Structural studies of Technetium Complexes. VIII. The Crystal Structure of Tetraphenylarsonium Tetrabromonitridotechnetate(VI)

1985 ◽  
Vol 38 (1) ◽  
pp. 215 ◽  
Author(s):  
J Baldas ◽  
J Bonnyman ◽  
GA Williams
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Bond Distance ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Angles ◽  
R Value

The crystal structure of [AsPh4] [TcNBr4] has been determined by single- crystal X-ray diffraction methods at 20�1°C. Crystals are tetragonal, space group P4/n, with a 12.875(2), c 7.992(1)Ǻ, and Z 2. Full-matrix least-squares refinement gave a final R value of 0.039 for 1263 independent reflections. The compound is isostructural with the series [AsPh4] [MNBr4] (M = Mo, Ru , Re or Os) and [AsPh4] [MNCl4](M = Mo, Tc , Ru, Re or Os), and with [AsPh4] [OsNI4] and [AsPh4]- [MOCl4](M = Mo or Re). The [TcNBr4]- anion in [AsPh4] [TcNBr4] possesses C4v symmetry with Br- Tc -Br bond angles of 87.08(1) and 153.91(4)°, and N= Tc -Br bond angles of 103.04(2)°. The Tc≡N bond distance is 1.596(6)Ǻ, and the Tc - Br distances are 2.4816(5)Ǻ.

Crystal Structure of Tetraethylammonium Bromopentacarbonyltungstate(0)

1995 ◽  
Vol 48 (5) ◽  
pp. 1045 ◽  
Author(s):  
T Whyte ◽  
GA Williams
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
R Value

The crystal structure of tetraethylammonium bromopentacarbonyltungstate (0), [NEt4] [W(CO)5Br], has been determined by single-crystal X-ray diffraction methods at 22�1°C. Crystals are tetragonal, space group P4/n, with a 9.206(2), c 10.484(2) Ǻ, and Z 2. Full-matrix least-squares refinement gave a final R value of 0.034 for 820 independent reflections. The [W(CO)5Br]- anion possesses exact C4v symmetry, with bond lengths W-Br 2.736(1), W-COtrans 1.93(1) and W-COcis 2.034(6) Ǻ.

Crystal structure of 8-Hydroxy-1H-naphtho[2,1,8-mna]xanthen-1-one

1984 ◽  
Vol 37 (8) ◽  
pp. 1763
Author(s):  
IR Castleden ◽  
LM Engelhardt ◽  
SR Hall ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Charge Transfer ◽  
Single Crystal ◽  
Least Squares ◽  
Interplanar Spacing ◽  
Charge Transfer Complexes ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray

The crystal structure of 8-hydroxy-1H-naphtho[2,1,8-mna]xanthen-1-one, C19H10O3, obtained as an indefinite methanolsolvate, has been determined at 295K by single-crystal X-ray diffraction methods, being refined by full matrix least squares to a residual of 0.056 for 892 independent 'observed' reflections. Crystals are monoclinic, P21/c, a 5.128(4), b 10.024(9), c 27.45(2) �, β 107.73(6)�, Z 4. The packing of the molecules is typically that of charge-transfer complexes, with an interplanar spacing of c.3.5 �.

scholarly journals Crystal structure of Tetraaqua(ethylenediamine)nickel(II) sulfate dihydrate and of Tetraaqua(2,2'-bipyridyl)nickel(II) sulfate dihydrate

1984 ◽  
Vol 37 (5) ◽  
pp. 921 ◽  
Author(s):  
PC Healy ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Oxygen Atoms

The crystal structures of the title compounds, [Ni(OH2)4(en)] [SO4].2H2O, (1), and [Ni(OH2)4(bpy)]- [SO4].2H2O, (2), have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by full matrix least-squares methods to residuals of 0.028,0.031 for 1852, 4323 independent 'observed' reflections respectively. Crystals of (1) are monoclinic, C2/c, a 9.459(4), b 12.192(7), c 12.294(3) �, β 119.84(4)�, Z 4. In the cation, Ni-N is 2.061(2) �; Ni-O (trans to O, N respectively) are 2.106(2), 2.063(2) �. Instead of being enlarged above 90� as predicted from repulsion theory, the angle between the pair of oxygen atoms trans to nitrogen is diminished, being 87 14(7)�. Crystals of (2) are triclinic, P1, a 11.476(5), b 9.351(5), c 7.793(4) �, α 77.63(4), β 83.52(3), γ87.40(4)�, Z 2. In the cation, Ni-N are both 2.063(2) �. Ni-O (trans to N, O respectively) are 2.060(2), 2.O42(2); 2.O80(2), 2�. The short Ni-O distance [2.042(2)�] is associated with the coordination of a trigonal water molecule.

Structural studies in the iron(III)/chloride/α,α'-diimine system. III. Crystal structures of Tris(2,2'-bipyridine)iron(II) μ-Oxo-bis[trichloroferrate(III)] and of 'Compound A', μ-Oxo-bis[cis-chlorobis(1 ,10-phenanthroline)iron(III)] chloride solvate

1983 ◽  
Vol 36 (10) ◽  
pp. 2057 ◽  
Author(s):  
PC Healy ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Single Crystal ◽  
Least Squares ◽  
Structure Determination ◽  
Ionic Species ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Compound A ◽  
X Ray

The crystal structure of [Fe(bpy)3] [CI3FeOFeCI3] (1) has been determined by single-crystal X-ray diffraction at 295 K, and refined by least squares to a residual of 0.058 for 2002 'observed' reflections. Crystals are monoclinic, P21/c, a 9.616(3), b 26.264(6), c 13.821(7) Ǻ, β 99.68(2)°, Z4. In the cation, Fe-N distances range from 1.956(9) to 1 .989(10) Ǻ; in the anion, Fe-Cl distances range from 2.196(5) to 2.225(5) Ǻ. Fe-O distances are 1.763(11) and 1.740(11) Ǻ, and the Fe-O-Fe angle is 148.9(7)°. Recrystallization of 'compound A' from methanolic aqueous solution yields crystals with stoichiometry [{cis-Fe(phen)2Cl}2O]Cl2.nH2O( n ≈ 4.5) as established by structure determination (hampered by serious disorder); R is 0.09 for 749 'observed' reflections. Crystals are orthorhombic, Pcn2, a 18.05(1), b 13.83(1), c 10.481(6) Ǻ, Z 2. The Fe-N distances trans to each other are 2.12(3) and 2.13(3) Ǻ; Fe-N distances trans to Cl and O are 2.20(2) and 2.28(2) Ǻ, respectively. Fe-CI is 2.34(1) and Fe-O 1.787(6) A; Fe-O-Fe is 161(1)°. For crystals from aqueous solution, an isomorphous but larger unit cell is obtained [2754(7), cf. 2616(3) Ǻ3]; it is believed that this is a consequence of variable occupancy of the disordered solvent layers which lie parallel to bc between the ionic species.

Studies of β-Diketone Complexes of Rhenium(V). The Molecular and Crystal Structure of trans-Dichlorobis(pentane-2,4-dionato)rhenium(IV)

1973 ◽  
Vol 51 (13) ◽  
pp. 2073-2076 ◽  
Author(s):  
I. D. Brown ◽  
C. J. L. Lock ◽  
Che'ng Wan
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Molecular And Crystal Structure ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths ◽  
Dimeric Structure

One of the compounds obtained by reacting acetylacetone with oxoethoxodichlorobis(triphenylphosphine)rhenium(V) has been shown by single crystal X-ray diffraction to be trans-dichlorobis(pentane-2,4-dionato)rhenium(IV). The crystals are triclinic, a = 8.032(4), b = 8.344(6), c = 7.429(6) Å, α = 118.1(2), β = 92.3(2), γ = 55.5(2)°, [Formula: see text], Z = 1. Intensities were measured with a microdensitometer from photographs recorded on an integrating precession camera. Of the 991 measured reflections all were observed and 984 were used in the refinement. The structure was refined by full matrix least squares to an R2 value of 0.0685. The compound was found to be a trans-monomer, in contrast to the dimeric structure claimed to exist in solution. The ligand atoms bonded to rhenium lie almost exactly at the apices of an octahedron and the bond lengths (Re—Cl, 2.326(8); Re—O1, 1.97(1); Re—O2, 2.01(1) Å) are in the range expected.

Crystal structure of Tris(N,N-diethyldithiocarbamato)thallium(III)

1978 ◽  
Vol 31 (9) ◽  
pp. 1927 ◽  
Author(s):  
DL Kepert ◽  
CL Raston ◽  
NK Roberts ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
Electron Pair ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The crystal structure of the title compound, [Tl(S2CNEt2)3], has been determined by single-crystal X-ray diffraction methods at 295 K and refined by full-matrix least squares to a residual of 0.050 for 2517 'observed' reflections. Crystals are monoclinic, with space group A2/a, a 14.789(7), b 10.428(4), c 18.207(9) Ǻ, β 118.11(4)°, Z 4, and are isostructural with those of the previously determined gallium and indium analogues, the molecule having 2 symmetry with <Tl-S> 2.666 Ǻ. As in the dimethyl/thallium analogue, the departure of the TlS6 core symmetry from 3 is large and is examined in terms of electron-pair repulsion theory.

Crystal Structure of ζ2' Martensite in Au-49.5at%Cd Alloy

1991 ◽  
Vol 246 ◽  
Author(s):  
Yutaka Emura ◽  
Takuya Ohba ◽  
Kazuhiro Otsuka
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Least Squares ◽  
Least Squares Method ◽  
Diffraction Method ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Lattice Constants

AbstractCrystal structure of the ζ2' martensite in a Au-49.5at%Cd ally has been analyzed by the single crystal x-ray diffraction method. The crystal lattice was trigonal and the lattice constants were a:0.8095(3) and c=o.57940(6) nm. There were 18 atoms in a unit cell. The space group was P3, which was different from that previously determined by Vatanayon and Hehemann. The structure was refined by the full matrix least squares method to a final R factor of 7.8% and a weighted R factor of 4.1%.

Crystal structure of diammonium aquapentachloroferrate(III)

1978 ◽  
Vol 31 (12) ◽  
pp. 2717 ◽  
Author(s):  
BN Figgis ◽  
CL Raston ◽  
RP Sharma ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Hydrogen Bonded

The crystal structure of the title compound, (NH4)2 [FeCl5(H2O)], has been redetermined by single-crystal X-ray diffraction at 295 K and refined by full matrix least squares to a residual of 0.054 for 1662 'observed' reflections. Crystals are orthorhombic, Pnma, a 13.706(2), b 9.924(1), c 7.024(1)Ǻ Z 4. Fe-O is 2.110(4)Ǻ; Fe-Cl range between 2.323(1)Ǻ (trans to OH2) and 2.350(1)-2.390(1) Ǻ (cis), the latter distances being very dependent upon hydrogen-bonded interactions with nearby species.

Crystal Structure of Alloxan Monohydrate: A Redetermination

1989 ◽  
Vol 42 (10) ◽  
pp. 1795 ◽  
Author(s):  
JM Harrowfield ◽  
BW Skelton ◽  
AA Soudi ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
X Ray Diffraction ◽  
Interatomic Distances ◽  
Full Matrix ◽  
X Ray ◽  
Alloxan Monohydrate ◽  
Long Chain

The structure of the title compound, C4H4N2O5, has been redetermined by single-crystal X-ray diffraction methods at c. 295 K. Crystals are triclinic, P1, a 8.217(2), b 6.809(2), c 5.765(4) �, α 66.49(3),β 81.87(3), γ 74.35(2)�, Z= 2; the structure was refined by full-matrix least squares to a residual of 0.042 for 2190 independent 'observed' reflections, typical non-hydrogen interatomic distances being determined with estimated standard deviations of 0.001 �. Together with the recent precise redetermination of the structure of alloxan , these results allow comparison of the geometries of essentially planar polycarbonyl (-hydrate) arrays with those of long-chain arrays previously recorded.

Structural Studies of Technetium Complexes. X. The Crystal-Structure of Tetraphenylarsonium Hexakis(Isothiocyanato)Technetate(IV)-Dichloromethane (1/1)

1987 ◽  
Vol 40 (1) ◽  
pp. 27 ◽  
Author(s):  
GA Williams ◽  
J Bonnyman ◽  
J Baldas
Keyword(s):  
Crystal Structure ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Octahedral Structure ◽  
Crystal Lattices ◽  
Full Matrix ◽  
X Ray ◽  
C And N ◽  
R Value ◽  
A Site

The crystal structure of [AsPh4]2 [ Tc (NCS)6].CH2Cl2 has been determined by single-crystal X-ray diffraction methods at 23 � 1�C . Crystals are tetragonal, space group I4/m, with a 11.523(5), c 22.43(2) �, and Z 2. Diffraction data from two different crystals were analysed and in both cases disorder was present in the crystal lattices. Full-matrix least-squares refinement gave a final R value of 0.073 for 1188m independent reflections. The [TC(NCS)6]2- anion has an octahedral structure with the technetium(1V) atom situated on a site of 4/m symmetry. The Tc -N bond lengths are 2.00(1) and 2.01(1) Ǻ with N- Tc -N angles of exactly 90�. Two of the Tc -NCS groups are constrained by the crystal symmetry to be perfectly linear, while for the remaining four Tc -NCS groupings the Tc -N-C and N-C-S angles are 175.9(9)� and 175.3(10)� respectively.

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