Reactions of benzo[b]thiophene with some aqueous platinum metal species at elevated temperatures

1991 ◽  
Vol 69 (4) ◽  
pp. 590-598 ◽  
Author(s):  
Peter D. Clark ◽  
James F. Fait ◽  
Colin G. Jones ◽  
Martin J. Kirk
Keyword(s):  
Elevated Temperatures ◽  
Fourier Method ◽  
Platinum Metal ◽  
Metal Species ◽  
Monoclinic Space Group ◽  
Mechanistic Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
A Cell

The desulfurization of benzo[b]thiophene 1 with aqueous transition metal species in the presence of various hydrocarbons at elevated temperatures is described. Mechanistic studies have shown that treatment of 1 with solutions of RuCl3 and other platinum metal species results in the formation of 2,3-dihydrobenzo[b]thiophene 2 and ethylbenzene 3 as major products. Metal coordinated species are probable intermediates in the formation of 2 and hydrocarbon products. 2 readily coordinates to PdCl2 to form square-planar trans-dichlorobis(2,3-dihydrobenzo[b]thiophene) palladium(II), which decomposes to ethylbenzene at 300 °C. The crystal structure of the complex was determined by a single crystal X-ray diffraction study. The complex crystallized in the monoclinic space group C 2/c with Z = 8 in a cell of dimensions a = 23.057 (3), b = 9.711 (1), c = 15.227 (2) Å and β = 99.74(1)°. The structure was solved by the Fourier method and was refined by full-matrix least-squares calculations to R = 0.042 for 2537 observed data with I > 2.5σ(I). Key words: benzo[b]thiophene, desulfurization, platinum metal species.

scholarly journals Crystal and molecular structure and 31P and 195Pt nmr spectroscopy of [Pt3S2(PMe2Ph)6][BEt4]2; a trinuclear complex containing triply-bridging sulphide ligands

1984 ◽  
Vol 62 (4) ◽  
pp. 696-702 ◽  
Author(s):  
Gordon William Bushnell ◽  
Keith Roger Dixon ◽  
Reiko Ono ◽  
Alan Pidcock
Keyword(s):  
Trinuclear Complex ◽  
Complete Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Interactions ◽  
Nuclear Magnetic Resonance Spectra ◽  
Square Planar ◽  
Metal Metal ◽  
Pd Complexes

An X-ray diffraction study of [Pt3S2(PMe2Ph)6][BEt4]2 shows that it crystallises in the monoclinic space group, C2/c, with a = 15.447(2), b = 18.033(3), c = 26.505(5) Å, β = 96.73(2)°. The cation consists of three, distorted, square-planar cis-PtS2(PMe2Ph)2 moieties combined by sharing of the two sulphur atoms to produce a central Pt3S2 unit with C2 symmetry and Pt—Pt distances of 3.182(1) Å (one edge) and 3.108(1) Å (two edges). Complete analysis and computer simulation of 31P{1H} and 195Pt{1H} nuclear magnetic resonance spectra give values for 1J(Pt—P), 3202 Hz; 3J(Pt—P), −25 Hz; and 2J(Pt—Pt), 476 Hz. The structure is compared with previous results for analogous Ni and Pd complexes and the structural and nmr parameters are discussed with reference to the possibility of metal–metal interactions.

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.

Preparation and Crystal Structure of Silver(I) Anthranilate

1999 ◽  
Vol 52 (4) ◽  
pp. 325 ◽  
Author(s):  
Graham Smith ◽  
Colin H. L. Kennard ◽  
Karl A. Byriel
Keyword(s):  
Major Constituent ◽  
Monoclinic Space Group ◽  
Zigzag Chain ◽  
Aminobenzoic Acid ◽  
X Ray Diffraction ◽  
Amine Nitrogen ◽  
Chain Polymer ◽  
X Ray ◽  
A Cell ◽  
Planar Angle

Silver(I) anthranilate, [Ag2(C7H6NO2)2]n, was isolated as the major constituent in the attempted preparation of the adduct of anthranilic acid (2-aminobenzoic acid) with silver(I) p-toluenesulfonate and its structure has been determined by using single-crystal X-ray diffraction. Crystals of the complex are monoclinic, space group P 21/n, with two dimers in a cell of dimensions a 5·3516(8), b 4·9746(2), c 25·386(5) Å, β 91· 547(8)°. The complex repeating unit comprises a distorted centrosymmetric biscarboxylato(-O,O′)-bridged dimer [Ag−O, 2·223, 2·409(4) Å; Ag---Ag 2·9128(9) Å] but has, in addition, a third bond to an adjacent amine nitrogen [Ag−N, 2·301(5) Å], which extends the structure into a zigzag chain polymer. The stereochemistry about each Ag centre is distorted trigonal planar [angle range, 89·9−142·9(2)°]. Relatively short inter-dimer Ag---Ag separations [2·989(1) Å] are also present.

The Crystal and Molecular Structure of Pentane-2,4-dionato-(2,3,5,6-tetrahepto-2,3-dicarbomethoxo[2.2.1]bicycloheptadiene)rhodium(I), Rh(C5H7O2) (C7H6(CO2CH3)2)

1975 ◽  
Vol 53 (18) ◽  
pp. 2707-2713 ◽  
Author(s):  
Debbie Allen ◽  
Colin James Lyne Lock ◽  
Graham Turner ◽  
John Powell
Keyword(s):  
Crystal And Molecular Structure ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Intensity Data ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Square Planar ◽  
Rhodium Atom

The crystal and molecular structures of pentane-2,4-dionato-(2,3,5,6-tetrahapto-2,3-dicarbomethoxo[2.2.1]bicycloheptadienerhodium(I), Rh(C5H7O2)(C7H6(CO2CH3)2), have been measured by single crystal X-ray diffraction. The orange crystals are monoclinic, space group P21/c, Z = 4, a = 9.245(4), b = 9.003(4), c = 21.680(15) Å, β = 113.41(5)°. The calculated and observed densities are 1.645 and 1.642(5) respectively. Intensity data were collected on a Syntex [Formula: see text] diffractometer and a full matrix least squares refinement on 3010 observed reflections leads to a conventional R = 0.0660. The structure can be considered as a roughly square planar arrangement of ligands around the rhodium atom composed of two β-ketoenolate oxygen atoms (Rh—O, 2.037(5) and 2.025(5) Å ) and the centers of the two ethylenic groups. The Rh—C distances for the olefin group attached to the two carbomethoxo groups, 2.117(8), 2.108(8) Å, appear to be slightly larger than those for the other olefinic group, 2.087(7), 2.082(6), and the corresponding C=C distances of 1.375(10) and 1.410(9) Å are different at the 95% confidence level.

Crystal and molecular structure of Z- and E-1,2-dichloro-1,2-bis(2-chlorophenyl)ethylene. An X-ray and NMR study

1995 ◽  
Vol 73 (9) ◽  
pp. 1520-1525
Author(s):  
Luciano Antolini ◽  
Ugo Folli ◽  
Dario Iarossi ◽  
Adele Mucci ◽  
Silvia Sbardellati ◽  
...  
Keyword(s):  
Chemical Shifts ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Nmr Study ◽  
Phenyl Rings ◽  
A Cell ◽  
C Nmr

The crystal structures of the title compounds were determined by single crystal X-ray diffraction techniques. The molecule of the Z isomer, which crystallizes in the monoclinic space group C2/c with Z = 4 in a cell of dimensions a = 14.891 (2), b = 10.780(2), c = 8.769(1) Å, β = 97.47(2)°, V = 1395.7(7) Å3 has crystallographic twofold symmetry. The E form crystallizes in the orthorhombic space group Pbca with a = 11.730(1), b = 6.932(1), c = 16.841(1) Å, V = 1369.4(2) Å3 and Z = 4. Its molecules have crystallographically dictated [Formula: see text] symmetry. In both isomers the phenyl rings are roughly perpendicular to the average ethylene plane. The atoms characterizing this plane show significant deviations from planarity in the Z isomer. Marked bond-angle distortions at the ethene carbons of both structures are observed. The 1H and 13C NMR spectra of the compounds were measured and, particularly in the case of the 1H chemical shifts, fall into two quite separate spectral regions. At low temperature, two conformational isomers, those with different relative orientation of the C—Cl bonds of the phenyl rings, are observed in the spectrum of each compound. Keywords: chlorostilbenes, overcrowded molecules. X-ray structure, conformations, NMR spectroscopy.

Synthesis and Structure of a Palladium(II) Chloride Complex with 2-(2-Methyl-3-phenyl-isoxazolidin-5-yl)-pyridine

2000 ◽  
Vol 55 (5) ◽  
pp. 373-376 ◽  
Author(s):  
Andrey B. Lysenko ◽  
Oleg V. Shishkin ◽  
Rostislav D. Lampeka
Keyword(s):  
Chelate Ring ◽  
Organic Ligand ◽  
Chloride Complex ◽  
Monoclinic Space Group ◽  
Equatorial Orientation ◽  
X Ray Diffraction ◽  
Methyl Group ◽  
X Ray ◽  
H Nmr ◽  
Square Planar

The 1:1 complex of palladium(II) chloride with 2-(2-methyl-3-phenyl-isoxazolidin-5-yl)- pyridine (L) has been prepared and studied by means of elemental analysis, 1H NMR spectroscopy and X-ray diffraction (monoclinic, space group P21/n with parameters: a = 8.141(2), b = 9.750(2),c = 20.691(6)Å ,β = 95.62(3)°,V = 1634.4(7)Å3 ,Z = 4 ;R1= 0.054 and wR2= 0.144 for 3352 unique reflections). A square-planar coordination polyhedron has been established for the palladium atom both in acetone solution and in the solid state. The organic ligand is coordinated toometal in a bidentate manner via nitrogen atoms of the pyridine substituent (Pd-N(2) 2.125(3) Å) and the isoxazolidine heterocycle (Pd-N(l) 2.102(3) Å). The other two coordination positions of palladium are occupied by chlorine atoms (Pd-Cl(l) 2.321(1) and Pd-Cl(2) 2.333(1) Å). The six-membered chelate ring formed by Pd, N(2), C(4), C(1), 0(1) and N (1) possesses a “twist-tub” conformation. The isoxazolidine cycle has an envelope conformation with an equatorial orientation of the methyl group.

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.

Reactions of "cyclen-" and "cyclam-phosphorane" with [Pt2Cl4(PEt3)2]. Monodentate and bidentate complexes and the crystal and molecular structure of [PtCl(PEt3)(cyclamPH)]Cl•CH2Cl2

1989 ◽  
Vol 67 (1) ◽  
pp. 48-53 ◽  
Author(s):  
David Eric Berry ◽  
Jane Browning ◽  
Gordon William Bushnell ◽  
Keith Roger Dixon ◽  
Alan Pidcock
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Simple Formula ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray ◽  
Square Planar ◽  
Coordination Plane

Reaction of "cyclamphosphorane" (cyclamPH) with [Pt2Cl4(PEt3)2] yields [PtCl(PEt3)(cyclamPH)]Cl. The complex crystallizes as a dichloromethane solvate in the monoclinic space group P21/n, with a = 13.877(3), b = 23.231(7), c = 8.295(2)Å, β = 91.86(4)°, and an X-ray diffraction study shows square planar platinum coordination in which the labile proton of cyclamPH has transferred from phosphorus to nitrogen and the ligand is attached via simple [Formula: see text] chelation. The phosphorus is trans to chlorine in the platinum coordination plane.The corresponding product, trans-[PtCl2(PEt3)(cyclenPH2)]Cl, derived from reaction of "cyclenphosphorane" (cyclenPH) with [Pt2Cl4(PEt3)2], is shown by NMR studies to have a quite different structure in which the ligand is protonated at two nitrogen sites but not at phosphorus. The phosphorus is pentacoordinate with four attachments to nitrogen atoms and one to platinum. The two chlorine atoms are mutually trans in the platinum coordination plane. Keywords: crystal structure, cyclenphosphorane reaction, cyclamphosphorane reaction, X-ray diffraction.

The crystal structures of two isomers of a macrocyclic binuclear compound each containing both divalent and trivalent cobalt

1975 ◽  
Vol 28 (12) ◽  
pp. 2593 ◽  
Author(s):  
BF Hoskins ◽  
GA Williams
Keyword(s):  
Bromine Atom ◽  
Fourier Method ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
R Factor ◽  
A Cell ◽  
Coordinated Water

The compound Lco2Br3,2H2O (where L is a binucleating ligand derived from the macrocycle LH2 formed by condensation of two molecules each of propane-1,3-diamine and 2-hydroxy-5- methylisophthalaldehyde) was found to occur in two crystalline forms. The structures of both have been determined by single-crystal X-ray diffraction techniques, revealing that each corresponds to a different geometrical isomer of composition Lco2Br3,2H2O. Each structure was determined by the conventional Patterson-Fourier method and refined by a least-squares procedure, with only the Co, Br, N and O atoms being refined anisotropically. The first form, designated the A-isomer, crystallizes in the orthorhombic space group Pn21a with four formula units in a cell of dimensions a 15.173(1), b 17.370(2) and c 10.493(1) Ǻ. The structure refined to a conventional R-factor of 0.074 by means of 1883 unique reflections collected by counter methods. The second form, or B-isomer, crystallizes in the monoclinic space group P21 with two formula units in a cell of dimen- sions a 10.676(1), b 15.235(2), c 9.304(1) Ǻ and β 111.83(2)°. The structure refined to a conventional R-factor of 0.101 by means of 2006 independent reflections collected by counter methods. Both isomers are composed of discrete bromide anions together with discrete binuclear cations of com- position [Lco2Br2,2H2O]+, each containing one cobalt(II) and one cobalt(III) atom with a Co...Co distance of 3.13 Ǻ. In both isomers the cobalt atoms are in octahedral environments. In the A-isomer two bromine atoms are bonded to the cobalt(III) atom in positions perpendicular to the ligand N2O2 donor plane, with the two water molecules occupying similar positions about the cobalt((II). But in the B-isomer, one water molecule and one bromine atom are bonded to each of the cobalt(III) and the cobalt((II) atoms in the comparable positions. In both structures the ionic bromide is involved in a hydrogen-bonding scheme with the coordinated water molecules.

Metal complexes of dicamba: the crystal and molecular structures of dicamba(3,6-Dichloro-2-methoxybenzoic acid) and catena-μ-Aqua-diaquabis(3,6-dichloro-2-methoxybenzoato)zinc(II) dihydrate

1983 ◽  
Vol 36 (11) ◽  
pp. 2175 ◽  
Author(s):  
G Smith ◽  
EJ O'Reilly ◽  
CHL Kennard
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bridging Ligand ◽  
Methoxy Groups ◽  
A Cell ◽  
Methoxybenzoic Acid

The crystal structures of the herbicide, dicamba (3,6-dichloro-2-methoxybenzoic acid) and the zinc(II) complex of this acid, {[Zn(dicamba)2(H2O)3].2H2O}}n (1), have been determined from X-ray diffraction data and refined by least squares to final residuals of 0.034 and 0.043 respectively. Dicamba is triclinic, space group P1, Z 2 with a cell a 7.232(1), b 7.971(1), c 9.050(3) �, α 102.76(3), β 91.33(3), γ 110.38(1)�, while (1) is monoclinic, space group P21/n, Z 4 with a cell a 10.467(1), b 8.135(3), c 28.079(2) �, β 96.497(7)�. Dicamba forms hydrogen-bonded cyclic dimers [O---O, 2.655(7) �] with the carboxyl and the methoxy groups synclinal to the benzene ring. The dicamba ligands retain their conformation in the ZnII complex and are cis-related and unidentate [Zn-0,2.083,2.095(4) �]. Three of the waters are coordinated [Zn-0, 2.036, 2.055, 2.099(4) �] with one of these also acting as a bridging ligand between the octahedral zinc centres [Zn-0, 2.326(4) �], giving a 'linear' polymer structure [Zn-0-Zn bridge angle, 133.6(3)�]. The MnII and CoII complexes of dicamba [(2) and (3)] have been confirmed as isomorphous and isostructural with the ZnII analogue.

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