Synthesis of Lanthanoid Complexes from Ln2O3 and Diatrizoic Acid

2018 ◽  
Vol 71 (12) ◽  
pp. 939
Author(s):  
Guillaume Bousrez ◽  
Philip C. Andrews ◽  
Peter C. Junk ◽  
Dominique T. Thielemann ◽  
Jun Wang
Keyword(s):  
Crystal Structures ◽  
Room Temperature ◽  
Direct Interaction ◽  
Unit Cell ◽  
Metal Centre ◽  
X Ray ◽  
Triiodobenzoic Acid ◽  
Solvent Molecules ◽  
Cell Data ◽  
Unit Cell Data

We present a pathway to synthesize diatrizoate lanthanoid complexes directly from Ln2O3 and diatrizoic acid (DTAH=3,5-diacetamido-2,4,6-triiodobenzoic acid) at room temperature yielding [Ln(H2O)8][DTA]3 in moderate (for the heavier lanthanoids) to good (for the lighter lanthanoids) yields. Compounds were recrystallized from DMSO or water and their X-ray crystal structures were obtained. The complexes have metal centres solely coordinated by solvent molecules with no direct interaction between the metal centre and the DTA anion. The compounds crystallized from DMSO have the formulation [Ln(DMSO)4(H2O)4][DTA]3.DMSO (Ln=La, Nd, Sm, Eu, Dy; only unit cell data were confirmed for Ln=Nd, Sm) whereas the compound crystallized from water has the formulation [Dy(H2O)8][DTA]3.7H2O.

Structural and vibrational studies of 1,1,3,3-tetracyanopropane and 2,2,4,4,6-pentacyanocyclohexenamine

1987 ◽  
Vol 65 (2) ◽  
pp. 261-270 ◽  
Author(s):  
R. A. Bell ◽  
B. E. Brown ◽  
M. Duarte ◽  
H. E. Howard-Lock ◽  
C. J. L. Lock
Keyword(s):  
Unit Cell ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
New Methods ◽  
Cell Dimensions ◽  
Cell Data ◽  
Unit Cell Data ◽  
Monoclinic Cell ◽  
C Nmr

1,1,3,3-Tetracyanopropane, 1, was prepared in low yields by a literature method with 2,2,4,4,6-pentacyanocyclohexenamine, 2, as a major by-product. The products were examined by X-ray crystallography. 1 has an orthorhombic space group, Pbcn (No. 60) with cell dimensions, a = 7.158(2), b = 10.510(3), c = 9.733(2) Å and has four formula units in the unit cell. 2 has a monoclinic cell, P21/c (No. 14) with cell dimensions a = 14.368(3), b = 6.626(1), c = 12.300(2) Å, β = 115.60(1)° and has 4 formula units in the unit cell. Data were collected with use of MoKα radiation and a Nicolet P3 diffractometer. The crystal structures were determined by standard methods and refined to Rw = 0.037 (1) and Rw = 0.040 (2) on the basis of 782 and 2108 unique reflections. Bond lengths and angles in the two compounds are normal. 2 has what has been considered to be the less likely tautomeric structure. Both compounds were examined by 1H, 13C nmr, vibrational spectroscopy, and mass spectroscopy. For 2 there was no evidence of the alternative tautomeric structure. New methods were developed for the preparation of both compounds and the mechanism of the original reaction rationalized.

Barium Rare Earth Titanates: X-Ray Characterization of BaR2Ti3O10 and BaR2Ti4O12: R = Lanthanide

1992 ◽  
Vol 7 (3) ◽  
pp. 176-178 ◽  
Author(s):  
X. Jing ◽  
C. Zheng ◽  
A.R. West
Keyword(s):  
Rare Earth ◽  
Solid State ◽  
Unit Cell ◽  
Lanthanide Ion ◽  
X Ray ◽  
Ion Size ◽  
Cell Data ◽  
Unit Cell Data ◽  
Cell Volumes

AbstractThe compounds, BaR2Ti3O10: R = La, Pr, Nd and Sm; BaR2Ti4O12: R = La, Pr, Sm, Gd, Eu have been prepared by solid state reaction and characterized by X-ray powder diffraction. Unit cell data are summarised; lattice parameters and unit cell volumes increase approximately linearly with lanthanide ion size.

Aegirine of possible authigenic origin in Middle Devonian sediments in Caithness, Scotland

1978 ◽  
Vol 42 (324) ◽  
pp. 439-442 ◽  
Author(s):  
N. J. Fortey ◽  
U. McL. Michie
Keyword(s):  
River Basin ◽  
Middle Devonian ◽  
Unit Cell ◽  
Green River Formation ◽  
Green River Basin ◽  
Green River ◽  
X Ray ◽  
Orcadian Basin ◽  
Cell Data ◽  
Unit Cell Data

SummaryAn occurrence of aegirine in Middle Devonian lacustrine beds in Caithness is described. The mineral occurs as euhedral to subhedral prismatic crystals within a finely laminated siltstone. Microprobe analyses reveal a remarkably ‘pure’ composition consisting almost entirely of Na, Fe3+, Si, and O. X-ray diffractometry yielded the unit cell data: a 9·657 Å, b 8·800 Å, c 5·296 Å, and β 107·37°. Comparison with other natural aegirine compositions shows marked differences from those of igneous or metamorphic origin but a close similarity to a unique occurrence of authigenic aegirine in the lacustrine Green River Formation of Wyoming, U.S.A. Consideration of the nature of the Caithness occurrence, and comparison of the Devonian Orcadian basin with the Eocene Green River basin indicate similar geological environments. It is suggested that the mineral formed in hypersaline conditions in which sodium may have been derived from contemporaneous alkaline volcanism within the Orcadian basin.

X-Ray structure of tris(acetonitrile)tricarbonylrhenium(I) tetrafluoroborate

1977 ◽  
Vol 55 (1) ◽  
pp. 111-114 ◽  
Author(s):  
Lillian Y. Y. Chan ◽  
E. E. Isaacs ◽  
W. A. G. Graham
Keyword(s):  
Least Squares ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
The Mean ◽  
Unit Cell Dimensions ◽  
Cell Data ◽  
Unit Cell Data

Reaction of [n-Bu4N]2[Re4(CO)16] with AgBF4 in acetonitrile affords the compound [(CH3CN)3Re(CO)3][BF4]. The latter crystallizes in monoclinic space group P21/c with unit cell dimensions a = 11.021(5) Å, b = 11.136(5) Å, c = 12.980(6) Å, β = 96.906(25)°, and four molecules per unit cell. Data were collected by counter methods and the structure was refined using least-squares procedures to give R = 0.041. The rhenium cation is approximately octahedrally coordinated by six facially arranged ligands. The mean rhenium–nitrogen distance is 2.13 Å, and the mean rhenium–nitrogen–carbon angle in the coordinated acetonitrile is 174.7°.

X-ray study on egg-yolk lecithin: Unit cell data and electron density profile

1977 ◽  
Vol 117 (1) ◽  
pp. 285-291 ◽  
Author(s):  
I. Sakurai ◽  
S. Iwayanagi ◽  
T. Sakurai ◽  
T. Seto
Keyword(s):  
Electron Density ◽  
Density Profile ◽  
Egg Yolk ◽  
Electron Density Profile ◽  
Unit Cell ◽  
X Ray ◽  
Cell Data ◽  
Unit Cell Data

Unit cell data of serpentine group minerals

1981 ◽  
Vol 44 (334) ◽  
pp. 153-156 ◽  
Author(s):  
Peter Bayliss
Keyword(s):  
Least Squares ◽  
Diffraction Data ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
X Ray ◽  
Unit Cells ◽  
Cell Data ◽  
Unit Cell Data ◽  
Varietal Name

AbstractLeast-squares analyses of powder X-ray diffraction data have been undertaken for minerals and synthetics of composition (Mg,Mn,Fe,Co,Ni)3−xSi2O5 (OH)4. New polytypes of nepouite and greenalite have been established, and eleven new or altered unit cells have been calculated. Baumite is an unnecessary varietal name for a manganoan ferroan lizardite-1T; tosalite is an unnecessary varietal name for a manganoan greenalite; clinochrysotile is an unnecessary polytype name for chrysotile-2Mc1; orthochrysotile is an unnecessary polytype name for chrysotile-2Orc1; ortho-antigorite and ortho-hexagonal serpentine are unnecessary names for lizardite-6T1; and septechlorite should not be used. The powder data of the serpentine group are in general, poor.

Taneyamalite, (Na,Ca)(Mn2+,Mg,Fe3+,Al)12Si12 (O,OH)44, a new mineral from the Iwaizawa mine, Saitama Prefecture, Japan

1981 ◽  
Vol 44 (333) ◽  
pp. 51-53 ◽  
Author(s):  
Satoshi Matsubara
Keyword(s):  
Empirical Formula ◽  
Unit Cell ◽  
Refractive Indices ◽  
New Mineral ◽  
Manganese Ore ◽  
Ore Deposit ◽  
X Ray ◽  
Light Yellow ◽  
Cell Data ◽  
Unit Cell Data

AbstractTaneyamalite, (Na,Ca)(Mn2+,Mg,Fe3+,Al)12 Si12(O,OH)44, is a Mn2+-dominant analogue of howieite, and has been found in the metamorphosed bedded manganese ore deposit of the lwaizawa mine, Saitama Prefecture, Japan. It is triclinic, P1 or P, a 10.198(1), b 9.820(1), c 9.485(1) Å, α 90° 30(1)′, β 70° 32(1)′, γ 108° 34(1)′, Z = 1. The strongest X-ray powder diffractions are: 9.29(80)010, 7.99(35)10, 4.62(50)020, 3.65(40)120, 3.273(100)30, 3.081(50)11, 2.790(35)31, 2.630(28)023, 2.216(35)014, 43. Taneyamalite occurs in association with minor bannisterite as small seams in a caryopilite mass or as a fissure mineral cutting a hematite-quartz mass. It is greenish grey-yellow, lustre vitreous. Streak light yellow. Cleavage {010}, perfect. H. (Mohs) about 5. Calculated sp. gr. 3.30 (on unit cell data and normalized empirical formula), 3.25 (after the Gladstone-Dale Law using the revised data of Mandarino, 1976). It is optically biaxial negative, 2Vα about 70°. The refractive indices: α = 1.646(2), β = 1.664(2), γ = 1.676(2). Extinction is nearly parallel, sign of elongation positive. Pleochroism distinct: α = β nearly colourless, γ pale yellow. Absorption: α ≈ β < γ.

The crystal structures of Cu1•8Se, Cu3Se2, α- and γCuSe, CuSe2, and CuSe2II

1976 ◽  
Vol 54 (6) ◽  
pp. 841-848 ◽  
Author(s):  
Robert Donald Heyding ◽  
Ritchie MacLaren Murray
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Unit Cell ◽  
Intensity Data ◽  
Diffraction Intensity ◽  
Space Group ◽  
X Ray ◽  
Model Based ◽  
Tetrahedral Sites

The crystal structures of a number of copper selenides have been re-examined using X-ray powder diffraction intensity data. |F0| values for Cu1•8Se at room temperature (a = 5.765 Å) are satisfied by a model based on space group Fm3m with 4 Se atoms per unit cell on the fcc sites, 5.2 Cu atoms on the tetrahedral sites, and 2.0 Cu atoms on the trigonal sites in the Se sublattice. Cu3Se2 is tetragonal, [Formula: see text] a = 6.402, c = 4.279 Å, with Cu(1) in 2(a), Cu(2) in 4(e) with x = 0.147 ± 5, z = 0.781 ± 9, and Se in 4(e) with x = 0.272 ± 3, z = 0.264 ± 7. CuSe2 has the orthorhombic C18 marcasite structure, Pnnm, a = 5.005, b = 6.182, c = 3.740 Å, with Cu in 2(a), and Se in 4(g) with x = 0.184 ± 1, y = 0.385 ± 1. CuSe2II has the cubic C2 pyrite structure, Pa3, a = 6.116 Å, with Cu in 4(a), and Se in 8(c) with x = 0.3891 ± 5.Neither αCuSe nor γCuSe have the CuS covellite structure.These results are discussed in some detail.

The use of Buerger's algorithm in crystallographic calculations

1961 ◽  
Vol 32 (253) ◽  
pp. 817-822 ◽  
Author(s):  
R. J. Davis
Keyword(s):  
Calculation Method ◽  
Worked Examples ◽  
Transformation Matrix ◽  
Unit Cell ◽  
X Ray ◽  
Cell Data ◽  
Unit Cell Data

SummaryBuerger (Zeits. Krist., 1957, vol. 109, p. 42) describes an algorithm for deriving data for the reduced unit cell from those obtained for an arbitrary crystal setting. It is shown that indices can be added to the algorithm so that one also derives the transformation matrix for the change of setting. Conversely, a known transformation matrix forms a set of instructions for using the algorithm to transform unit cell data, whether X-ray or morphological, from the initial to the final setting, One can thus use the algorithm to calculate the lengths of any unit cell vectors and the angles between them, and, using reciprocal cell data, to obtain any interfacial angles. Worked examples of these applications show that the proposed calculation method is shorter and simpler than those at present accepted.

Dwornikite, (Ni,Fe)SO4 · H2O, a member of the kieserite group from Minasragra, Peru

1982 ◽  
Vol 46 (340) ◽  
pp. 351-355 ◽  
Author(s):  
Charles Milton ◽  
Howard T. Evans ◽  
Robert G. Johnson
Keyword(s):  
Unit Cell ◽  
Oxidation Products ◽  
Powder Pattern ◽  
Space Group ◽  
X Ray ◽  
Fine Grained ◽  
Sulphide Ores ◽  
Cell Data ◽  
Unit Cell Data

AbstractDwornikite, (Ni1−xFex)SO4 · H2O is a member of the kieserite group, monoclinic with space group C2/c. Specimens from Minasragra, Peru with x ∼ 0.1 have a unit cell with a = 6.839(2), b = 7.582(2), c = 7.474(2) Å, and β = 117.85(2)°. The six strongest lines of the powder pattern are: 3.342 (12, 100), 4.732 (110, 70), 3.024 (200, 70), 4.754 (11, 50), 3.293 (021, 35), 2.491 (022, 35). The mineral occurs as fine grained white aggregates associated with vanadium sulphide ores containing patronite and bravoite, mixed with other oxidation products. New unit cell data for the synthetic end-member compounds NiSO4 · H2O and FeSO4 · H2O, and new X-ray powder data for retgersite (NiSO4 · 6H2O) are provided.

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