Mixed Transition Metal/Lanthanide Complexes: Structural Characterization of Solids Containing Cage Amine Chromium(III) Cations and Tris(dipicolinato)lanthanide Anions

1995 ◽  
Vol 48 (4) ◽  
pp. 807 ◽  
Author(s):  
JM Harrowfield ◽  
Y Kim ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Transition Metal ◽  
Crystal Lattice ◽  
Structural Characterization ◽  
Lanthanide Complexes ◽  
Room Temperature ◽  
X Ray ◽  
Structure Determinations ◽  
Full Structure ◽  
Mixed Transition

As the foundation to a survey of interactions between chromium(III) and lanthanide(III) ions within the same crystal lattice, a series of complexes of stoichiometry [Cr((NH2)2sar)]- [ Ln ( dipic )3].8H2O (sar = 3,6,10,13,16,19-hexaazabicyclo[6.6.6] icosane, Ln = La-Lu plus Y, dipic = pyridine-2,6-dicarboxylate) has been synthesized and structurally characterized by room-temperature single-crystal X-ray studies. An isomorphous series is found for all Ln, being triclinic, Pī , a ≈ 18.1, b ≈ 13.3, c ≈ 11 Ǻ, α ≈ 111.5, β ≈ 96.2, γ ≈ 109.2°, Z = 2 formula units, full structure determinations being recorded for Ln = La (conventional R 0.048 on |F| for No 6494 independent 'observed' [I > 3σ(I)] reflections at convergence), Ce (R 0.036 for No 8980) and Lu (R 0.046 for No 6791). A less well defined protonated series, with a 2:3 Cr/ Ln ratio, has also been characterized specifically for Ln = La [orthorhombic, Pbca , a 26.223(8), b 53.17(3), c 18.329(9) Ǻ, Z = 8; R 0.092 for No 5104], the lutetium analogue having a similar cell.

Single Crystal X-Ray Structural Characterization of [BiX2(S2CNEt2)]Infinity∞, X=Cl, Br

1994 ◽  
Vol 47 (2) ◽  
pp. 405 ◽  
Author(s):  
PK Bharadwaj ◽  
AM Lee ◽  
BW Skelton ◽  
BR Srinivasan ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Sulfur Atom ◽  
Structural Characterization ◽  
Structure Determination ◽  
Room Temperature ◽  
X Ray ◽  
Structure Determinations

Single-crystal room-temperature X-ray structure determinations of the title compounds have been carried out. The two compounds are isomorphous, and isomorphous with the previously determined iodide analogue, being monoclinic, P 21/c, a ≈ 10.0, b ≈ 14.9, c ≈ 7.8 Ǻ, β ≈ 92°, Z = 4 formula units; residuals were 0.037, 0.036 for 2197, 1654 'observed' reflections for X = Cl , Br respectively. As in the iodide, the complexes are infinite polymers, with successive bismuth atoms bridged by the two halides and one sulfur atom of the ligand , which also chelates each bismuth. The structure determination of C5H5NCONEt2]2 [Cl5Bi(NC5H5)], isostructural with its thiocarbamoyl analogue, is also recorded.

Structural Systematics of Rare Earth Complexes. VII. Crystal Structure of Bis(2,2'/6',2␛-Terpyridinium) Octaaquaterbium(III) Heptachloride Hydrate

1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Single Crystal ◽  
Structural Characterization ◽  
Title Compound ◽  
Room Temperature ◽  
Chloride Ions ◽  
Full Matrix ◽  
X Ray

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXIV Syntheses, Spectroscopy and Structures of Some 1 : 4 Adducts of Copper(I) and Silver(I) Perchlorates with Triphenylarsine and Triphenylstibine

1997 ◽  
Vol 50 (6) ◽  
pp. 539 ◽  
Author(s):  
Graham A. Bowmaker ◽  
Effendy ◽  
Robert D. Hart ◽  
John D. Kildea ◽  
Brian W. Skelton ◽  
...  
Keyword(s):  
Room Temperature ◽  
Far Infrared ◽  
Lewis Base ◽  
X Ray ◽  
Cation Disorder ◽  
Structure Determinations ◽  
Consistent Picture ◽  
Far Infrared Spectra

Syntheses and room-temperature single crystal X-ray structure determinations are recorded for adducts [M(EPh3)4] (ClO4), M = Cu, E = As (1), Sb (2); M = Ag, E = As (3), Sb (4), enabling comparison with analogous, previously studied MP4 and MN4 environments. The four complexes so characterized all crystallize in the familiar rhombohedral R-3 array (a ≈ 14·4, c ≈ 52 Å, hexagonal setting) with the metal and chlorine atoms located on crystallographic threefold axes. In these arrays Cu–E (axial, off axis) are 2·493(2), 2·533(1) for (1), and 2·572(1), 2·577(1) Å for (2), the disparity in the two independent M-E distances being diminished relative to those of previously studied phosphorus analogues, perhaps in consequence of increasing E size. In (3) and (4), some cation disorder is evident in respect of the ligand pnictide atom (E); for the major components Ag-E are 2·652(3), 2·680(2) in (3); 2·732(2), 2·7295(8) Å in (4). Problems associated in defining the metal atom environment geometries in the latter are, nevertheless, more satisfactorily overcome in two further determinations of nitrate salts: [Ag(SbPh3)4] (NO3) (5) is of the rhombohedral family with no cation core disorder, Ag–E (axial, off axis) being 2·720(4), 2·725(2) Å, while the structural characterization of a 1 : 4 triphenylarsine adduct of silver nitrate is recorded as its tetraethanol solvate, namely [Ag(AsPh3)4] (NO3).~ 4C2H5OH(6), monoclinic, C2/c, a 18·373(4), b 20·786(5), c 21·070(8) Å, β 108·18(3)°, Z = 4 f.u. The silver atom of the [Ag(AsPh3)4]+cation unusually lies on a crystallographic 2 (rather than a 3 ) axis of the incipiently23 (T) array, with Ag-As 2·649(2), 2·650(2) Å and As-Ag-As ranging from 108·22(4) to 111·41(6)°. The structure determination of a chloroform solvate of (2), denoted (2a), of low precision, is noted, together with the structure of an interesting artefact, isomorphous with the rhombohedral oxoanion array, modelled as [Ag(PPh3)4]2 (SiF6).py (7). Bands in the far-infrared spectra of [M(AsPh3)4] (ClO4) are assigned to v(MAs) vibrations at 119 (M = Cu) and 103 cm¯1 (M = Ag); this produces a more consistent picture of the variation in the wavenumbers of the v(ME) modes in [M(EPh3)4]+ compounds than was available previously.

Structural Characterization of a Cage Ligand Fragmentation Reaction

1994 ◽  
Vol 47 (1) ◽  
pp. 181 ◽  
Author(s):  
JM Harrowfield ◽  
AM Sargeson ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Room Temperature ◽  
Fragmentation Reaction ◽  
X Ray ◽  
Nitrogen Donor ◽  
Crystal Structural

The room temperature X-ray single-crystal structural characterization of a protonated copper(II) complex of a ligand artefact, L′, of L = N-Me6sar (described in an accompanying paper) is recorded, the new ligand L′ being generated formally by elimination of a CH2CH2 bridge between a pair of nitrogen donor atoms of L. The complex, [ ClCu (H2L′) (ClO4)3.2H2O, is orthorhombic, Pccn , a 22.528(7), b 10.544(3), c 13.748(6) Ǻ, Z = 4 formula units, R being 0.053 for 1133 independent 'observed' [I > 3σ(I)] reflections. The cation, containing five-coordinate square-pyramidal ClCuN4 copper, is disposed with the Cu- Cl bond [2.458(3)Ǻ] lying on a crystallographic 2 axis; Cu-N distances are 2.094(8) and 2.093(8)Ǻ.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LIII. Synthesis and Structural Characterization of Binuclear μ,μ'-Dichloro-, Dibromo and Diiodo-bis[(pyridine)(triphenylphosphine)copper(I)] Complexes, and Their Pyridine-4-carbonitrile Analogues

1989 ◽  
Vol 42 (6) ◽  
pp. 913 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Lewis Base ◽  
The Other ◽  
X Ray ◽  
Structure Determinations ◽  
M Phase ◽  
And Inversion ◽  
Iodide Single Crystal

Mixed base pyridine (py)/triphenylphosphine adducts of the copper(1) halides, CuX, have been synthesized for 1 : 1 : 1 stoichiometry for X = chloride and iodide; single-crystal X-ray structure determinations of these show them to be isomorphous and isostructural with that of the bromide recorded elsewhere, being �,�′- dihalo-bridged dimers , [(PPh3)( py )CuX2Cu( py )(PPh3)], monoclinic, C2/c, a ≈ 26.2, b ≈ 14.3, c ≈ 11 .2 � , β ≈ 95, Z = 4 dimers. The bromide has been isolated as a new monoclinic C 2/m polymorph, a 11 .279(8), b 14.268(6), c 13.858(4) �, β 109.33(6)�, Z=4 dimers, and details of its structure are also recorded. The structures of their pyridine-4-carbonitrile (pycn) analogues have also been determined and found to be also binuclear, with no cyano-copper interactions; these also are an isomorphous, isostructural series, monoclinic P21/n, a ≈ 15.4, b ≈ 8.1, c ≈ 17.9 � , β ≈ 101 �, Z = 2 dimers. In each series of dimers, one half of the dimer is crystallographically independent, the generators of the other half being twofold rotor (C2/c phase), mirror (C2/m phase) and inversion centre (P21/n phase) respectively.

scholarly journals Transition metal complexes with thiosemicarbazide-based ligands, Part 58. Synthesis, spectral and structural characterization of dioxovanadium(V) complexes with salicylaldehyde thiosemicarbazone

2011 ◽  
Vol 76 (6) ◽  
pp. 865-877 ◽  
Author(s):  
Ljiljana Vojinovic-Jesic ◽  
Vukadin Leovac ◽  
Mirjana Lalovic ◽  
Valerija Cesljevic ◽  
Ljiljana Jovanovic ◽  
...  
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Elemental Analysis ◽  
Structural Characterization ◽  
Ammoniacal Solution ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Oxo Ligand

The first two complexes of dioxovanadium(V) with salicylaldehyde thiosemicarbazone (SALTSC), of the coordination formulas [VO2(SALTSC-H)]?H2O (1) and NH4[VO2(SALTSC-2H] (2), were synthesized and characterized by elemental analysis, conductometric measurements, IR and UV-vis spectroscopy and X-ray analysis. The complexes were obtained in the reaction of an aqueous ammoniacal solution of NH4VO3 and SALTSC. The results of the characterization showed that SALTSC was coordinated in the usual ONS tridentate mode as monoanion in complex 1 and dianion in complex 2. In both complexes, the vanadium atom is in a deformed square-pyramidal environment and is slightly shifted towards the apical oxo-ligand (? 0.52 ?).

Lewis-Base Adducts of Group 11 Metal-Compounds. XXXIII. Structural Characterization of Two Novel 'Trigonal Planar' Halobis(N-Base)Copper(I) Complexes

1988 ◽  
Vol 41 (3) ◽  
pp. 335 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Lewis Base ◽  
Metal Compounds ◽  
Base Complex ◽  
X Ray ◽  
Structure Determinations

Single-crystal X-ray structure determinations are recorded for two unusual trigonal planar XCuL2 species, X = halogen, L = monodentate N- base. For iodobis (2-methylquinoline)copper(I) (1) crystals are orthorhombic, P212121, a 15.079(7), b 12.592(7), c 9.585(4)Ǻ, Z 4. R was 0.028 for 1285 independent 'observed' reflections; the copper(I) environment is trigonal planar [I-Cu, 2.533(2); Cu-N, 2.034(6), 2.0l5(7)Ǻ; I-Cu-N are 119.1(2), 120.4(2) and N-Cu-N, 120.4(2)°]. For the mixed base complex bromo (3,5-dimethylpyridine)(2,4,6-trimethylpyridine )copper(I) (2), crystals are triclinic, pī , a 13.643(5), b 8.434(5), c 8.163(4)Ǻ, α 59.65(4), β 79.76(4), γ 89.68(4)°, Z 2; R was 0.046 for 1551 'observed' reflections. Br-Cu is 2.418(2); Cu-N, 1.971(5), 1.963(6)Ǻ; Br-Cu-N are 113.5(2), 110.0(2) and N-Cu-N, 136.4(3)°.

scholarly journals Structural features and near infra-red (NIR) luminescence of isomeric Yb(iii) bipyridyl-N,N′-dioxide coordination polymers

2015 ◽  
Vol 44 (29) ◽  
pp. 13378-13383 ◽  
Author(s):  
Gail M. Sequeira ◽  
Wayne Y. Tan ◽  
Evan G. Moore
Keyword(s):  
Coordination Polymers ◽  
Structural Characterization ◽  
Lanthanide Complexes ◽  
Structural Features ◽  
X Ray ◽  
X Ray Crystallography ◽  
Infra Red ◽  
Nir Luminescence

The synthesis and structural characterization of a series of lanthanide complexes formed from YbX3 salts (X = NO3− or CF3SO3−) and the isomeric 4,4′-bipyridine-N,N′-dioxide (4,4′-bpdo) or 3,3′-bipyridine-N,N′-dioxide (3,3′-bpdo) ligands has been undertaken by X-ray crystallography.

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