space group Pcab, with a = 14.168(4), b = 13.541(6), c = 19.314(8) Angstrom, Z = 8, D-calc. = 1.66 g cm(-3).

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.

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.

X-Ray Photoelectron Spectroscopy Study of LaMn1-xFexO3 (x=0-1) Oxides

The redox potential, surface composition and oxygen species of a series of complex oxides LaMn1-xFexO3 (x=0-1) having perovskite structure (ABO(3)) have been investigated by means of XI'S. The variation of binding energies referring to Mn2p and Fe 2p under different treatment offerred an obvious evidence of redox between Mn and Fe, which could be expressed as Mn4+ + Fe(3-delta)+ Mn(4-delta)+ Fe3+ Feat Through computer fit three kinds of adsorbed oxygen species (O-I, O-II, O-III) have been evaluated based on the XPS spectra of O1s. From the variation of contents of different oxygen species, it could be concluded that. the redox occuring in the surface might be related with the adsorbed oxygen species O-I and O-II, furthermore the possibility of transfer of electron between adsorption site and oxygen was also discussed.

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

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.

X-RAY PHOTOELECTRON-SPECTRA OF SOME BIOINORGANIC COMPLEXES OF THE RARE-EARTHS WITH N-ACETYLALANINE

X-Ray photoelectron spectra of some bioinorganic complexes of La, Ce, PT, Nd, Sm and Eu with N-acetylalanine have been measured and the 3d5/2 and 3d3/2 main peaks and their satellites have also been assigned. ne spin-orbit splitting between the 3d5/2 and 3d3/2 core-level of the rare earth ion in these complexes becomes slightly larger than that of the free rare earth atom due to the effect of the crystal field. The satellite for the 3d main peaks of La in the solid state complex are in higher binding energy region and may be attributable to the L --> 4f charge-transfer shake-up process. The satellites for the 3d main peaks of Ce, Pr, Nd, Sm and Eu are in the lower binding energy region and may be attributable to the 4f --> L charge-transfer shake-down process.