The crystal structure of diethylene tetraxanthogen, the oxidation product of the diethylene dixanthate ion

1974 ◽  
Vol 27 (1) ◽  
pp. 27
Author(s):  
BF Hoskins ◽  
MR Hunt
Keyword(s):  
Oxidation Product ◽  
Least Squares Method ◽  
Ring Structure ◽  
The Novel ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
X Ray ◽  
Disulphide Bonds ◽  
A Site ◽  
Short Carbon

The structure of the oxidation product of the diethylene dixanthate anion, diethylene tetraxanthogen (Cl12H1606S8), has been determined by single crystal X-ray diffraction methods. The crystals are tetragonal of space group Z41/acd with a 15.798(1), c 17.755(1) �, containing eight molecules per unit cell. The structure was solved using conventional Patterson and Fourier methods and refined by a full-matrix least-squares method to R 0.055 for the 817 independent statistically significant reflections collected by counter methods. The crystals are composed of discrete molecules held together by van der Waals forces. Each molecule, situated about a site of symmetry 222, has the novel 22-membered ring structure involving disulphide bonds of length 2.035(2) �. The planarity of the dithiocarbonate moiety and the relatively short carbon-to-oxygen and carbon-to-sulphur bond lengths correlate with extensive π-electron delocalization over the group.

The crystal and molecular stucture of μ-Bis(diphenylarsino)methanehexacarbonyldi-μ-chloro-dirhenium(I)-n-hexane (4/1)

1975 ◽  
Vol 28 (6) ◽  
pp. 1201 ◽  
Author(s):  
CJ Commons ◽  
BF Hoskins
Keyword(s):  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
X Ray ◽  
Carbonyl Ligands ◽  
Rhenium Complex ◽  
Metal Atoms ◽  
A Site

The crystal and molecular structure of the n-hexane solvate of μ- bis(diphenylarsino)methane-hexacarbonyldi-μ-chloro-dirhenium(I), Re2(CO)6(Ph2AsCH2AsPh2)Cl2, has been determined by three-dimensional X-ray diffraction methods. The complex crystallizes in the space group Pī with a 15.763(1), b 19.077(1), c 12.233(1) Ǻ and α 88.745(10), β 110.506(5), γ 92.900(6)�. The structure was solved by conventional Patterson and Fourier methods and refined by a block-diagonal least- squares method to R and Rw of 0.045 and 0.054, respectively, for 7061 independent statistically significant reflections collected by counter methods. The crystal consists of discrete molecules of the complex and n-hexane held together by van der Waals forces. There are two molecules of the dirhenium complex in the crystallographic asymmetric unit with the n-hexane molecule situated about a site of symmetry ī. The binuclear rhenium complex contains bridging halogen atoms and a bridging diarsine ligand. Three carbonyl ligands are also bonded to each rhenium atom, giving the metal atoms approximately octahedral environments. The average Re-As, Re-Cl, and Re-C bond lengths are 2.58, 2.52, and 1.89 Ǻ respectively.

The crystal structure of tetraethylammonium Tris(O-ethylxanthato)tellurate(II): An example of five-coordinate pentagonal-planar geometry

1976 ◽  
Vol 29 (11) ◽  
pp. 2337 ◽  
Author(s):  
BF Hoskins ◽  
CD Pannan
Keyword(s):  
Crystal Structure ◽  
Least Squares Method ◽  
Three Dimensional ◽  
Planar Geometry ◽  
Maximum Deviation ◽  
Valence Shell ◽  
X Ray Diffraction ◽  
Electron Pairs ◽  
Fourier Methods ◽  
X Ray

The crystal structure of tetraethylammonium tris(O-ethylxanthato) tellurate(11), [Et4N] [Te(S2COEt)3], has been determined by single-crystal three-dimensional X-ray diffraction methods. Crystals are monoclinic of space group P21/c with four cation-anion pairs per unit cell which has the dimensions a 8.121(1), b 18.858(2), c 19.260(2) � and β 105.22(2)�. The structure was solved by the normal Fourier methods and was refined with anisotropic thermal parameters by a full-matrix least-squares method converging with R and Rw values of 0.061 and 0.082 for the 2404 independent statistically significant reflections collected by counter methods. The tris(ethylxanthato)tellurate(11) anion has a novel five-coordinate pentagonal-planar structure with only two of the xanthato ligands bidentate and with the Te-S bond distances having values in the range 2.503(4)-3.059(3)�. The TeS5 atoms are coplanar, the maximum deviation from the plane being 0.122 �. This, together with the intra-planar S...S distances of 3.340-3.661 �, indicates that the ligand atoms of the pentagonal plane are not over-crowded. The geometry of the anion configuration can be explained in terms of the VSEPR theory using a pentagonal-bipyramidal arrangement of the seven electron pairs in the valence shell of the tellurium.

A novel carbonyl bridging mode: the structure of the metal carbonyl complex [Mn2(CO)5(Ph2PCH2PPh2)2]

1975 ◽  
Vol 28 (8) ◽  
pp. 1663 ◽  
Author(s):  
CJ Commons ◽  
BF Hoskins
Keyword(s):  
Least Squares Method ◽  
Metal Carbonyl ◽  
Three Dimensional ◽  
Carbonyl Complex ◽  
X Ray Diffraction ◽  
Carbonyl Ligand ◽  
Fourier Methods ◽  
X Ray ◽  
Carbonyl Bond ◽  
Temperature Factors

The crystal structure of the solvated complex Mn2(CO)5(dpm)2,CH2Cl3,C6H14 (where dpm = Ph2PCH2PPh2) has been determined by three-dimensional X-ray diffraction methods. The crystals are monoclinic, of space group Cc, with a 19.650(3), b 16.908(2), c 22.253(4) Ǻ and β 130.89(1)�, containing four molecules per unit cell. The structure, solved by conventional Patterson and Fourier methods, was refined by a least- squares method, using individual isotropic temperature factors, to R and Rw of 0.105 and 0.125 respectively, for 1893 independent statistically significant reflections collected by counter methods. The crystals are molecular, being composed of discrete molecules of complex and solvent. The principal feature of interest in the binuclear manganese complex is the presence of a carbonyl ligand simultaneously bonded to both manganese atoms in a manner quite different from the normal symmetrical bridging mode. This novel arrangement, which seems to involve a metal-carbonyl bond analogous to that found for many metal-olefin complexes, accounts for the anomalously low carbonyl stretching frequency observed at 1645 cm-1. The Mn-Mn distance is 2.934(6) Ǻ.

Complexes of the dicyclohexylphosphinodithioformate anion involving the nickel triad metals: the crystal and molecular structures of the platinum(II) and palladium(II) derivatives

1984 ◽  
Vol 37 (1) ◽  
pp. 197 ◽  
Author(s):  
D Dakternieks ◽  
BF Hoskins ◽  
ERT Tiekink
Keyword(s):  
Phosphorus Atom ◽  
Least Squares Method ◽  
Central Atom ◽  
Three Dimensional ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
Full Matrix ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal and molecular structures of bis (dicyclohexylphosphinodithioformato-S,P)M, M[S2CP-(C6Hl1)2]2 where M = Pt (1) and Pd (2), have been determined by single-crystal three-dimensional X-ray diffraction methods. The isomorphous crystals are monoclinic, of space group P21/c with four molecules per unit cell which has dimensions for (1) a 14.732(4), b 15.11 8(4), c 16.000(3) � and β 120.90(2)� and for (2) a 14.721(2), b 15.142(2), c 15.986(2) � and β 120.80(1)�. The structures were solved by normal Fourier methods and were refined with anisotropic thermal parameters. A full-matrix least-squares method was used, involving 3454 and 5052 statistically significant reflections for (1) and (2) respectively with final R and Rw values of 0.058 and 0.055 for (1) and 0.038 and 0.039 for (2). The complexes are isostructural. The ligand coordinates in a bidentate manner to the central atom through the phosphorus atom and one of the sulfur atoms with the metal atom in a cis-planar environment.

Chemical and Electrochemical Heteroepitaxial Growth of Chalcogenide Semiconductors from Solutions

1996 ◽  
Vol 451 ◽  
Author(s):  
D. Lincot ◽  
M. J. Furlong ◽  
M. Froment ◽  
R. Cortes ◽  
M. C. Bernard
Keyword(s):  
Heteroepitaxial Growth ◽  
X Ray Diffraction ◽  
Basic Principles ◽  
Lattice Match ◽  
X Ray ◽  
Chalcogenide Semiconductors ◽  
Influence Of Temperature On ◽  
Deposition Processes ◽  
A Site ◽  
Site Selective

ABSTRACTChalcogenide semiconductors have been deposited epitaxially from aqueous solutions either chemically or electrochemically at growth rates of up to 0.7 μmhr−1. After recalling the basic principles of these deposition processes, results are presented concerning chemically deposited CdS on InP, GaP and CuInSe2 substrates, electrodeposited CdTe on InP, and CdSAnP heterostructures. Characterisation of these structures by RHEED, TEM, HRTEM, and glazing angle X ray diffraction allows to analyse the effects of substrate orientation, polarity, lattice match plus the influence of temperature on epitaxial growth. These results are discussed in terms of self organisation and a site selective growth mechanisms due to the free enegy of formation of each compound.

Ten-Vertex Polyhedral Monocarbaborane Chemistry. The Novel High-Yield Formation of the Ten-Vertex closo Compound [6-(PMe2Ph)-closo-1-CB9H9] from the Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11]

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
High Yield ◽  
Monoclinic Space Group ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
X Ray ◽  
Yield Formation ◽  
Boiling Toluene

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.

scholarly journals Some Novel Cobalt Diphenylphosphine Complexes: Synthesis, Characterization, and Behavior in the Polymerization of 1,3-Butadiene

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 4067
Author(s):  
Giovanni Ricci ◽  
Giuseppe Leone ◽  
Giorgia Zanchin ◽  
Benedetta Palucci ◽  
Alessandra Forni ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
And Behavior

Some novel cobalt diphenylphosphine complexes were synthesized by reacting cobalt(II) chloride with (2-methoxyethyl)diphenylphosphine, (2-methoxyphenyl)diphenylphosphine, and 2-(1,1-dimethylpropyl)-6-(diphenylphosphino)pyridine. Single crystals suitable for X-ray diffraction studies were obtained for the first two complexes, and their crystal structure was determined. The novel compounds were then used in association with methylaluminoxane (MAO) for the polymerization of 1,3-butadiene, and their behavior was compared with that exhibited in the polymerization of the same monomer by the systems CoCl2(PnPrPh2)2/MAO and CoCl2(PPh3)2/MAO. Some significant differences were observed depending on the MAO/Co ratio used, and a plausible interpretation for such a different behavior is proposed.

scholarly journals Synthesis and structure of 2,8-dimethyl-10,10-dichlorophenoxatellurine

2020 ◽  
Vol 44 (1) ◽  
pp. 9-11
Author(s):  
Farzin Mostaghimi ◽  
Daniel Duvinage ◽  
Enno Lork ◽  
Jens Beckmann
Keyword(s):  
Ring Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Tellurium Tetrachloride

Abstract The condensation of 4,4’-dimethyldiphenylether with tellurium tetrachloride yielded 2,8-dimethyl-10,10-dichlorophenoxatellurine (3), which was characterized by X-ray diffraction. Unlike the parent phenoxatellurine (1) and the 10,10,-dichlorophenoxatellurine (2) showing butterfly conformations, 3 reveals a planar ring structure.

scholarly journals Crystal Structure Refinements of Four Monazite Samples from Different Localities

Minerals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1028 ◽  
Author(s):  
M. Mashrur Zaman ◽  
Sytle M. Antao
Keyword(s):  
Crystal Structure ◽  
Electron Probe ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Large Unit Cell ◽  
A Site

This study investigates the crystal chemistry of monazite (APO4, where A = Lanthanides = Ln, as well as Y, Th, U, Ca, and Pb) based on four samples from different localities using single-crystal X-ray diffraction and electron-probe microanalysis. The crystal structure of all four samples are well refined, as indicated by their refinement statistics. Relatively large unit-cell parameters (a = 6.7640(5), b = 6.9850(4), c = 6.4500(3) Å, β = 103.584(2)°, and V = 296.22(3) Å3) are obtained for a detrital monazite-Ce from Cox’s Bazar, Bangladesh. Sm-rich monazite from Gunnison County, Colorado, USA, has smaller unit-cell parameters (a = 6.7010(4), b = 6.9080(4), c = 6.4300(4) Å, β = 103.817(3)°, and V = 289.04(3) Å3). The a, b, and c unit-cell parameters vary linearly with the unit-cell volume, V. The change in the a parameter is large (0.2 Å) and is related to the type of cations occupying the A site. The average <A-O> distances vary linearly with V, whereas the average <P-O> distances are nearly constant because the PO4 group is a rigid tetrahedron.

scholarly journals Insertion of Phosphenium Ions into a Bicyclo[1.1.0]Tetraphosphabutane Iron Complex

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3920
Author(s):  
Martin Weber ◽  
Gábor Balázs ◽  
Alexander V. Virovets ◽  
Eugenia Peresypkina ◽  
Manfred Scheer
Keyword(s):  
Diffraction Analysis ◽  
Room Temperature ◽  
31P Nmr ◽  
Spectroscopic Studies ◽  
Iron Complex ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Phosphenium Ions

By reacting [{Cp‴Fe(CO)2}2(µ,η1:1-P4)] (1) with in situ generated phosphenium ions [Ph2P][A] ([A]− = [OTf]− = [O3SCF3]−, [PF6]−), a mixture of two main products of the composition [{Cp‴Fe(CO)2}2(µ,η1:1-P5(C6H5)2)][PF6] (2a and 3a) could be identified by extensive 31P NMR spectroscopic studies at 193 K. Compound 3a was also characterized by X-ray diffraction analysis, showing the rarely observed bicyclo[2.1.0]pentaphosphapentane unit. At room temperature, the novel compound [{Cp‴Fe}(µ,η4:1-P5Ph2){Cp‴(CO)2Fe}][PF6] (4) is formed by decarbonylation. Reacting 1 with in situ generated diphenyl arsenium ions gives short-lived intermediates at 193 K which disproportionate at room temperature into tetraphenyldiarsine and [{Cp‴Fe(CO)2}4(µ4,η1:1:1:1-P8)][OTf]2 (5) containing a tetracyclo[3.3.0.02,7.03,6]octaphosphaoctane ligand.

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