Structural Systematics of Rare Earth Complexes. XXI Polymeric Sodium Bis(thiodiglycolato)neodymiate(III)

1999 ◽  
Vol 52 (6) ◽  
pp. 617 ◽  
Author(s):  
Cameron J. Kepert ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Room Temperature ◽  
Rare Earth Complexes ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Thiodiglycolic Acid

A single-crystal, room-temperature, X-ray structure determination is recorded for the title compound, NaNd(tdga)2 (‘tdga2-’ ≡ −OCOCH2SCH2COO-). Crystals are monoclinic, space group Pc, a 9·5058(4), b 7·323(1), c 9·402(4) Å, β 97·71(2)°, Z = 2 f.u., conventional R on |F| being 0·028 for No 1054 independent ‘observed’ (I > 3σ(I)) diffractometer reflections. The compound is a novel polymeric array; the neodymium atom is eight-coordinated by ligand oxygen atoms at distances ranging from 2·43(2) to 2·54(1) Å. A redetermination of the parent thiodiglycolic acid is also recorded (orthorhombic Pnam, a 5·0444(8), b 6·690(1), c 17·73(1) Å, Z = 4, R 0·038 for No 866).

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.

Structural Systematics of Rare Earth Complexes. XIV Hydrated 1 : 1 Adducts of Lanthanoid(III) Nitrates with 2,2′:6′,2″-Terpyridine

1999 ◽  
Vol 52 (6) ◽  
pp. 507 ◽  
Author(s):  
Lioubov I. Semenova ◽  
Allan H. White
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Room Temperature ◽  
Rare Earth Complexes ◽  
X Ray ◽  
C 23 ◽  
Structure Determinations

Room-temperature single-crystal X-ray structure determinations are recorded for (hydrated) lanthanoid(III) nitrate/2,2′:6′,2″-terpyridine (‘tpy’) (1 : 1) complexes; all are of the form Ln(NO3)3/tpy/H2O(1 : 1 :x), [(tpy)Ln(O2NO)2(OH2)y](NO3)(.z H2O), and form two series of compounds. For Ln = La(-)Gd, the complexes are [(tpy)Ln(O2NO)2(OH2)3](NO3), the lanthanoid atom being ten-coordinate; crystals are triclinic, P 1, a ≈ 11·8, b ≈ 11·3, c ≈ 8·9 Å, α ≈ 75, β 69, γ ≈ 89°, Z = 2 f.u., conventional R on |F| 0·045, 0·062 for No 4513, 2710 independent ‘observed’ (I > 3σ(I)) diffractometer reflections for Ln = La, Gd respectively. For Ln = Tb(-)Lu, a different form is found: monoclinic, P 21/c, a ≈ 8·8, b ≈ 11·5, c ≈ 23·8 Å, β ≈ 111°, Z = 4, R 0·055, 0·037, 0·056 for No 2427, 3079, 1857 for Ln = Tb, Lu, Y respectively, the form of the complex being [(tpy)Ln(O2NO)2(OH2)2](NO3).2H2O, with nine-coordinate lanthanoid. Crystallization of the Ln = La adduct from methanol yields an adduct of La(NO3)3/tpy/MeOH (1 : 1 : 2) [(tpy)La(O2NO)3(HOMe)2] stoichiometry with 11-coordinate lanthanum. Crystals are triclinic, P 1, a 12·361(2), b 12·244(3), c 7·753(2) Å, α 96·56(2), β 103·22(2), γ 91·16(2)°, Z = 2, R 0·037 for No 6597.

scholarly journals Synthesis and Single Crystal X-Ray Structure of New (2E)-2-[3-(1H-Imidazol-1-yl)-1-phenylpropylidene]-N-phenylhydrazinecarboxamide

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Mohamed I. Attia ◽  
Hazem A. Ghabbour ◽  
Aida A. El-Azzouny ◽  
Omar A. Al-Deeb ◽  
Maha S. Almutairi ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Single Crystal ◽  
Title Compound ◽  
Spectroscopic Characterization ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Imine Bond

Synthesis, spectroscopic characterization and X-ray crystal structure of a new (2E)-2-[3-(1H-imidazol-1-yl)-1-phenylpropylidene]-N-phenylhydrazinecarboxamide (4) are reported. The stereochemistry of the title compound4, C19H19N5O, about the imine bond [1.296 (4) Å] was assigned to have (E)-configuration. In the urea moiety, the N–H entities aretransto each other, and one of these forms is an intramolecular N–H⋯H hydrogen bond. The compound crystallizes in the monoclinic space groupP21/cwitha= 5.8093 (2) Å,b= 20.5575 (6) Å,c= 14.0355 (5) Å,α= 90.00°,β= 97.365° (2),γ= 90.00°,V= 1662.36 (10) Å3, andZ= 4. The molecules are packed in crystal structure by weak intermolecular hydrogen interactions.

scholarly journals Synthesis and Crystal Structure ofN-Dichloroacetyl-3,4-dihydro-3-methyl-6-chloro-2H-1,4-benzoxazine

2015 ◽  
Vol 2015 ◽  
pp. 1-5
Author(s):  
Shuang Gao ◽  
Hai-Tao Qu ◽  
Fei Ye ◽  
Ying Fu
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Compound C

A new compound,N-dichloroacetyl-3,4-dihydro-3-methyl-6-chloro-2H-1,4-benzoxazine, was synthesized and characterized. The crystal structure of the title compound (C11H10Cl3NO2,Mr=294.55) has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space groupP21/c, witha=6.7619(14),b=24.866(5),c=9.737(3) Å,α=90.00,β=130.982(18),γ=90.00°,V=1235.9(5) Å3,Z=4,Dx=1.583 Mg/cm3,λ(Mo  Ka)=0.71073 Å,F(000)=600,μ=0.729 mm−1,R=0.0476, andwR=0.1274for 2217 reflections withI>2σ(I).

Preparation and Crystal Structure Determination of [(C2Η5)4N]2Hg3Cl8

1995 ◽  
Vol 50 (1) ◽  
pp. 66-70 ◽  
Author(s):  
Inge Pabst ◽  
Peter Sondergeld ◽  
Mirjam Czjzek ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Analysis ◽  
Structure Determination ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Coordination Type ◽  
X Ray

The title compound has been prepared in two different ways: First, by boiling single crystals of [(C2H5)4N]HgCl3 in a mixture of n-hexane/n-octane [4:1] at T = 350 K, and second, in a synthesis from stoichiometric quantities of the components. X-ray structure analysis gave the stoichiometry [(C2H5)4N]2Hg3Cl8, monoclinic, space group P21, a = 7.538(3), b = 19.909(6), c = 10.274(3) Å, β = 95.13(1)°, V = 1535.7(9) A3, Z = 2. The basic [Hg3Cl8]2--units form broken zig-zag chains along [100]. The Hg–Cl distances within the [Hg3Cl8]2- clusters range from 2.315(3) to 2.755(4) Å. This is a new coordination type for halomercurates.

Structural Systematics of Rare Earth Complexes. XVI (‘Maximally’) Hydrated Rare Earth(III) Bromides

1999 ◽  
Vol 52 (6) ◽  
pp. 531 ◽  
Author(s):  
Lioubov I. Semenova ◽  
Peter C. Junk ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Room Temperature ◽  
Rare Earth Complexes ◽  
X Ray ◽  
Structure Determinations ◽  
First Time

Room-temperature single-crystal X-ray structure determinations carried out on rare earth bromides crystallized from water at room temperature define three series of hydrates LnBr3.nH2O. For Ln = La, Ce, a heptahydrate phase (n = 7) is defined, triclinic P 1, a ≈ 8·6, b ≈ 9·4, c ≈ 8·3 Å, α ≈ 108, β ≈ 99, γ ≈ 72°, isomorphous with the array described for the ‘early’ (Ln = La-Pr) rare earth chlorides, being binuclear [(H2O)7Ln(-Br)2Ln(OH2)7] Br4, Z = 1 dimer; conventional R on |F| were 0·051, 0·042 for 2323, 3451 independent ‘observed’ (I > 3σ(I)) diffractometer reflections respectively. For Ln = Pr(-)Dy, a hexahydrate phase is defined, monoclinic P 2/n, a ≈ 10·0, b ≈ 6·8, c ≈ 8·2 Å, β ≈ 93·5°, Z = 2 f.u., isomorphous with the array defined for the heavier (Ln = Nd, Lu, Y) rare earth chlorides, being [(H2O)6LnBr2] Br, with R 0·029, 0·034 for No 1590, 1388 respectively. For Ln = Ho(-)Lu, Y, an octahydrate is defined for the first time, monoclinic P 21/n, a ≈ 8·1, b ≈ 16·0, c ≈ 10·1 Å, b ≈ 94·0°, Z = 4 f.u., a new array of the form [Ln(OH2)8] Br3 emerging, with R 0·061, 0·048, 0·042 for No 1191, 2402, 1674 respectively, the metal environment being square antiprismatic.

Structural Systematics of Rare Earth Complexes. XX (Maximally) Hydrated Rare Earth Sulfates and the Double Sulfates (NH4)Ln(SO4)2.4H2O (Ln = La, Tb)

1999 ◽  
Vol 52 (6) ◽  
pp. 601 ◽  
Author(s):  
Cameron J. Kepert ◽  
Peter C. Junk ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Room Temperature ◽  
Rare Earth Complexes ◽  
Two Dimensional ◽  
Sulfate Ions ◽  
X Ray ◽  
Double Sulfate ◽  
Trivalent Rare Earth ◽  
Double Sulfates

Room-temperature single-crystal X-ray studies carried out on trivalent rare earth sulfate hydrates, Ln2(SO4)3.xH2O, crystallized at local ambience suggest the following arrays to be prevalent. For Ln = La, the nonahydrate is found, hexagonal P 63/m, with conventional R on |F| 0·023 for No 1159 ‘observed’ (I >3σ(I)) diffractometer reflections (redetermination). Although for Ln = Ce a similar structure has been previously recorded, we have obtained that adduct as the monoclinic C 2/c, Z = 4, octahydrate, a phase also found for Ln = Lu and diverse representative intermediate lanthanoids: a ≈ 13·6, b ≈ 6·6, c ≈ 18·2 Å, β ≈ 102°; for Ln = Ce (redetermination), Dy, Yb (redetermination), Lu, R was 0·022, 0·035, 0·031, 0·024 for No 3279, 2127, 3008, 3325 respectively. The structures of two lower hydrates adventitiously obtained are also recorded: the pentahydrate for Ln = Ce, monoclinic C 2/c, a 15·741(3), b 9·632(3), c 10·358(3) Å, β 119·72(2)°, Z = 4, R 0·030 for No 3372 (a redetermination), and the trihydrate for Ln = Lu, orthorhombic Cmc21, a 13·527(5), b 18·415(5), c 9·242(7) Å, Z = 8, R 0·040 for No 1743. All structures are infinite polymeric arrays, the lanthanoid atoms being bridged by sulfate ions. Studies are also recorded for the ammonium/trivalent rare earth double sulfate tetrahydrate salts, (NH4)Ln(SO4)2.4H2O, for the (hitherto) extremal members Ln = La, Tb, which are isomorphous with the previously studied Ln = Sm monoclinic P 21/c, Z = 4 array, a ≈ 6·6, b ≈ 19, c ≈ 8·8 Å, β 97°; R 0·035, 0·037 for No 3631, 3337. The array is a two-dimensional polymer, parallel to the ac plane.

scholarly journals Die Kristallstruktur von Calciumhexacyanoferrat(II)- Hexamethylentetramin-Wasser(1/1/6) Ca2 [Fe(CN)6] · C6H12N4 · 6H2O / The Crystal Structure of Calciumhexacyanoferrate(II)- Hexamethylenetetramine-Water(1/1/6) Ca2[Fe(CN)6] · C 6H12N4 · 6H2O

1988 ◽  
Vol 43 (2) ◽  
pp. 135-137 ◽  
Author(s):  
H.-Jürgen Meyer ◽  
Joachim Pickardt
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
Unit Cell ◽  
Single Crystal Structure ◽  
Crystal Structure Determination ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

Ca2[Fe(CN)6] · C6H12N4 · 6H2O crystallizes in the monoclinic space group B2/b with a = 1130,2(4), b = 1373,5(4), c = 1353,0(4) pm and γ = 97,17°. The X-ray single crystal structure determination converged at R = 0.055 (2057 reflections). Each of the four Fe(CN)6 octahedra (Z = 4) in the unit cell is coordinated by six Ca atoms with mean NCYAN - Ca distances of 253.5(3) pm. The Ca atoms are bridged by hexamethylenetetramine and water molecules

Synthesis and Single Crystal Structure Determination of Bis(carbido)bis(μ-diphenylphosphido)heptadecacarbonyloctaruthenium-Dichloromethane (1/1), Ru8(μ6-C)(μ5-C)(μ-PPh2)2(CO)17.CH2Cl2

1993 ◽  
Vol 46 (11) ◽  
pp. 1811 ◽  
Author(s):  
CJ Adams ◽  
MI Bruce ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Room Temperature ◽  
Single Crystal Structure ◽  
Crystal Structure Determination ◽  
Triangular Face ◽  
X Ray

The synthesis and room-temperature single-crystal X-ray structure determination of the title compound are recorded. Crystals are monoclinic, P 21/c, a 14.43(2), b 18.39(1), c 23.64(3) Ǻ, β 123.16(7)°, Z = 4, isostructural with the recently described Fe3Ru5 analogue; R was 0.048 for 6892 'observed' data [I > 3σ(I)]. The cluster is one of the few containing separated carbide ligands within a polyhedral metal skeleton, consisting of an Ru5C square pyramid and an Ru6C octahedron sharing a triangular face, with two PPh2 groups bridging opposite Ru-Ru vectors in each polyhedron.

Solvento Complexes of Main Group Metals: The Structure of the Dimethyl-Sulfoxide Adduct of Indium(III) Perchlorate

1990 ◽  
Vol 43 (4) ◽  
pp. 759 ◽  
Author(s):  
JM Harrowfield ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Dimethyl Sulfoxide ◽  
Structure Determination ◽  
Title Compound ◽  
Crystalline Solid ◽  
Threefold Axis ◽  
Space Group ◽  
X Ray ◽  
Main Group Metals ◽  
A Site

The title compound is readily obtained as a colourless , crystalline solid by recrystallization of hydrated indium perchlorate from dimethyl sulfoxide. The crystals are rhombohedral , space group R3, a 9.911(3)Ǻ, α 73.66(2)?, Z= 1 f.u.;a single-crystal X-ray structure determination at 295 K refined to R 0.039 for 806 'observed' reflections. Unlike many Me2SO complexes, the indium species contains nicely ordered cations , [In(Me2SO)6]3+. Indium lies on a site of 3 symmetry, with In-O 2.140(3)Ǻ and the angle between the oxygens related by the threefold axis being 94.2(1)°. Two independent perchlorate moieties are disordered about sites of 3 and 3 symmetry.

Sign in / Sign up

Export Citation Format

Share Document