Lanthanide Ion Complexes of Calixarenes. VIII. Bimetallic Lanthanide Complexes of p-t-Butylcalix[8]arene From Dimethylformamide Solutions

1991 ◽  
Vol 44 (9) ◽  
pp. 1249 ◽  
Author(s):  
JM Harrowfield ◽  
MI Ogden ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Lanthanide Complexes ◽  
Complex Molecule ◽  
Lanthanide Ion ◽  
X Ray

Reaction of lanthanide(III) ion p- toluenesulfonates with a warm p-t- butylcalix [8] arene (L) solution in dmf/triethylamine ( dmf denotes N,N- dimethylformamide ), yields crystalline 2 : 1 Ln/ligand adducts, as dmf solvates: [Ln2(L-6H)( dmf )5]. xdmf , Ln = La, Pr, Lu and Eu (previously recorded; 2 phases) have been characterized by single-crystal X-ray studies; all phases are triclinic but only the praseodymium and α-form of the europium derivative are isostructural : Ln = La, Pr, α- Eu have Z = 2 formula units, while Ln = β- Eu , Lu have Z = 4. In all cases, the stoichiometry of the complex molecule is the same and the same as that of the dmso adducts recorded in the previous paper, with similar ligand dispositions.

Lanthanide Ion Complexes of Calixarenes. VII. Bimetallic Lanthanide Complexes of p-t-Butylcalix[8]arene From Dimethyl Sulfoxide Solutions

1991 ◽  
Vol 44 (9) ◽  
pp. 1237 ◽  
Author(s):  
JM Harrowfield ◽  
MI Ogden ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Dimethyl Sulfoxide ◽  
Lanthanide Complexes ◽  
Complex Molecule ◽  
Asymmetric Unit ◽  
Lanthanide Ion ◽  
X Ray ◽  
Twofold Axis ◽  
Lanthanide Atoms ◽  
Similar Complex

Reaction of Ln (ClO4)3.x dmso ( dmso denotes dimethyl sulfoxide ) with a warm p-t- butylcalix [8] arene (L) slurry in acetone/ dmso yields crystalline 2:1 Ln/ligand adducts, characterized as dmso olvates and established to be [Ln2(L-6H)( dmso )5].~2dmso by single- crystal X-ray studies at c. 295 K for Ln = La, Eu , Tm and Lu. All complexes are isomorphous , orthorhombic, Pcnb, a ≈ 34, b ≈ 23, c ≈ 14 Ǻ, Z 4, with a similar complex molecule in each case, one half comprising the asymmetric unit; the second half is generated by a crystallographic twofold axis. The two lanthanide atoms are encompassed by the macrocycle and are eight coordinate, involving phenolic and dmso O-donor atoms, five of the former (two bridging) and three of the latter (one bridging). The array closely resembles that found in analogous dmf solvent adducts: the bridging dmso lies on the crystallographic twofold axis through the complex, its peripheral atoms being modelled by disorder.

On Attempts to Synthesize Lanthanide Complexes of the Dianionic Fluorenyl-alkoxo Ligand [C13H8-cyclo-C6H10-O]2-. Crystal Structure of (C13H9-cyclo-C6H10-O)LaI2(DME)2

2003 ◽  
Vol 58 (5) ◽  
pp. 389-394 ◽  
Author(s):  
Alexander A. Trifonov ◽  
Mikhail N. Bochkarev ◽  
Herbert Schumann ◽  
Sebastian Dechert
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Ir Spectra ◽  
Single Crystal ◽  
Lanthanide Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Elemental Analyses ◽  
C Nmr

Racemic trans-2-(9(H)-fluoren-9-yl)cyclohexanol, C13H9-cyclo-C6H10-OH (1), reacts with two equivalents of potassium naphthalenide in THF to give the dipotassium salt [C13H8-cyclo-C6H10-O]- K2(THF) (2). Recrystallization of 2 from pyridine affords the solvent free salt [C13H8-cyclo-C6H10- O]K2 (3). The reactions of LaI3(THF)4 with one equivalent of 2 or of YbI2(THF)2 with equimolar amounts of 2 produce the alkoxolanthanum diiodide (C13H9-cyclo-C6H10-O)LaI2(DME)2 (4) and the ytterbium dialkoxide (C13H9-cyclo-C6H10-O)2Yb(THF)0.5(5), respectively. [(Me3Si)2N]3Y reacts with three equivalents of 1 with elimination of hexamethyldisilazane and formation of the yttrium trialkoxide (C13H9-cyclo-C6H10-O)3Y (6). The compounds 2 to 5 were characterized by elemental analyses, 1H NMR, 13C NMR and IR spectra. The molecular structure of 4 was determined by single crystal X-ray diffraction.

Crystal structure of Bis(N,N-diethyldithiocarbamato)(isothiocyanato)iron(III)

1980 ◽  
Vol 33 (1) ◽  
pp. 221 ◽  
Author(s):  
CL Raston ◽  
WG Sly ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Single Crystal ◽  
Iron Atom ◽  
Title Compound ◽  
Complex Molecule ◽  
X Ray Diffraction ◽  
X Ray

The crystal structure of the title compound [Fe(NCS)(S2CNEt2)2] has been determined by single-crystal X-ray diffraction methods at 295(1) K and refined to a residual of 0.054 for 998 'observed' reflections. Crystals are orthorhombic, P212121, with a 18.70(2), b 15.43(2), c 6.667(6)Ǻ, Z 4. The iron atom of the complex molecule [Fe(NCS)(S2CNEt2)2] is five- coordinated, being bonded by four sulfur atoms [Fe-S, 2.257-2.300(5) Ǻ] and the nitrogen atom of the thiocyanate [Fe-N, 1.91(2)Ǻ].

Electron Microscopy of Shock Loaded Polycrystalline Beryllium

1974 ◽  
Vol 32 ◽  
pp. 506-507 ◽  
Author(s):  
J. M. Galbraith ◽  
L. E. Murr ◽  
A. L. Stevens
Keyword(s):  
Electron Microscopy ◽  
Wave Propagation ◽  
Structural Change ◽  
Single Crystal ◽  
Diffraction Pattern ◽  
Shock Loading ◽  
Slip Systems ◽  
Compression Tests ◽  
X Ray Diffraction ◽  
X Ray

Uniaxial compression tests and hydrostatic tests at pressures up to 27 kbars have been performed to determine operating slip systems in single crystal and polycrystal1ine beryllium. A recent study has been made of wave propagation in single crystal beryllium by shock loading to selectively activate various slip systems, and this has been followed by a study of wave propagation and spallation in textured, polycrystal1ine beryllium. An alteration in the X-ray diffraction pattern has been noted after shock loading, but this alteration has not yet been correlated with any structural change occurring during shock loading of polycrystal1ine beryllium.This study is being conducted in an effort to characterize the effects of shock loading on textured, polycrystal1ine beryllium. Samples were fabricated from a billet of Kawecki-Berylco hot pressed HP-10 beryllium.

Crystal structure of an inclusion complex between chiral monoaza-15-crown-5 and S(–)-1-phenyl-ethyl ammonium percholorate

2003 ◽  
Vol 218 (5) ◽  
Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören
Keyword(s):  
Crystal Structure ◽  
Inclusion Complex ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
New Type

AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

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