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.

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.

SYNTHESIS AND X-RAY CRYSTAL-STRUCTURE OF AN ORGANOLANTHANIDE COMPLEX [(BU(T)CP)3NDBRLI(THF)3]

(ButCp)2NdCl.2THF reacts with one equivalent of phenyllithum in THF yielding tris(tert-butylcyclopentadienyl)neodymium lithium bromide tetrahydrofuran, [(ButCP)3 NdBrLi(THF)3], as a by-product, whose structure has been determined by X-ray crystallography. The 10-coordinated neodymium atom is bonded to three tert-butyl-cyclopentadienyl groups and one bromine atom, forming a distorted pseudo-tetrahedron.

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.

SYNTHESIS, THERMAL-STABILITY AND X-RAY CRYSTAL-STRUCTURE OF THE BIS(CYCLOPENTADIENYL)YTTERBIUM NAPHTHOXIDE DERIVATIVE (C5H5)2YB(OC10H7)(THF)

Cp3Yb (Cp = C5H5) reacts with a-naphthol (HNP) in THF to form Cp2Yb(NP)(THF) (1), which crystallizes in the space group P2(1)/n with unit cell dimensions a = 8.084(2), b = 15.996(6), c = 15.973(7) angstrom, beta = 98.95(3), V = 2040.3 angstrom and D(calc.) = 1.69 g cm-3 for Z = 4. Least-squares refinement based on 2242 observed reflections converged to a final R value of 0.081. The average Yb-C(Cp) distance is 2.60(2) angstrom and Yb-O(THF) and Yb-O(NP) distances are 2.30(1) and 2.06(1) angstrom, respectively. The title compound loses the coordinated THF molecule readily by heating under vacuum to give dimeric [Cp2Yb(NP)]2 (2), which undergoes disproportionation to give Cp3Yb and Yb(NP)3 on heating above 230-degrees-C.

STRUCTURE-ANALYSIS OF MOLTEN CACL2-KCL SYSTEM BY X-RAY-DIFFRACTION

Radial distribution function of CaCl2-KCl (1:2 mol) melt was measured by X-ray scattering of high temperature liquid. The nearest neighbour distances of Ca2+-Cl-, K+-Cl- and Cl--Cl- ionic pairs are 0.278, 0.306 and 0.380 nm, respectively, Discussion on the relation between structure and physicochemical properties in the melt was simply done in this paper.

SYNTHESIS AND X-RAY CRYSTAL-STRUCTURE OF [EU(ETA-6-C6ME6)(ALCL4)2]4 - THE 1ST CYCLOTETRAMERIC LANTHANIDE(II) COMPLEX WITH A NEUTRAL PI-LIGAND

The reaction of EuCl3, AlCl3 and C6Me6 in toluene gives the Eu(II) complex [Eu(eta-6-C6Me6)(AlCl4)2]4; X-ray crystal determination shows the molecule to be a cyclotetramer, in which the four Eu(C6Me6)AlCl4 units are connected via four groups of eta-2-AlCl4.

SYNTHESIS AND X-RAY CRYSTAL-STRUCTURE OF SM(C8H8)(2,4-C7H11).THF

SmCl3 reacts with K2C8H8 to yield the complex Sm(C8H8)Cl.2thf, which reacts with K(2,4-C7H11) (2,4-C7H11 = 2,4-dimethylcyclopentadienyl) to form Sm(C8H8)(2,4-C7H11).thf; the X-ray crystal structure of Sm(C8H8)(2,4-C7H11).thf shows that the 2,4-dimethylcyclopentadienyl has a 'U' conformation.

FACTOR-ANALYSIS APPLIED TO X-RAY-DIFFRACTION DIAGRAMS OF POLYMER BLENDS

The feasibility of applying the method of factor analysis to X-ray diffraction diagrams of binary blends of polypropylene and ethylene-propylene-diene terpolymer (PP/EPDM) was examined. The result of mathematical treatment was satisfactory. The number of scattering species and their concentrations in six kinds of PP/EPDM blends were determined. The separation of the spectral peaks of each species in the blends, contributing spectral intensities, was carried out.

SYNTHESIS AND X-RAY CRYSTAL-STRUCTURE OF A MONOPENTAMETHYLCYCLOPENTADIENYL DERIVATIVE OF GADOLINIUM (NA(MU-2-THF)[(C5ME5)GD(THF)]2(MU-2-CL)3(MU-3-CL)2)2.6THF

The reaction of GdCl3 with 1 equiv of NaC5Me5 generates a neutral complex C5Me5GdCl2(THF)3 and a novel complex {Na(mu-2-THF)[(C5Me5)Gd(THF)]2(mu-2-Cl)3(mu-3-Cl)2}2.6THF whixh recrystallizes from THF in triclinic, the space group P1BAR with unit cell dimentions of a 12.183(4), b 13.638(6), c 17.883(7) angstrom, alpha-110.38(3), beta-94.04(3), gamma-99.44(3)-degrees, V 2721.20 angstrom-3 and D(calc) 1.43 g cm-3 for Z = 1. Least-squares refinement of 2170 observed reflections led to a final R value of 0.047. The title complex consists of two Na(mu-2-THF)[(C5Me5)Gd(THF)]2(mu-3-Cl)3(mu-3-Cl)2 units bridged together via two mu-2-THF to Na coordination. Each Gd ion is surrounded by one C5Me5 ligand, two mu-3-Cl, two mu-2-Cl and one THF in a distorted octahedral arrangement with average Gd-C(ring) 2.686(33), Gd-mu-2-Cl 2.724(7), Gd-mu-3-Cl 2.832(8) and Gd-O 2.407(11) angstrom. The sodium ion coordinates to two bridging THF, two mu-2-Cl and two mu-3-Cl to form a distorted octahedron with average Na-mu-2-O, Na-mu-2-Cl and Na-mu-3-Cl of 2.411(21), 2.807(15) and 2.845(12) angstrom, respectively.

The magnetic structure of a coronal X-ray bright point

Brown, D.S., Parnell, C.E., Deluca, E., McMullen, R. and Golub, L., 2001, The magnetic structure of a coronal X-ray bright point, Solar Physics, 201, 305-321.