Preparation and Structure of Tetraphenylarsonium Bis[1,2-Dicyanoethenedithiolato]oxotechnetate(V)

1988 ◽  
Vol 41 (1) ◽  
pp. 151 ◽  
Author(s):  
SF Colmanet ◽  
MF Mackay
Keyword(s):  
Bond Distance ◽  
Apical Position ◽  
Space Group ◽  
Ethanol Yields ◽  
Oxo Ligand

The reaction of sodium 1,2-dicyanoethenedithiolate with [AsPh4][TcOCl4] in ethanol yields crystals of [AsPh4][ TcO ( mnt )2] (1). Crystals of (1) are monoclinic and belong to the space group P21/c with a 12.636(1), b 13.749(1), c 18.484(1)Ǻ, β 93.49(1)� with Z 4. Refinement on 3669 data measured with Cu Kα radiation converged at R 0.063. The structure consists of [ TcO ( mnt )2]- anions and [AsPh4]+ cations. The technetium(V) atom is five-coordinate with the four sulfur atoms in the basal positions and the oxo ligand in the apical position, to give a distorted square-pyramidal environment about the technetium. The Tc =O bond distance is 1.655(6)Ǻ.

Preparation and Structure of Tetraphenylarsonium Bis(Benzene-1,2-Dithiolato)Oxotechnetate(V)

1987 ◽  
Vol 40 (7) ◽  
pp. 1301 ◽  
Author(s):  
SF Colmanet ◽  
MF Mackay
Keyword(s):  
Crystal Structure ◽  
Aqueous Alcohol ◽  
X Ray Diffraction ◽  
Apical Position ◽  
Space Group ◽  
X Ray ◽  
Oxo Ligand

The reaction of benzene-1,2-dithiol (bdtH2) with [AsPh4] [TcOCl4] in aqueous alcohol yields crystals of [AsPh4] [ TcO ( bdt )2] (1) from acetonitrilelethanol. The crystal structure of (1) has been determined by X-ray diffraction and found to be isostructural with [PPh4] [ MoO ( bdt )2]. Crystals art monoclinic and belong to the space group Cc with a 12.652(1), b 15.783(1), c 16.622(1) �, β 93.03(1)� with Z 4. Refinement on 2828 diffractometer data measured with Cu Ka radiation converged at R 0.030. The structure consists of [ TcO ( bdt )2]- anions and [AsPh4]+ cations. The technetium(V) atom is five-coordinate, with the four sulfur atoms in the basal positions and the oxo ligand in the apical position, to give a distorted square-pyramidal environment about the technetium.

scholarly journals Synthesis and molecular structures of monooxo aryl complexes of osmium(VI)

2001 ◽  
Vol 79 (5-6) ◽  
pp. 607-612 ◽  
Author(s):  
Man-Kit Lau ◽  
Joyce LC Chim ◽  
Wing-Tak Wong ◽  
Ian D Williams ◽  
Wa-Hung Leung
Keyword(s):  
Solid State ◽  
Molecular Structures ◽  
Cyclic Voltammograms ◽  
Apical Position ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Aryl Complexes ◽  
Oxo Ligand ◽  
Solid State Structures

Reaction of [OsO4] with C7H7MgBr (C7H7 = 2-methylphenyl) followed by column chromatography afforded the reported osmium tetraaryl [Os(C7H7)4] along with the oxo-osmium(VI) ([OsO(C7H7)4]) (1) (13%) and the dioxo-osmium(VI) ([OsO2(C7H7)2]) (2) (25%) complexes. Treatment of [OsO4] with C8H9MgBr (C8H9 = 2,5-dimethylphenyl) gave a mixture of [Os(C8H9)4] (3) (34%) and [OsO(C8H9)4] (4) (4%) while that with C8H9OMgBr (C8H9O = 4-methoxy-2-methylphenyl) afforded [OsO(C8H9O)4] (5) in 20% yield. Oxidation of 3 with 3-chloroperoxybenzoic acid afforded 4 in good yield. The solid-state structures of 1 and 4 have been established by X-ray crystallography. Crystals of 1 are tetragonal with a = 13.080(1) and c = 6.6506(5) Å, V = 1137.9(1) Å3, Z = 2, and space group of P4/n; while those of 4 are tetragonal with a = 13.593(2) and c = 7.377(2) Å, V = 1363.0(5) Å3, Z = 4, and space group of P4/n. The geometry around osmium in both complexes is square pyramidal with the oxo ligand occupying apical position. The Os—O and Os—C distances in 1 are 1.652(2) and 2.084(1) Å, respectively, while those in 4 are 1.688(7) and 2.088(4) Å, respectively. The cyclic voltammograms of the monooxo aryl osmium(VI) compounds show reversible Os(VI/V) couple at around –1.4 V vs. ferrocene/ferrocenium couple.Key words: osmium(VI), oxo aryl complexes.

Zur Umsetzung von ReO2I(PPh3)2 mit PhNCO. Synthese und Kristallstrukturen von ReO2I(PPh3)2 · CHCl3, [ORe(OCONPh)I(PPh3)]3, Re(NPh)(NH2Ph)I2(PPh3)(OCONHPh) und Re(NPh)(NH2Ph)I2(PPh3) ( OReO3) / On the Reaction of ReO2I(PPh3)2 with PhNCO. Synthesis and Crystal Structures of ReO2I(PPh3)2 · CHCl3, [ORe(OCONPh)I(PPh3)]3, Re(NPh)(NH2Ph)I2(PPh3)(OCONHPh) and Re(NPh)(NH2Ph)I2(PPh3) ( OReO3)

1991 ◽  
Vol 46 (2) ◽  
pp. 235-244 ◽  
Author(s):  
S. Schmid ◽  
J. Strähle
Keyword(s):  
Hydrolysis Product ◽  
Phosphine Ligands ◽  
Partial Hydrolysis ◽  
Monoclinic Space Group ◽  
Linear Arrangement ◽  
Triclinic Space Group ◽  
Metal Centers ◽  
Space Group ◽  
Trimeric Complex ◽  
Oxo Ligand

PhNCO reacts with oxo ligands at metal centers to form phenyl nitrene complexes. As an intermediate of this reaction we obtained with ReO2I(PPh3)2 (1) the trimeric complex [ORe(OCONPh)I(PPh3)]3 (2) in which the PhNCO moiety was added to an oxo ligand to form an N -phenyl carbamato group. This group acts as a bridging ligand chelating one Re atom via its N and one O atom and coordinating an other Re atom by its second O atom . 2 crystallizes as 2 · 2 CHCl3 in the triclinic space group P1̄ with a = 1423.1(5), b = 2443.3(7), c = 1403.8(6) pm , α = 92.31(3), β = 94.76(3), γ = 81.48(3)°, and Z = 2. From the mother liquor of 2 after a few days Re(NPh)(NH2Ph)I2(PPh3)(OCONHPh) (3) is formed as a partial hydrolysis product. 3 is monoclinic with the space group P21/n and a = 1163.0(4), b = 2527.0(3), c = 1243.9(5) pm, β = 98.04°, Z = 4. The Re atom exhibits an octahedral coordination w ith the two I atom s in a ?ra«s-arrangem ent and the phenyl nitrene ligand trans to the m onodentate PhN HCO2 group. The coordination is completed by a phosphine and an aniline ligand. Reaction of 2 with excess PPh3 yields 1. It crystallizes from CHCl3 as 1 · CHCl3 in the monoclinic space group P21/n with a = 975.9(3), b = 2731(1), c = 1417.3(6) pm , β = 93.35° and Z = 4. In 1 the Re atom is pentacoordinated in form of a trigonal bipyram id with the two phosphine ligands in axial positions. A solution of 2 in THF forms Re(NPh)(NH2Ph)I2(PPh3) (OReO3) (4) upon exposure to air at room temperature. 4 is obtained as orthorhombic crystals with the space group Pca21 and a = 1727(1), b = 1064.2(4), c = 1765.7(9) pm , Z = 4, and is an analogue of 3 from which it can be derived by substituting the carbamato ligand by a perrhenat ion. In 3 and 4 the phenyl nitrene ligand is bound by a Re = N triple bond of 172 pm in a linear arrangement Re = N - Ph .

Darstellung und Kristallstruktur des Bis(diisobutylammonium)-heptasulfids [H2N(i-C4H9)2]2S7 / Synthesis and Crystal Structure of Bis(diisobutylammonium)-heptasulfide [H2N(i-C4H9)2]2S7

1993 ◽  
Vol 48 (12) ◽  
pp. 1732-1736 ◽  
Author(s):  
C. Müller ◽  
P. Böttcher
Keyword(s):  
Crystal Structure ◽  
Orthorhombic Space Group ◽  
Trans Conformation ◽  
Torsion Angles ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Lattice Constants ◽  
Ethanol Yields ◽  
The Common

The reaction of diisobutylamine, H2S, and sulfur in a mixture of dimethylformamide, formamide, and ethanol yields orange crystals of bis(diisobutylammonium)-heptasulfide. The compound crystallizes in the centrosymmetric orthorhombic space group Pbca, the lattice constants are a = 11.234(4), b = 17.875(7), c = 27.009(10) Å. The S72-chain does not have the common helical all-trans-conformation, but a mixed conformation trans-cis-trans (sequence of the signs of torsion angles + + - - and - - + +).

Primäre und sekundäre Ethyl-und i-Propylsulfoniumsalze sowie Kristallstruktur von i-C3H7SH2+SbF6- [1]

1996 ◽  
Vol 51 (2) ◽  
pp. 277-285
Author(s):  
Rolf Minkwitz ◽  
Ulrike Lohmann ◽  
Hans Preut
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Bond Distance ◽  
Crystal Structure Analysis ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Spectroscopic Methods ◽  
Sulfonium Salt ◽  
Space Group

Abstract The synthesis of salts of the type RnSH3-n+MF6- (R = C2H5, i-C3H7; n = 1, 2; M = As, Sb) by protonation of the corresponding thiols and sulfides in the superacid systems HF/MF5 is reported. The salts have been characterized by vibrational and NMR spectroscopic methods. Isopropylsulfonium hexafluoroantimonate is the first known example of a sulfonium salt, for which a SH bond distance has been determined by a crystal structure analysis, i-C3H7SH2+SbF6- crystallizes in the monoclinic space group P21/m with a = 568.0(4), b = 801.1(6), c = 1019.7(8) pm, β = 82.63(6) °, with two formula units per unit cell.

Die Kristallstruktur des Phosphaniminato-Komplexes [TiCl3(NPPh3)•TiCl4]2 / Crystal Structure of the Phosphorane Iminato Complex [TiCl3(NPPh3)•TiCl4]2

1996 ◽  
Vol 51 (9) ◽  
pp. 1359-1362 ◽  
Author(s):  
Frank Weller ◽  
Fritjof Schmock ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Double Bond ◽  
Ir Spectroscopy ◽  
Structure Determination ◽  
Title Compound ◽  
Titanium Tetrachloride ◽  
Bond Distance ◽  
Space Group ◽  
Yellow Orange ◽  
Centrosymmetric Dimers

The title compound was prepared from Me3SiNPPh3 and an excess of titanium tetrachloride. It forms yellow-orange crystals, which were characterized by IR spectroscopy and by crystal structure determination. Space group P21/n, Z = 2; lattice dimensions at 20°C: a = 1189.2(1), b - 1718.5(1), c = 1238.1(1) pm, β = 93.363(7)°. The compound forms centrosymmetric dimers in which the titanium atoms are triply and doubly bridged by chlorine atoms to give face- and edgesharing octahedra, respectively. In the linear units [Ti]=N =PPh3 the Ti-N bond distance of 171.6(3) pm corresponds to a double bond.

Darstellung und Kristallstruktur des Bis(trimethylammonium)hexasulflds [HN(CH3)3]2S6 / Preparation and Crystal Structure of Bis(trimethylammonium)hexasulfide [HN(CH3)3]2S6

1994 ◽  
Vol 49 (4) ◽  
pp. 489-493 ◽  
Author(s):  
C. Müller ◽  
P. Böttcher
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Trans Conformation ◽  
Torsion Angles ◽  
Space Group ◽  
Lattice Constants ◽  
Ethanol Yields

The reaction of trimethylamine, H2S, and sulfur in ethanol yields orange crystals of bis(trimethylammonium) hexasulfide. The com pound crystallizes in the centrosymmetric monoclinic space group P 2/c. The lattice constants are a = 10.310(7), b = 5.752(2), c = 13.348(10) Å, β = 98.41(6)°. The S26-chain has a helical all-trans-conformation (sequence of the signs of torsion angles +++ and --- ).

Facets of Induced Internal Redox Involving WS42 - and WSe42 - : Synthesis and X-Ray Crystal Structures of syn-W2S2(μ-S)2(S2PPh2)2 and WO(Se2)(S2CNEt2)2

2000 ◽  
Vol 53 (9) ◽  
pp. 779 ◽  
Author(s):  
Edward R. T. Tiekink ◽  
Aston A. Eagle ◽  
Charles G. Young
Keyword(s):  
Crystal Structures ◽  
Redox Process ◽  
Space Group ◽  
X Ray ◽  
Complex Features ◽  
Oxo Ligand

Reaction of (NEt4)2[WS4] and [S2PPh2]2 in acetonitrile results in the formation of diamagnetic, orange syn-W2S2(µ-S) 2(S2PPh2)2 by an induced internal redox process. Crystals of the toluene solvate W2S2(µ-S) 2(S2PPh2)2 . C7H8 are triclinic and belong to space group P1– with a 13.845(5), b 16.536(7), c 8.387(2) Å, α 99.75(3), β 95.51(3), γ 83.08(3)˚, and Z 2. Refinement of 5445 data converged at R 0.038 and Rw 0.038. The complex possesses a syn-[W V 2S2(µ-S)2]2+ core with a W–W bond of 2.8161(5) Å and two terminal W=S bonds of 2.097(3) and 2.096(3) Å. The W-(µ-S) bond distances are in the range 2.310(2)–2.315(2) Å. Each of the five-coordinate, square-pyramidal tungsten atoms is further coordinated by a bidentate dithiophosphinate ligand with W–S bond distances ranging from 2.464(2) to 2.481(2) Å. Extended reaction of (NH4)2[WSe4] and [S2CNEt2]2 in acetonitrile produces green WS(Se2)(S2CNEt2)2 and red WO(Se2)(S2CNEt2)2 in 40% and 15% yields, respectively. Crystals of WO(Se2)(S2CNEt2)2 are monoclinic and belong to space group P21/n with a 9.609(6), b 15.053(7), c 13.120(9) Å, β 100.08(4)˚, and Z 4. Refinement of 2473 data converged at R 0.039 and Rw 0.039. The seven-coordinate, pentagonal bipyramidal complex features C1 symmetry, an axial oxo ligand (W=O 1.705(6) Å), an equatorial, side-on bonded diselenido ligand (W–Se(1) 2.509(1), W–Se(2) 2.547(1) Å, Se(1)–Se(2) 2.306(2) Å) and two bidentate dithiocarbamate ligands.

A New Copper (II) Complex with the N,N'-Bis(antipyryl-4-methyl)-piperazine (BAMP) Ligand: [Cu(BAMP)](ClO4)2

2002 ◽  
Vol 57 (12) ◽  
pp. 1454-1460 ◽  
Author(s):  
Otilia Costișor ◽  
Ramona Tudose ◽  
Ingo Pantenburg ◽  
Gerd Meyer
Keyword(s):  
Crystal Structure ◽  
Copper Complex ◽  
Structural Parameters ◽  
Complex Molecule ◽  
Lattice Parameters ◽  
Tetragonal Symmetry ◽  
Apical Position ◽  
Space Group ◽  
Symmetry Space ◽  
Symmetry Space Group

The synthesis of the Mannich base N,N’-bis(antipyryl-4-methyl)-piperazine (BAMP) (1), its crystal structure as well as the synthesis and the crystal structure of the copper complex Cu(BAMP)(ClO4)2 (2) are reported. C28H34N6O2 ∙ 4H2O (BAMP ∙ 4H2O) crystallizes with triclinic symmetry, space group P1̄, lattice parameters: a = 704,9(2), b = 983,4(2), c = 1198,9(3) pm, α = 68,72°, β = 73,62°, γ = 78,49°. The copper-complex Cu(BAMP)(ClO4)2 crystallizes with tetragonal symmetry, space group P42/n, lattice parameters: a = 2295,1(3), c = 1412,2(2) pm. The copper(II) atom is five-coordinate by the two nitrogen atoms belonging to the piperazine ring and the oxygen atoms of the antipyrinemoieties. The geometry of the copper(II) atom can be described as a square-based pyramid with the N2O2 donor atoms of BAMP forming the basal plane and an oxygen atom of the neighbouring complex molecule occupying the apical position. BAMP acts as a tetradentate ligand, which incorporates a piperazine-fused ring. The structural parameters illustrate well the reinforcing effect exerted by the double “straps” of the piperazine molecule.

Preparation and Structure of Tetraphenylarsonium Tris(1,2-dicyanoethenedithiolato)technetate(IV)

1988 ◽  
Vol 41 (7) ◽  
pp. 1127 ◽  
Author(s):  
SF Colmanet ◽  
MF Mackay
Keyword(s):  
Crystal Structure ◽  
Distorted Octahedron ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ethanol Yields

The reaction of sodium 1,2-dicyanoethenedithiolate [( mnt )Na2] with (NH4)2 [TcBr6] in ethanol yields crystals of (AsPh4)2 [ Tc ( mnt )3] (1) after precipitation with AsPh4Cl. The crystal structure of (1) has been determined by X-ray diffraction. Crystals are orthorhombic, space group Pbcn , a 20.256(1), b 15.513(1), c 18.274(1)Ǻ, Z 4. Refinement on 2910 diffractometer data measured with Cu Kα radiation converged at R 0.056. The structure consists of [ Tc ( mnt )3]2- anions and (AsPh4)+ cations . The technetium(IV) atom is coordinated to six sulfur atoms to give a distorted octahedron.

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