Synthesis and characterization of hydrophilic hydroxy-pyridinones and their complexes with molybdenum(VI)

2000 ◽  
Vol 53 (8) ◽  
pp. 687 ◽  
Author(s):  
Noah A. Epstein ◽  
Jennifer L. Horton ◽  
Christopher M. Vogels ◽  
Nicholas J. Taylor ◽  
Stephen A. Westcott
Keyword(s):  
Diffraction Study ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Hydroxy Groups

We have prepared four N-substituted hydroxypyridinones containing alcohol and morpholine groups. Complexes of the type cis-MoO2L2, where L represents the hydroxypyridinonato ligands have also been synthesized. The ethanolamine derivative, cis-MoO2(hep)2 (5), has been characterized by an X-ray diffraction study whereby the pyridinone ligands are bound to molybdenum in a cis bidentate fashion via the deprotonated hydroxy groups and the ketone moieties. Crystals of (5) are triclinic, with a 9.1930(7), b 14.2718(8), c 14.6219(9) Å, α 106.816(5), β 95.902(5), γ 96.350(5)°, Z 4, space group P–1.

scholarly journals Synthesis and Characterization of New Diiron and Diruthenium μ-Aminocarbyne Complexes Containing Terminal S-, P- and C-Ligands

2007 ◽  
Vol 62 (3) ◽  
pp. 427-438 ◽  
Author(s):  
Vincenzo G. Albano ◽  
Luigi Busetto ◽  
Fabio Marchetti ◽  
Magda Monari ◽  
Stefano Zacchini ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Coordination Mode ◽  
Bond Cleavage ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dithiocarbamate Ligand ◽  
High Yields

The diiron aminocarbyne complexes [Fe2{μ-CN(Me)(R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (R = Xy1, 1a; R = Me, 1b; R = CH2Ph, 1c; Xy1 = 2,6-Me2C6H3) undergo replacement of the coordinated nitrile by halides, diethyldithiocarbamate, and dicyanomethanide to give [Fe2{μ-CN(Me) (R)}(μ-CO)(CO)(X)(Cp)2] complexes (R = Me, X = Br, 4a; R = Me, X = I, 4b; R = CH2Ph, X = Cl, 4c; R = CH2Ph, X = Br, 4d; R = CH2Ph, X = I, 4e; R = Xy1, X = SC(S)NEt2, 5a; R = Me, X = SC(S)NEt2, 5b; R = Xy1, X = CH(CN)2, 7), in good yields. The molecular structure of 5a shows an unusual η1 coordination mode of the dithiocarbamate ligand. Similarly, treatment of [M2{μ-CN(Me) (R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (M = Fe, R = Xy1, 1a; M = Fe, R = Me, 1b; M = Ru, R = Xy1, 2a; M = Ru, R = Me, 2b) with a series of phosphanes generates the cationic complexes [M2{μ- CN(Me)(R)}(μ-CO)(CO)(P)(Cp)2][SO3CF3] (M = Fe, R = Xy1, P = PPh2H, 6a; M = Fe, R = Xy1, P = PPh3, 6b; M = Fe, R = Xy1, P = PMe3, 6c; M = Fe, R = Me, P = PMe2Ph, 6d; M = Fe, R = Me, P = PPh3, 6e; M = Fe, R = Me, P = PMePh2, 6f; M = Ru, R = Xy1, P = PPh2H, 6g; M = Ru, R = Me, P = PPh2H, 6h), in high yields. The molecular structure of 6a has been elucidated by an X-ray diffraction study. The reactions of [Fe2{μ-CN(Me)(Xyl)}(μ-CO)(CO)(NCR′)(Cp)2][SO3CF3] [R′ = Me, 1a; R′ = tBu, 3] with PhLi and PPh2Li yield [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(Ph)(Cp)2] (8) and [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(PPh2)(Cp)2] (9), respectively. The molecular structure of 8 has been ascertained by X-ray diffraction. Conversely, the reaction of 1a with MeLi generates the aminoalkylidene compound [Fe2{C(Me)N(Me)(Xy1)}(μ-CO)2(CO)(Cp)2] (10).Finally, the acetone complex [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(OCMe2)(Cp)2][SO3CF3] (12) reacts with lithium acetylides to give complexes [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(C≡CR)(Cp)2] (R = p-C6H4Me, 11a; R = Ph, 11b; R = SiMe3, 11c), in high yields. Filtration through alumina of a solution of 11a in CH2Cl2 results in hydration of the acetylide group and C-Si bond cleavage, affording [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO){C(O)Me}(Cp)2] (12).

scholarly journals Gold(I) Complexes with Ferrocenylphosphino Sulfonate Ligands: Synthesis and Application in the Catalytic Addition of Carboxylic Acids to Internal Alkynes in Water

Catalysts ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 955 ◽  
Author(s):  
Javier Francos ◽  
María Esther Moreno-Narváez ◽  
Victorio Cadierno ◽  
Diego Sierra ◽  
Katherine Ariz ◽  
...  
Keyword(s):  
Diffraction Study ◽  
Carboxylic Acids ◽  
Reaction Medium ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Internal Alkynes ◽  
Unsaturated Carboxylic Acids ◽  
Catalytic Addition

The synthesis and characterization of novel gold(I) complexes containing hydrophilic ferrocenylphosphino sulfonate ligands, i.e., compounds [AuCl{(η5-C5H3PR2(SO3iPr))Fe(η5-C5H5)}] (R = Ph (2a), p-Tol (2b), Cy (2c)), are presented, including a single-crystal X-ray diffraction study on 2a. Complexes 2a–c were checked as catalysts for the intermolecular addition of carboxylic acids to nonactivated internal alkynes using water as a green reaction medium. The best results in terms of activity were obtained with 2a in combination with AgOAc, which was able to promote the selective anti addition of a variety of aromatic, aliphatic, and α,β-unsaturated carboxylic acids to both symmetrical and unsymmetrical internal alkynes at 60 °C, employing metal loadings of only 2 mol %.

Solvothermal Synthesis and Characterization of Two Iron Complexes

2011 ◽  
Vol 492 ◽  
pp. 324-327
Author(s):  
Ya Wei Hu ◽  
Yang Min Ma
Keyword(s):  
Solvothermal Synthesis ◽  
Layer Structure ◽  
Iron Complexes ◽  
Synthesis And Characterization ◽  
Molecular Architecture ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Two iron complexes, Fe3(dtdb)2(HCO2)2(DMF)2(H2O)2(1) and Fe(bpy)(Hdtdb)(H2O) (2) were solvothermally synthesized and characterized by single crystal X-ray diffraction. Fe3(dtdb)2(HCO2)2(DMF)2(H2O)2 (1) shows 2D layer structure crystallized in a triclinic with space group P-1 and cell parameters, a = 8.5591(10) nm, b = 11.2502(13) nm, c = 11.4370(14) nm, α = 90.687(2)º, β = 110.275(2)º , γ = 90.712(2)º, and Z = 1. Fe(bpy)(Hdtdb)(H2O) (2) shows surper- molecular architecture crystallized in a triclinic with space group P-1 and cell parameters, a = 8.286(12) nm, b = 11.5937(16) nm, c = 11.8477(17) nm, α = 93.932(3)º, β = 102.442(3)º, γ = 97.117(3)º, and Z = 1.

Synthesis and hydroboration of lipophilic hydroxy-pyridinones and their complexes with molybdenum(VI)

2000 ◽  
Vol 53 (8) ◽  
pp. 693 ◽  
Author(s):  
M. Karen J. Gagnon ◽  
Timothy R. St. Germain ◽  
Christopher M. Vogels ◽  
Robert A. McNamara ◽  
Nicholas J. Taylor ◽  
...  
Keyword(s):  
Metal Complexes ◽  
Diffraction Study ◽  
Vinyl Ether ◽  
Unsaturated Hydrocarbon ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Ether Derivative ◽  
Hydroxy Groups

We have prepared four potentially lipophilic N-substituted hydroxypyridinones containing unsaturated hydrocarbon groups. The propyl vinyl ether derivative (3) has been characterized by an X-ray diffraction study. Complexes of the type cis-MoO2L2, where L represents the hydroxypyridinonato ligands, have also been prepared. The pyridinone ligands are bound to molybdenum in a cis bidentate fashion via the deprotonated hydroxy groups and the ketone moieties. Initial investigations into the hydroboration of the alkene groups in the pyridinone ligands and corresponding metal complexes is presented. Crystals of (3) are monoclinic, with a 10.466(1), b 13.388(1), c 15.386(2) Å, β 102.343(8)˚, Z 8, space group P21/n.

scholarly journals Synthesis of 3-oxo-3-Phenyl-2,2,5-trimethyl-1,3-oxaphosphorinanes and their tetrafluoroborate salts

Quimica Hoy ◽  
2011 ◽  
Vol 1 (2) ◽  
pp. 8
Author(s):  
Susana López Cortina ◽  
Perla Elizondo Martínez ◽  
Nancy Pérez Rodríguez ◽  
Eugenio Hernández Fernández ◽  
Mario Fernández Zertuche
Keyword(s):  
Diffraction Study ◽  
Organophosphorus Compounds ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Relative Configuration ◽  
X Ray ◽  
Cis And Trans

The synthesis and characterization of cis- and trans- 3-oxo-3-phenyl-2,2,5-trimethyl-1,3-oxaphosphorinanes (7a and 7b) and their corresponding tetrafluoroborate salts (3a and 3b) , heterocyclic organophosphorus compounds not previously reported in the literature, was accomplished. They were fully characterized by 1H, 13C and 31PNMR. It was established the relative configuration of these compounds on the basis of an X-ray diffraction study of oxide 7a.

The Reaction of Cp*ReH6, Cp* = C5Me5, with Monoborane to Yield a Novel Rhenaborane. Synthesis and Characterization of arachno-Cp*ReH3B3H8

2002 ◽  
Vol 67 (6) ◽  
pp. 808-812 ◽  
Author(s):  
Sundargopal Ghosh ◽  
Alicia M. Beatty ◽  
Thomas P. Fehlner
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Diffraction Study ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

The rhenaborane Cp*ReH3B3H8, which is generated by the reaction of Cp*ReH6 with BH3·THF, has been characterized spectroscopically in solution and by a single-crystal X-ray diffraction study in the solid state as a hydrogen-rich arachno-metallatetraborane.

Synthese und Charakterisierung von Halogen-phosphor(III)- Derivaten des 8-Hydroxychinolins. Röntgenstrukturanalyse von 8-[Phenyl(chloro)-phosphito]-chinolin/ Synthesis and Characterization of Halogen-phosphorus(III) Derivatives of 8-Hydroxyquinoline. X -Ray Structure Analysis of 8-[Phenyl(chloro)phosphito]-quinoline

1993 ◽  
Vol 48 (1) ◽  
pp. 85-89 ◽  
Author(s):  
Lin Yang ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Study ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Compounds ◽  
Derivatives Of

The reaction of 8 -trimethylsiloxyquinoline, 2 with PCl3, PhPCl2, and PhPF2 has furnished the corresponding 8 -quinolyl halophosphite derivatives, 3-5 . The synthesis of two metal complexes, 8 and 9, of 4 with Au(I) and Pt(II) is described. The new compounds were characterized by elemental analysis and by 1H and 31P NMR spectroscopy. A single crystal X-ray diffraction study of 4 has been conducted; a short intramolecular P ··· N contact (230.9 pm) and a long P-Cl bond (218.7 pm) were observed.

Synthesis and characterization of TiN / Ti / AISI 410 coatings

2018 ◽  
Vol 2 (1) ◽  
pp. 7
Author(s):  
S Chirino ◽  
Jaime Diaz ◽  
N Monteblanco ◽  
E Valderrama
Keyword(s):  
Synthesis And Characterization ◽  
Photoemission Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Columnar Grains ◽  
Tin Thin Films ◽  
Steel Aisi ◽  
Interacting Surfaces ◽  
Stainless Steel Aisi

The synthesis and characterization of Ti and TiN thin films of different thicknesses was carried out on a martensitic stainless steel AISI 410 substrate used for tool manufacturing. The mechanical parameters between the interacting surfaces such as thickness, adhesion and hardness were measured. By means of the scanning electron microscope (SEM) the superficial morphology of the Ti/TiN interface was observed, finding that the growth was of columnar grains and by means of EDAX the existence of titanium was verified.  Using X-ray diffraction (XRD) it was possible to observe the presence of residual stresses (~ -3.1 GPa) due to the different crystalline phases in the coating. Under X-ray photoemission spectroscopy (XPS) it was possible to observe the molecular chemical composition of the coating surface, being Ti-N, Ti-N-O and Ti-O the predominant ones.

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