Structural Studies of Technetium Complexes. XI. The Crystal Structure of Bis(tetraphenylarsonium) Bis(1,2-dicyanoethenedithiolato)nitridotechnetate(V)

1989 ◽  
Vol 42 (6) ◽  
pp. 875 ◽  
Author(s):  
GA Williams ◽  
J Baldas
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Apical Position ◽  
Full Matrix ◽  
X Ray ◽  
R Value ◽  
Centrosymmetric Structure

The crystal structure of [AsPh4]2 [ TcN(mnt)2] ( mnt = 1,2-dicyanoethenedithiolate) has been determined by single-crystal X-ray diffraction methods at 21 � 1 C. Crystals are monoclinic, space group Pn , with a 11 369(2), b 15.530(2), c 14.421(3) � , P 97.58(2)�, and Z 2. Full-matrix least-squares refinement gave a final R value of 0.057 for 4232 independent reflections. The technetium atom in the [TcN( mnt )2]2- anion has square-pyramidal coordination geometry with the nitrido ligand in the apical position, Tc =N 1.59(1) � , and four Tc -S bonds with distances varying between 2.367(4) and 2.419(4) �. The Tc =N core is disordered about a pseudo-inversion centre, but unequal occupancies of the disordered sites preclude a centrosymmetric structure.

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.

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.

Preparation and Structure of Dibromobis(N,N-diethyldithiocarbamato)-thionitrosyltechnetium(III)

1991 ◽  
Vol 44 (8) ◽  
pp. 1125 ◽  
Author(s):  
J Baldas ◽  
SF Colmanet ◽  
GA Williams
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Trans Influence ◽  
R Value

The title compound, [Tc (NS)(S2CNEt2)2Br2], has been prepared by the reaction of [ TcN (S2CNEt2)2] with SOBr2, and its crystal structure has been determined by single-crystal X-ray diffraction methods at 23�1°C. Crystals are orthorhombic, space group Pnma , with a 14.864(7), b 15.857(7), c 8.938(4)Ǻ, and Z 4. Full-matrix least-squares refinement gave a final R value of 0.047 for 1685 independent reflections. The technetium atom is seven-coordinate with a distorted pentagonal- bipyramidal coordination geometry. The thionitrosyl ligand and a bromo ligand occupy the axial positions, with the thionitrosyl group exerting a small trans influence with Tc-Brtrans 2.595(1) and Tc-Brcis 2.564(1)Ǻ. The coordination of the thionitrosyl group is essentially linear with Tc -N=S 177.2(7)°, Tc -N 1.754(9), and N=S 1.504(9)Ǻ.

Synthesis and Crystal and Molecular Structure of trans-Dichloro(ethanedial dioximato(1—)-N,N')(ethanedial dioxime-N,N')rhodium(III)

1989 ◽  
Vol 44 (1) ◽  
pp. 5-8
Author(s):  
Michel Mégnamisi-Bélombé
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Room Temperature ◽  
Crystal And Molecular Structure ◽  
Crystallographic Direction ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cl Atoms

Abstract trans-Dichloro(ethanedial-dioximato)(ethanediaI-dioxime)rhodium (III), RhCl2(GH)(GH2), has been synthesized and its structure determined by single crystal X-ray diffraction at room temperature. C4H7Cl2N4O4Rh, Mr = 348.94. monoclinic space group P21/ɑ; a = 10.543(3), b = 8.363(2), c = 11.512(3)Å ; β = 92.79(2)°; V = 1024Å3; Z = 4; Dc = 2.26 Mg m-3. Final Rw = 0.075 for 2035 reflections and 139 parameters. The coordination geometry around Rh is a dis­torted (4+2) octahedron, with four chelating N atoms lying in the equatorial plane and the two Cl atoms in the apical positions. The H atoms of the oxime groups are involved in relatively weak intramolecular O-H-O bridgings, as well as in very strong intermolecular bridgings which extend throughout the crystal structure and propagate nearly parallel to the [101] crystallographic direction.

Synthese und Kristallstruktur von [Hg2(p-SC6H4NO2)]NO3 / Synthesis and Crystal Structure of [Hg2(p-SC6H4NO2)]NO3

1990 ◽  
Vol 45 (8) ◽  
pp. 1193-1196 ◽  
Author(s):  
Klaus Brodersen ◽  
Axel Knörr
Keyword(s):  
Crystal Structure ◽  
Chain Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Nitrate Ions ◽  
R Value ◽  
A Chain

[Hg2(p-SC6H4NO2)]NO3 is formed by the reaction of p-nitrothiophenol with dimercury(I)-dinitrate in methanol. It crystallizes in the monoclinic space group P21/n with a = 1175.5(9) pm, b = 1079.8(8) pm, c = 876.2(8) pm, β = 110.74(4)° and Z = 4. The crystal structure has been determined by X-ray diffraction and refined to an R-value of 0.052. The results show that the compound exists as a chain structure of [—®S(C6H4NO2)— Hg— Hg—]n with nitrate ions connecting the chains.

The Crystal Structure of (2,2′-Bipyridine)(pyrazine)(2,2′:6′,2″-terpyridine)ruthenium(II) Hexafluorophosphate

1996 ◽  
Vol 49 (4) ◽  
pp. 527 ◽  
Author(s):  
PT Gulyas ◽  
TW Hambley ◽  
PA Lay
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Steric Strain ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Distorted Octahedral ◽  
Back Bonding

The crystal structure of [ Ru ( terpy )( bpy )( pz )] (PF6)2 has been determined by X-ray diffraction methods and refined to a residual of 0.046 for 1855 independent observed reflections. The crystals are monoclinic, space group P 21/a, a 16.836(7), b 10.778(5), c l9.342(5) Ǻ, β 115.11(3)°. The coordination geometry around the ruthenium(II) ion is distorted octahedral, with the various Ru -N bond lengths indicative of considerable interligand steric strain. The Ru -N pyrazine bond is the longest within the structure, consistent with other evidence that n back-bonding to pyrazine is weak in the complex.

Synthesis of aminoalcohol compounds of platinum and crystal structure of trans-[Pt(2-amino-2-methyl-1-propanol)2Cl2]

1984 ◽  
Vol 62 (12) ◽  
pp. 2657-2660 ◽  
Author(s):  
F. D. Rochon ◽  
P. C. Kong ◽  
R. Melanson
Keyword(s):  
Crystal Structure ◽  
Organic Ligand ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
R Factor ◽  
Bonding System ◽  
Square Planar ◽  
Hydrogen Bonding System

Three types of complexes, trans-[Pt(LH)2Cl2], [Pt(L)2], and [Pt(LH)2(SR)2] where LH = NH2—C(CH3)2(CH2OH) and NH2—C(CH2OH)3 and L are the deprotonated ligands, have been synthesized.The crystal structure of trans-[Pt(NH2—C(CH3)2CH2OH)2Cl2] has been determined by X-ray diffraction methods. The crystals are monoclinic, space group P21/c, with a = 6,282(3), b = 20,901(13), c = 10,769(10) Å, β = 92,64(6)°, and Z = 4. The structure was refined by full-matrix least-squares analysis to a conventional R factor of 0.049 and Rw = 0.042. The coordination around the platinum atom is square planar. The Pt—Cl distances are 2.306(2) and 2.309(3) Å and the Pt—N bonds are 2.060(8) and 2.071 (7) Å. The hydroxyl oxygen atoms are disordered; the disorder is different for each organic ligand. The structure is stabilized by an extensive hydrogen bonding system.

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.

Darstellung und Kristallstruktur von Bis-(N-Methylhydroxylamido(1-)-O.N)(N-methyl-N-oxo-dithiocarbamato-O.S)- oxo-molybdän(VI) / Synthesis and Crystal Structure of Bis(N-methylhydroxylamido(1-)-O,N)- (N-methyl-N-oxo-dithiocarbamato-O,S)-oxo-molybdenum(VI)

1981 ◽  
Vol 36 (3) ◽  
pp. 289-292 ◽  
Author(s):  
Wolfgang Holzbach ◽  
Karl Wieghardt ◽  
Johannes Weiss
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Aqueous Suspension ◽  
Membered Ring ◽  
Pentagonal Bipyramid ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
R Value

Abstract The reaction of [MoO2((CH3)HN-O)2] and N-methylhydroxylammoniumchloride in an aqueous suspension with CS2 yields red crystals of the analytical composition MOC4H14N3O4S2. The crystal structure has been determined by single crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/c, with cell constants a= 1333.2(3), b = 814.2(2), c = 2179.8(6) pm, β = 105.42(2)°, and Z = 8. The final R-value is 4.5% for 2965 unique reflexions. The structure consists of two crystallographically independent neutral complexes of molybdenum(VI). The geometry about the molybdenum is a distorted pentagonal bipyramid containing a terminal oxygen atom, two N-methylhydroxylamido(1-) ligands coordinated via the O-and N-atoms and an N-methyl-N-oxo-dithiocarbamato(2-) ligand forming a planar five membered ring with the molybdenum(VI) center (O,S-coordination).

Structural studies of technetium complexes. III. The crystal structure of Tris[2-aminobenzenethiolato(2 - )-S, N]technetium(VI) : a trigonal-prismatictechnetium geometry

1982 ◽  
Vol 35 (12) ◽  
pp. 2413 ◽  
Author(s):  
J Baldas ◽  
J Boas ◽  
J Bonnyman ◽  
MF Mackay ◽  
GA Williams
Keyword(s):  
Crystal Structure ◽  
Hydrochloric Acid ◽  
Acid Solution ◽  
Room Temperature ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Trigonal Prismatic

Tris[2-aminobenzenethiolato(2–)-S,N]technetium(VI), Tc(NHC6H4S)3, has been prepared by the reaction of ammonium pertechnetate with 2-aminobenzenethiol in 0.1 M hydrochloric acid solution at room temperature. The crystal structure of Tc(NHC6H4S)3 has been determined by single-crystal X-ray diffraction methods at 17�C. Crystals are orthorhombic, space group P212121, with a 10.696(2), b 11.363(1), c l5.220(2) �, and Z 4. Automatic diffractometry has provided significant Bragg intensities for 1413 independent reflections, and the structure of the correct enantiomorph has been refined by full-matrix least-squares methods to R 0.044. The compound, which is isostructural with the molybdenum analogue, consists of discrete molecules of Tc(NHC6H4S)3. The environment about the technetium atom closely approximates a trigonal-prismatic geometry. This is the first example where this geometry has been established with technetium. Differences in detail between the structures of TC(NHC6H4S)3 and its molybdenum analogue are discussed. In particular the S3N3 coordination polyhedron in TC(NHC6H4S)3is contracted and the distortions from ideal trigonal-prismatic geometry are less than in the molybdenum analogue.

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