Molecular and Crystal Structure, and EPR Studies of Tetraphenylarsonium [Bis-(1,3-dithia-2-one-4,5-dithiolato)-nickelate], (AsPh4)[Ni(dmid)2]

1988 ◽  
Vol 43 (9) ◽  
pp. 1137-1143 ◽  
Author(s):  
R. Vicente ◽  
J. Ribas ◽  
C. Zanchini ◽  
D. Gatteschi ◽  
J.-P. Legros ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Dihedral Angle ◽  
Unpaired Electron ◽  
Room Temperature ◽  
Monoclinic Space Group ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Variable Parameters ◽  
X Ray

AbstractThe crystal structure of (AsPh4)[Ni(dmid)2 (dmid2- = 1,3-dithia-2-one-4,5-dithiolato) has been determined by X-ray diffraction studies: crystals are monoclinic, space group P21/n a = 14.724(2), b = 14.305(5), c = 15.570(3) Å, β = 92.20(1)°, V = 3277 Å3 , ᵨx = 1.63 g cm-3 for Z = 4, final conventional agreement indices R = 0.038 and Rw = 0.049 for 2115 unique, observed reflections and 211 variable parameters. The asymmetric unit contains one (AsPh4)+ cation and one [Ni(dmid)2] anion, both in general positions. The anions are isolated from each other by the bulky cations. The [Ni(dmid)2]- ion deviates strongly from planarity: the dihedral angle between the two Ni(dmid) moieties is 10.7°; one of the dmid ligand is almost planar, while the second one is severely puckered. Polycristalline powder and single crystal EPR spectra have been recorded at room temperature. Only one signal was observed in all crystal orientations. The angular depend-ences of the linewidth and of the g values have been determined, as well as the principal g values and directions. These results have been compared to those previously obtained for the analogue (n-Bu4N)[Ni(dmit)2 ] (drnit2- = 1,3-dithia-2-thione-4,5-dithiolato), and discussed in terms of the localization of the unpaired electron on the ligands. leading to a formal (III) and actual (II) nickel oxidation state.

scholarly journals Crystal structures of (η4-cycloocta-1,5-diene)bis(1,3-dimethylimidazol-2-ylidene)iridium(I) iodide and (η4-cycloocta-1,5-diene)bis(1,3-diethylimidazol-2-ylidene)iridium(I) iodide

2020 ◽  
Vol 76 (5) ◽  
pp. 611-614
Author(s):  
Chad M. Bernier ◽  
Christine M. DuChane ◽  
Joseph S. Merola
Keyword(s):  
Crystal Structure ◽  
Amino Acid ◽  
Single Crystal ◽  
Room Temperature ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Atomic Coordinates

The title complexes, (η4-cycloocta-1,5-diene)bis(1,3-dimethylimidazol-2-ylidene)iridium(I) iodide, [Ir(C5H8N2)2(C8H12)]I, (1) and (η4-cycloocta-1,5-diene)bis(1,3-diethylimidazol-2-ylidene)iridium(I) iodide, [Ir(C7H12N2)2(C8H12)]I, (2), were prepared using a modified literature method. After carrying out the oxidative addition of the amino acid L-proline to [Ir(COD)(IMe)2]I in water and slowly cooling the reaction to room temperature, a suitable crystal of 1 was obtained and analyzed by single-crystal X-ray diffraction at 100 K. Although this crystal structure has previously been reported in the Pbam space group, it was highly disordered and precise atomic coordinates were not calculated. A single crystal of 2 was also obtained by heating the complex in water and letting it slowly cool to room temperature. Complex 1 was found to crystallize in the monoclinic space group C2/m, while 2 crystallizes in the orthorhombic space group Pccn, both with Z = 4.

The crystal and molecular structure of dipyrrolidylthiuram disulfide

1983 ◽  
Vol 36 (7) ◽  
pp. 1371 ◽  
Author(s):  
GA Williams ◽  
JR Statham ◽  
AH White
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Dihedral Angle ◽  
Crystal And Molecular Structure ◽  
Structural Parameters ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray

The crystal structure of dipyrrolidylthiuram disulfide has been determined by single-crystal X-ray diffraction techniques at 295 K. Crystals are monoclinic, space group C2/c, unit cell a 13.835(3), b 10.422(2), c 9.427(3) �, β 97.08(2)� and Z 4. Automatic diffractometry has provided significant Bragg intensities for 1402 independent reflections, and the structure has been refined by least-squares methods to R 0.037. The structure consists of discrete C4H8NC(S)S2C(S)NC4H8 molecules. Half of each molecule is crystallographically unique with distances S-S 2.002(1), and C-S 1.804(2) and 1.645(2) �. The dihedral angle between planar C2NC(S)S portions is 87.9�. The relevance of the derived structural parameters to the question of why the tris(pyrrolidine-1-carbodithioato)iron(III) complex is, uniquely, high spin is discussed.

The first proof of protonated anion tetrahedra in the tsumcorite-type compounds

2004 ◽  
Vol 68 (5) ◽  
pp. 757-767 ◽  
Author(s):  
T. Mihajlović ◽  
H. Effenberger
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Single Crystal ◽  
Diffraction Data ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Synthetic Compounds ◽  
X Ray

AbstractHydrothermal synthesis produced the new compound SrCo2(AsO4)(AsO3OH)(OH)(H2O). The compound belongs to the tsumcorite group (natural and synthetic compounds with the general formula M(1)M(2)2(XO4)2(H2O,OH)2; M(1)1+,2+,3+ = Na, K, Rb, Ag, NH4, Ca, Pb, Bi, Tl; M(2)2+,3+ = Al, Mn3+, Fe3+, Co, Ni, Cu, Zn; and X5+,6+ = P, As, V, S, Se, Mo). It represents (1) the first Sr member, (2) the until now unknown [7]-coordination for the M(1) position, (3) the first proof of (partially) protonated arsenate groups in this group of compounds, and (4) a new structure variant.The crystal structure of the title compound was determined using single-crystal X-ray diffraction data. The compound is monoclinic, space group P21/a, with a = 9.139(2), b = 12.829(3), c = 7.522(2) Å, β = 114.33(3)°, V = 803.6(3) Å3, Z = 4 [wR2 = 0.065 for 3530 unique reflections]. The hydrogen atoms were located experimentally.

Evolution of crystal structure of dual layered molecular conductor (ET)4ZnBr4(C6H4Cl2) with temperature

CrystEngComm ◽  
2021 ◽  
Author(s):  
Gennady V. Shilov ◽  
Elena I. Zhilyaeva ◽  
Sergey M. Aldoshin ◽  
Alexandra M Flakina ◽  
Rustem B. Lyubovskii ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Electrical Resistivity ◽  
Single Crystal ◽  
Room Temperature ◽  
Organic Conductor ◽  
X Ray Diffraction ◽  
X Ray ◽  
Resistivity Measurements ◽  
Molecular Conductor ◽  
Abrupt Changes

Electrical resistivity measurements of a dual layered organic conductor (ET)4ZnBr4(1,2-C6H4Cl2) above room temperature show abrupt changes in resistivity at 320 K. Single-crystal X-ray diffraction studies in the 100-350 K range...

Crystal Structure and Vibrational Behaviour of Aqua Di(saccharinato)di(nicotinamide)copper(II)

2002 ◽  
Vol 57 (1) ◽  
pp. 43-46 ◽  
Author(s):  
Beatriz S. Parajón-Costaa ◽  
Enrique J. Baran ◽  
Oscar E. Piro ◽  
Eduardo E Castellano
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Ir Spectrum ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal structure of [Cu(sac)2(nic)2(H2O)] (sac = saccharinate anion; nic = nicotinamide) has been determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group C2/c with Z = 4 and the Cu(II) ion presents a CuN4O square pyramidal coordination. Some comparisons with related structures are made and the most important features of its IR spectrum were also discussed.

scholarly journals Serendipitous formation and characterization of K2[Pd(NO3)4]·2HNO3

2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
Solvothermal Process ◽  
X Ray Diffraction ◽  
Glass Ampoule ◽  
Space Group ◽  
X Ray ◽  
Complex Anions

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.

A New Supramolecular Synthon Using N-Methylaniline. The Crystal Structure of the 1 : 1 Adduct of N-Methylaniline with 5-Nitrofuran-2-carboxylic Acid

1998 ◽  
Vol 51 (9) ◽  
pp. 867 ◽  
Author(s):  
Daniel E. Lynch ◽  
Lisa C. Thomas ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Proton Transfer ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Supramolecular Synthon ◽  
X Ray ◽  
C 23 ◽  
A Cell

The crystal structure of the 1 : 1 adduct of N-methylaniline with 5-nitrofuran-2-carboxylic acid has been determined by single-crystal X-ray diffraction. Crystals are monoclinic, space group P21/c with Z 4 in a cell of dimensions a 8·467(5), b 6·106(2), c 23·95(1) Å, β 94·48(3)°. The molecules associate in a tetrameric, proton-transfer formation which has potential as a new supramolecular synthon.

scholarly journals The caesium phosphates Cs3(H1.5PO4)2(H2O)2, Cs3(H1.5PO4)2, Cs4P2O7(H2O)4, and CsPO3

2020 ◽  
Vol 151 (9) ◽  
pp. 1317-1328
Author(s):  
Matthias Weil ◽  
Berthold Stöger
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Single Crystal ◽  
Diffraction Data ◽  
Room Temperature ◽  
Structure Type ◽  
Solid State Reactions ◽  
X Ray Diffraction ◽  
Hydrogen Phosphate ◽  
X Ray

Abstract The caesium phosphates Cs3(H1.5PO4)2(H2O)2 and Cs3(H1.5PO4)2 were obtained from aqueous solutions, and Cs4P2O7(H2O)4 and CsPO3 from solid state reactions, respectively. Cs3(H1.5PO4)2, Cs4P2O7(H2O)4, and CsPO3 were fully structurally characterized for the first time on basis of single-crystal X-ray diffraction data recorded at − 173 °C. Monoclinic Cs3(H1.5PO4)2 (Z = 2, C2/m) represents a new structure type and comprises hydrogen phosphate groups involved in the formation of a strong non-symmetrical hydrogen bond (accompanied by a disordered H atom over a twofold rotation axis) and a very strong symmetric hydrogen bond (with the H atom situated on an inversion centre) with symmetry-related neighbouring anions. Triclinic Cs4P2O7(H2O)4 (Z = 2, P$$\bar{1}$$ 1 ¯ ) crystallizes also in a new structure type and is represented by a diphosphate group with a P–O–P bridging angle of 128.5°. Although H atoms of the water molecules were not modelled, O···O distances point to hydrogen bonds of medium strengths in the crystal structure. CsPO3 is monoclinic (Z = 4, P21/n) and belongs to the family of catena-polyphosphates (MPO3)n with a repetition period of 2. It is isotypic with the room-temperature modification of RbPO3. The crystal structure of Cs3(H1.5PO4)2(H2O)2 was re-evaluated on the basis of single-crystal X-ray diffraction data at − 173 °C, revealing that two adjacent hydrogen phosphate anions are connected by a very strong and non-symmetrical hydrogen bond, in contrast to the previously described symmetrical bonding situation derived from room temperature X-ray diffraction data. In the four title crystal structures, coordination numbers of the caesium cations range from 7 to 12. Graphic abstract

scholarly journals The reaction of 3,5-diphenyl-1,2-dithiolium-4-olate with aniline: the crystal structure of 1-phenylimino-2-phenylamino-3-phenylindene

1987 ◽  
Vol 65 (12) ◽  
pp. 2830-2833 ◽  
Author(s):  
David M. McKinnon ◽  
Peter D. Clark ◽  
Robert O. Martin ◽  
Louis T. J. Delbaere ◽  
J. Wilson Quail
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

3,5-Diphenyl-1,2-dithiolium-4-olate (1) reacts with aniline to form 1-phenylimino-2-phenylamino-3-phenylindene (3a). Under suitable conditions, 6-phenylbenzo[b]indeno[1,2-e]-1,2-thiazine is also formed. These structures are confirmed by alternative syntheses. The molecular structure of 3a has been determined by single crystal X-ray diffraction. Compound 3a crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 20.777(3) Å, b = 6.130(3) Å, c = 31.327(3) Å, 3 = 99.59(1)°, and Z = 8. The structure was solved by direct methods and refined by least squares to a final R = 0.055. The molecular structure of 3a shows the three phenyl containing substituents to have the planes of their ring systems tilted between 40° and 60° from the plane of the indene system due to steric repulsions.

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