The synthesis, characterization, and some reactions of phosphonium thiolates and selenolates: the X-ray crystal structure of tetraphenylphosphonium 2,4,6-trimethy lbenzenethiolate

1989 ◽  
Vol 67 (4) ◽  
pp. 751-758 ◽  
Author(s):  
Joanne M. Ball ◽  
P. Michael Boorman ◽  
James F. Fait ◽  
A. Scott Hinman ◽  
Penelope J. Lundmark
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Characterization ◽  
Synthetic Methods ◽  
X Ray ◽  
H Nmr ◽  
Iminium Salts ◽  
Irreversible Oxidation ◽  
Oxidation Wave ◽  
Ionic Nature ◽  
Halocarbon Solvents

Synthetic methods for the preparation of PPh4[SAr], PPN[SAr], and PPh4 [SeAr] (Ar = aryl; PPN = bis(triphenylphos-phine)iminium) salts are described, and 1H NMR, infrared, and 77Se NMR spectroscopic characterization is given. The X-ray crystal structure of [PPh4]Smes] (mes = 2,4,6-trimefhylbenzene) was carried out: space group [Formula: see text] a = 9.946(3) Å, b = 10.100(2) Å, c = 14.874(3) Å, α = 70.19(2)°, β = 69.13(2)°, γ = 82.54(2)°, Z = 2, R = 0.100, Rw = 0.074. The structure establishes the ionic nature of this compound in the solid state, and conductance measurements in acetonitrile are consistent with 1:1 electrolyte behaviour. It is shown, however, that solutions of the thiolates are quite sensitive to hydrolysis to the thiol, and also the strong nucleophilicity of the thiolate and selenolate anions enables them to react with halocarbon solvents. The selenolate solutions are extremely sensitive to oxidation to the diselenide, which limited their study. Cyclic voltammetry on selected thiolate salts shows that impurities quickly develop even in acetonitrile solvent, but comparisons with the voltammograms of thiols and disulphides confirm the assignment of an irreversible oxidation wave at ca. −0.3 V (vs. Ag/AgNO3, 0.01 M) to the process: 2SR− → R2S2 + 2e−. The potential at which this reaction occurs is related to the degree of substitution of the phenyl ring of the SAr− ion. Keywords: phosphonium thiolates, phosphonium selenolates, tetraphenylphosphonium 2,4,6-trimefhylbenzene thiolate.

Preparation, Crystal Structure and Spectroscopic Characterization of [Ga(OH)(SO4)(terpy)(H2O)] · H2O (terpy=2,2’:6’,2-Terpyridine): The First Characterized Gallium(III) Sulfato Complex

2004 ◽  
Vol 59 (3) ◽  
pp. 291-297 ◽  
Author(s):  
Andreas Sofetis ◽  
Giannis S. Papaefstathiou ◽  
Aris Terzis ◽  
Catherine P. Raptopoulou ◽  
Theodoros F. Zafiropoulos
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Good Yield ◽  
Spectroscopic Data ◽  
Spectroscopic Characterization ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr

The reaction of Ga2(SO4)3·18H2O and excess 2,2′:6′,2″-terpyridine (terpy) in MeOH / H2O leads to [Ga(OH)(SO4)(terpy)(H2O)]·H2O (1·H2O] in good yield. The structure of the complex has been determined by single-crystal X-ray crystallography. The GaIII atom in 1·H2O is 6-coordinate and ligation is provided by one terdentate terpy molecule, one monodentate sulfate, one terminal hydroxide and one terminal H2O molecule; the coodination polyhedron about the metal is described as a distorted octahedron. There is an extensive hydrogen-bonding network in the crystal structure which generates corrugated layers parallel to bc. The new complex was characterized by IR and 1H NMR spectroscopy. The spectroscopic data are discussed in terms of the nature of bonding

Zur Chemie der 1,3,5-Triaza-2-phosphorin-4,6-dione, Teil XIII. Darstellung und Röntgenstrukturanalyse des 1,3,5-Trimethyl-2-trichlormethyl-Derivats. Reaktionen einiger 1,3,5-Trimethyl-1,3,5-triaza-2-(R)-phosphorin-4,6-dione/Chemistry of the l,3,5-Triaza-2-phosphorine-4.6-diones, Part XIII. Synthesis and X -Ray Crystal Structure Determination of the 1,3,5-Trimethyl-2- trichlorom ethyl Derivative. Reactions of Some 1,3,5-Trimethyl-1,3,5-triaza-2-(R )-phosphorine-4,6-diones

1997 ◽  
Vol 52 (12) ◽  
pp. 1510-1516 ◽  
Author(s):  
Vasily A. Pinchuk ◽  
Ion Neda ◽  
Thomas Kaukorat ◽  
Michael Farkens ◽  
Axel K. Fischer ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Acid Methyl Ester ◽  
Intramolecular Hydrogen Bonding ◽  
Spectroscopic Characterization ◽  
Crystal Structure Analysis ◽  
X Ray ◽  
H Nmr ◽  
First Case ◽  
Sterically Demanding ◽  
Intramolecular Hydrogen

Abstract Upon heating 1,3,5-trimethylbiuret (1) with trichloromethyldichlorophosphine in the presence of triethylamine, 2-trichloromethyl-1,3,5-trimethyl-1,3,5-triaza-2σ3λ3-phosphorine-4,6-dione (2) was obtained in good yield. Aside from NMR spectroscopic characterization, compound 2 was investigated by X-ray crystal structure analysis, representing the first case of the solid state characterization of a 2-trihalomethyl-1,3,5-trimethyl-1,3,5-triaza-2σ3λ3-phosphorine-4,6-dione derivative. The heterocycle presents an envelope conformation with phosphorus out of the plane of the other atoms. Reaction of the monochloromethyl derivative (3) corresponding to 2, with a sterically demanding azide led by oxidation of phosphorus to the stable σ4λ5-P derivative (4). 2-Hydro-1,3,5-trimethyl-1,3,5-triaza-2-oxo-2σ4λ5-phosphorine-4,6-dione (5) reacted with p-nitrobenzylidene benzylimine with formation of 6 by insertion of the C=N double bond of the imine into the P-H bond. Intramolecular hydrogen bonding in 6 was observed by 1H NMR and IR spectroscopy. Reaction of 2-(methylamino)-methyl-1,3,5-trimethyl-1,3,5-triaza-2-oxo-2σ4λ5-phosphorine-4,6-dione (7) with diethylamino-trimethylsilane led to the corresponding N-trimethylsilylated compound 8. Compound 9. bearing a peptoid group, was formed by reaction of 7 or 8 with 3-(chloroformyl)propionic acid methyl ester. The preferred method of synthesis of 9 is indicated.

A new supramolecular compound of chrome(III): Synthesis, spectroscopic characterization, X-ray crystal structure, DFT, and solution studies

2010 ◽  
Vol 973 (1-3) ◽  
pp. 1-8 ◽  
Author(s):  
Hossein Eshtiagh-Hosseini ◽  
Zakieh Yousefi ◽  
Masoud Mirzaei ◽  
Ya-Guang Chen ◽  
S. Ali Beyramabadi ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Characterization ◽  
Supramolecular Compound ◽  
X Ray ◽  
Solution Studies ◽  
Chrome Iii

Crystal structure of 3-chlorobenzo[b]thiophene-2-carbonyl chloride

2009 ◽  
Vol 2009 (7) ◽  
pp. 437-439 ◽  
Author(s):  
Sara Tarighi ◽  
Alireza Abbasi ◽  
Sara Zamanian ◽  
Alireza Badiei ◽  
Mahmood Ghoranneviss
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Cinnamic Acid ◽  
Thionyl Chloride ◽  
Structure Determination ◽  
X Ray ◽  
Packing Structure ◽  
H Nmr ◽  
Carbonyl Chloride ◽  
C Nmr

3-Chlorobenzo[b]thiophene-2-carbonyl chloride was synthesised from cinnamic acid and thionyl chloride. The single crystal X-ray structure determination confirmed the earlier proposed structure and the product was further characterised by 1H NMR, 13C NMR and mass spectrometry. The X-ray structure determination revealed two sets of symmetry related molecules along the b-axis that are loosely connected by relatively weak CH…π ( 3.626, 3.628 Å) interactions, giving rise to two infinite chains. The packing structure is dominated by Van der Waals forces between these chains. No significant π–π interactions are found in the crystal structure.

Darstellung, Reaktionen und spektroskopische Charakterisierung von [Os2X8]2-, X = Cl, Br, I, und Kristallstruktur von (PPN)2[Os2I8] · 2 CH2Cl2 / Preparation, Reactions and Spectroscopic Characterization of [Os2X8]2-, X = Cl, Br, I, and Crystal Structure of (PPN)2[Os2I8] · 2 CH2Cl2

1990 ◽  
Vol 45 (10) ◽  
pp. 1416-1424 ◽  
Author(s):  
W. Preetz ◽  
P. Hollmann ◽  
G. Thiele ◽  
H. Hillebrecht
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Triple Bond ◽  
Room Temperature ◽  
Spectroscopic Characterization ◽  
Spectroscopic Constants ◽  
Monoclinic System ◽  
X Ray ◽  
Fine Structures

The triply bonded octahalogenodiosmate(III) anions [Os2X8]2-, previously known with X = Cl, Br, have now been extended to include the iodide with two staggered OsI4 units. This compound was prepared by treating [Os2Cl8]2- with Nal at room temperature in acetone solution. The structure determination by X-ray diffractometry on single crystals of (PPN)2[Os2I8] · 2 CH2Cl2, reveals crystallization in the monoclinic system, space group P21/c with Z = 4. The Os-Os triple bond is with 2.212(1) Å the longest within the three octahalogenodiosmates(III). The Raman spectra show ν(OsOs) at 285, [Os2Cl8]2-; at 287, [Os2Br8]2- and for the iodo compound at 270.1 cm-1 with up to three overtones. The spectroscopic constants are calculated to be ω1 = 270.9 cm-1; X11 = -0.50 cm-1. The 10 Κ UV-VIS spectra of solid [(n-C4H9)4N]2[Os2X8] exhibit δ-π* transitions with maxima at 723, 690 and 643 nm, superimposed by vibrational fine structures with long progressions of 195, 211 and 183 cm-1 for X = Cl, Br, I, respectively. Oxidation of [Os2X8]2-, X = Cl, Br with the corresponding halogen leads to the cleavage of the Os-Os bond, and the dekahalogenodiosmates(IV), [Os2X10]2-, are formed

scholarly journals Crystal structure and molecular docking studies of new pyrazole-4-carboxamides

2019 ◽  
Vol 25 (1) ◽  
pp. 66-72 ◽  
Author(s):  
Li Qiao ◽  
Peng-Peng Cai ◽  
Zhong-Hua Shen ◽  
Hong-Ke Wu ◽  
Cheng-Xia Tan ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Molecular Docking ◽  
Botrytis Cinerea ◽  
Inhibitory Activity ◽  
Docking Studies ◽  
Active Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molecular Docking Studies ◽  
H Nmr

AbstractTwo pyrazol-4-carboxamides, 3-(difluoromethyl)-N-(mesitylcarbamoyl)-1-methyl-1H-pyrazole-4-carboxa-mide (7a) and 3-(difluoromethyl)-N-((3,5-dimethylphenyl) carbamoyl)-1-methyl-1H-pyrazole-4-carboxamide (7b) were synthesized and their structures were confirmed by the aid of 1H NMR and HRMS analyses. The structure of the pyrazole-4-carboxamide, 7a was also determined by X-ray diffraction. The preliminary activity results demonstrate that these two compounds exhibit good inhibitory activity against Botrytis cinerea. Further docking results indicated that the key active group is difluoromethyl pyrazole moiety.

Preparation and characterization of some ruthenium(II) porphyrins containing tertiary phosphine axial ligands, including the crystal structure of (octaethylporphinato)bis(triphenylphosphine)ruthenium(II)

1984 ◽  
Vol 62 (4) ◽  
pp. 755-762 ◽  
Author(s):  
Sara Ariel ◽  
David Dolphin ◽  
George Domazetis ◽  
Brian R. James ◽  
Tak W. Leung ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Phosphine Ligands ◽  
Tertiary Phosphine ◽  
X Ray ◽  
Porphyrin Complex ◽  
H Nmr ◽  
Axial Ligands ◽  
Nmr Data ◽  
Phosphine Complex

The ruthenium(II) porphyrin complex Ru(OEP)(PPh3)2 (OEP = the dianion of octaethylporphyrin) has been prepared from Ru(OEP)(CO)EtOH, and the X-ray crystal structure determined; as expected, the six-coordinate ruthenium is situated in the porphyrin plane and has two axial phosphine ligands. Synthesized also from the carbonyl(ethanol) precursors were the corresponding tris(p-methoxyphenyl)phosphine complex, and the Ru(TPP)L2 (TPP = the dianion of tetraphenylporphyrin, L = PPh3, P(p-CH3OC6H4)3, P″Bu3) and Ru(TPP)(CO)PPh3 complexes. Optical and 1H nmr data are presented for the complexes in solution. In some cases dissociation of a phosphine ligand to generate five-coordinate species occurs and this has been studied quantitatively in toluene at 20 °C for the Ru(OEP)L2 and Ru(TPP)L2 systems.

Structural and IR-spectroscopic characterization of magnesium acesulfamate

2016 ◽  
Vol 71 (1) ◽  
pp. 51-55 ◽  
Author(s):  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Elemental Analysis ◽  
Spectroscopic Characterization ◽  
Magnesium Carbonate ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Ir Spectroscopic

AbstractMagnesium acesulfamate, Mg(C4H4NO4S)2·6H2O, was prepared by the reaction of acesulfamic acid and magnesium carbonate in aqueous solution, and characterized by elemental analysis. Its crystal structure was determined by single crystal X-ray diffraction methods. The substance crystallizes in the triclinic space group P1̅ with one molecule per unit cell. The FTIR spectrum of the compound was also recorded and is briefly discussed. Some comparisons with other simple acesulfamate and saccharinate salts are also made.

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