The direct electrochemical synthesis of thiolato complexes of cobalt and nickel, and the crystal structure of bis(phenylthiolato)bis(1,10-phenanthroline)cobalt(III) perchlorate

1988 ◽  
Vol 66 (9) ◽  
pp. 2151-2156 ◽  
Author(s):  
Raj K. Chadha ◽  
Rajesh Kumar ◽  
Jaime Romero Lopez-Grado ◽  
Dennis G. Tuck
Keyword(s):  
Crystal Structure ◽  
Electrochemical Oxidation ◽  
Electrochemical Synthesis ◽  
Crystallographic Analysis ◽  
High Yield ◽  
X Ray ◽  
Metal Anode ◽  
Aerial Oxidation ◽  
Perchlorate Salt ◽  
Cobalt And Nickel

Cobalt(II) and nickel(II) thiolates, M(SR)2, can be prepared in high yield by the electrochemical oxidation of a metal anode in an acetonitrile or acetone solution of RSH (R = C6H5, o-CH3C6H4, 2-C10H7, 2,3,4,5-C6F4H; not all combinations). When 2,2-bipyridine or 1,10-phenanthroline (=L) is added to the electrolyte phase, the products are the adducts M(SR)2L2. In the case of Co(SC6H5)2(phen)2, aerial oxidation leads to the formation of the cobalt(III) cation [Co(SC6H5)2(phen)2]+, isolated as the perchlorate salt. X-ray crystallographic analysis showed that this cation has a cis-CoS2(N2)2 kernel.

The direct electrochemical synthesis of some metal derivatives of lapachol

1997 ◽  
Vol 75 (5) ◽  
pp. 499-506 ◽  
Author(s):  
E.H. De Oliveira ◽  
G.E.A. Medeiros ◽  
C. Peppe ◽  
Martyn A. Brown ◽  
Dennis G. Tuck
Keyword(s):  
Electrochemical Oxidation ◽  
Copper Atom ◽  
Electrochemical Synthesis ◽  
Acetonitrile Solution ◽  
Triclinic Space Group ◽  
X Ray ◽  
Metal Anode ◽  
X Ray Crystallography ◽  
Metal Derivatives ◽  
Derivatives Of

The electrochemical oxidation of a sacrificial metal anode (M = Zn, Cd, Cu) in an acetonitrile solution of 2-hydroxy-3-(3-methyl-2-butenyl)-1,4-naphthoquinone, lapachol, C15H14O3 (=HL) gives ML2. The results are in keeping with earlier work on direct electrochemical synthesis in related systems. Adducts with 2,2′-bipyridine (bpy) and N,N,N′,N′-tetramethylethanediamine (tmen) have also been prepared. The structure of the 2,2′-bipyridine adduct of Cu(lapacholate)2 has been established by X-ray crystallography. The parameters are triclinic, space group [Formula: see text], a = 12.748(59) Å, b = 13.859(49) Å, c = 11.770(59) Å, α = 108.30(4)°, β = 108.08(3)°, γ = 68.94(3)°, Z = 2, R = 0.059 for 2256 unique reflections. The copper atom is in a distorted CuN2O2O2′ environment. The mechanism of the formation of this Cu(lapacholate)2 is discussed. Keywords: electrochemical synthesis, lapachol, X-ray crystallography, copper(II) complex.

The direct electrochemical synthesis of thiolato complexes of copper, silver, and gold; the molecular structure of [Cu(SC6H4CH3-o)(1,10-phenanthroline)]2•CH3CN

1987 ◽  
Vol 65 (6) ◽  
pp. 1336-1342 ◽  
Author(s):  
Raj K. Chadha ◽  
Rajesh Kumar ◽  
Dennis G. Tuck
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Aqueous Solutions ◽  
Electrochemical Oxidation ◽  
Copper Atom ◽  
Electrochemical Synthesis ◽  
High Yield ◽  
Space Group ◽  
Anodic Copper

The electrochemical oxidation of anodic copper or silver (= M) into non-aqueous solutions of RSH (R = alkyl, axyl) gives MISR as insoluble materials in high yield. In the presence of 1,10-phenanthroline (= L), the products are MISR•phen for M = Cu, but not Ag. Gold resists oxidation under such conditions, and AuISR (R = n-C4H9, C6H5) was obtained in only poor yield. The crystal structure of the solvated dimeric adduct [Cu(SC6H4CH3-o)•phen]2•CH3CN is triclinic, with a = 10.682(3) Å, b = 11.729(4) Å, c = 15.608(5) Å, α = 76.87(2)°, β = 76.35(2)°, γ = 68.07(2)°, V = 1742(1) Å3, Z = 2 and space group [Formula: see text]. The structure is based on a folded Cu2S2 ring with an unusually short Cu—Cu distance of 2.613(3) Å Each copper atom has CuS2N2 pseudo-tetrahedral stereochemistry, with Cu—S = 2.337 Å(av) and Cu—N = 2.10 Å(av).

Electrochemical Synthesis of N-Oxopyridine-2-thionate Complexes of Cd(II): The Crystal Structure of Bis(2,2′-bipyridine)(N-oxopyridine-2-thionate) Cadmium(II) Perchlorate 1/4 (Bipyridine)

1993 ◽  
Vol 48 (4) ◽  
pp. 431-437 ◽  
Author(s):  
J. Sanmartin ◽  
M. R. Bermejo ◽  
J. Romero ◽  
J. A. García-Váquez ◽  
A. Sousa ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Electrochemical Oxidation ◽  
Electrochemical Synthesis ◽  
Acetonitrile Solution ◽  
Distorted Octahedral ◽  
Perchlorate Salt

The electrochemical oxidation of Cd in acetonitrile solution of 1-hydroxy-2-pyridinethione (HPT) and 2,2′-bipyridine (bipy) affords [Cd(PT)2(bipy)] · H2O and [Cd(PT)(bipy)2]ClO4· 1/4(bipy). The crystal structure of the perchlorate salt shows the molecule to have a distorted octahedral CdN4OS skeleton.

The Meisenheimer rearrangement in heterocyclic synthesis. II. Synthesis and X-ray crystal structure of a tetrahydro-1H-2,3-benzoxazocine and preparation of a hexahydro-2,3-benzoxazonine

1980 ◽  
Vol 33 (6) ◽  
pp. 1323 ◽  
Author(s):  
JB Bremner ◽  
EJ Browne ◽  
PE Davies ◽  
CLWAH Raston
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Acetic Acid ◽  
Crystal And Molecular Structure ◽  
Phosphorus Oxychloride ◽  
Crystallographic Analysis ◽  
Heterocyclic Synthesis ◽  
Reaction Conditions ◽  
X Ray ◽  
Heterocyclic Derivatives

The heterocyclic derivatives, 8,9-dimethoxy-3-methyl-1-phenyl-3,4,5,6- tetrahydro-1H-2,3-benzoxazocine(3a) and 9,10-dimethoxy-3-methyl-1- phenyl-1,3,4,5,6,7-hexahydro-2,3-benzoxazonine (3b),examples of two new ring systems, have been prepared by Meisenheimer rearrangement of the corresponding 2-benzazepine and 2-benzazocine N-oxide derivatives (2a) and (2b). The Bischler-Napieralski-type cyclization reaction was used in the preparation of the tertiary amine precursors of these N-oxides reaction conditions for the cyclization were critical and phosphorus oxychloride in refluxing butanenitrile was found to give the best yields of the seven- or eight-membered cyclic imine intermediates. Reductive cleavage of the benzoxazocine derivative (3a) with zinc in acetic acid followed by N-methylation gave the expected product, [2-{3- (dimethylamino)propyl}-4,5-di-methoxyphenyl]phenylmethanol (12). The crystal and molecular structure of (3a) has been determined by X-ray crystallographic analysis.

A Novel Alkali-Metal Hydrido-tris(pyrazolyl)borate (Tp*) Complex. Isolation and Crystal Structure of [(Me2CO)3(NaTp*)2]

2014 ◽  
Vol 69 (7) ◽  
pp. 793-798
Author(s):  
Laurent Plasseraud ◽  
Hélène Cattey
Keyword(s):  
Crystal Structure ◽  
Alkali Metal ◽  
Sodium Hydroxide ◽  
Title Compound ◽  
Room Temperature ◽  
Crystallographic Analysis ◽  
Monoclinic Space Group ◽  
Large Excess ◽  
X Ray ◽  
Acetone Water

The title compound was isolated from the treatment of Tp*Sn(Cl)2Bu (1) with a large excess of sodium hydroxide in a mixture of acetone-water at room temperature. [(Me2CO)3(NaTp*)2] (2) crystallizes at 4 °C as prismatic colorless crystals, in the monoclinic space group P21/c with Z = 4, a = 12.2837(6), b = 24.3197(12), c = 16.9547(8) Å, β = 110.017(1)°, and V = 4759.0(4) Å3. The X-ray crystallographic analysis revealed a dinuclear unit in which two Tp*Na moieties are held together by three bridging acetone molecules acting as oxygen-based donors.

The Crystal Structure of Dimethyl (1aα,2aα,5β,6aβ-Hexahydroazirino[2,1-b]benzoxazole-1a, 5(1H)-dicarboxylate

1991 ◽  
Vol 44 (8) ◽  
pp. 1145 ◽  
Author(s):  
MF Mackay ◽  
M Campbell ◽  
MJ Mcleish
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Crystallographic Analysis ◽  
Aminobenzoic Acid ◽  
X Ray ◽  
Relative Stereochemistry

The title compound formed the major component in a rearrangement of an analogue of 4-amino-4-deoxychorismic acid (1), an intermediate in the chorismate-p-aminobenzoic acid biotransformation. X-Ray crystallographic analysis has defined the relative stereochemistry at the four chiral centres in the tricyclic molecule.

Pentamethylcyclopentadienyl-Vanadium Complexes Containing Halogeno- and Oxo-Ligands

1987 ◽  
Vol 42 (12) ◽  
pp. 1520-1526 ◽  
Author(s):  
Max Herberhold ◽  
Walter Kremnitz ◽  
Markus Kuhnlein ◽  
Manfred L. Ziegler ◽  
Karl Brunn
Keyword(s):  
Crystal Structure ◽  
Mass Spectra ◽  
High Yield ◽  
Vanadium Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Oxygen Bond ◽  
Single Bonds ◽  
Oxo Ligands

AbstractA simple and high-yield preparation of the pentamethylcyclopentadienyl vanadium(IV) trihalides Cp*VX3 (X = CL, Br, I) from Cp*V(CO)4 as well as their conversion into the oxo-vanadium(V) compounds Cp*VOX2 (X = CL, Br) and [Cp*VOX]2(μ-O) (X = CL, Br, I) are described. The equilibrium between the two fluoride species Cp*VOF2 and [Cp*VOF]2(μ-O) has also been investigated. The complexes are characterized by their NMR (51V, l3C, 1H), IR, and mass spectra. The crystal structure of the binuclear chloro-oxo complex [Cp*VOCl]2(μ-O) has been determined by X-ray diffraction. The molecules contain two [Cp*VOCl] units combined via a bent oxo bridge (V-O-V angle of 142.2(2)°). The vanadium-oxygen bond lengths are 157.6(8) and 179.4(1) pm for the terminal and the bridging oxo ligands, respectively, corresponding to double and single bonds.

scholarly journals Wastewater Minimization in Indirect Electrochemical Synthesis of Phenylacetaldehyde

2002 ◽  
Vol 2 ◽  
pp. 48-52 ◽  
Author(s):  
Zhirong Sun ◽  
Xiang Hu ◽  
Ding Zhou
Keyword(s):  
Sulfuric Acid ◽  
Current Efficiency ◽  
Electrochemical Oxidation ◽  
Acid Concentration ◽  
Electrochemical Synthesis ◽  
Chemical Process ◽  
Sulfuric Acid Concentration ◽  
High Yield ◽  
High Current ◽  
High Current Efficiency

Wastewater minimization in phenylacetaldehyde production by using indirect electrochemical oxidation of phenylethane instead of the seriously polluting traditional chemical process is described in this paper. Results show that high current efficiency of Mn(III) and high yield of phenylacetaldehyde can be obtained at the same sulfuric acid concentration (60%). The electrolytic mediator can be recycled and there will be no waste discharged.

The Electrochemical Synthesis of Neutral Zinc(II) Complexes of Schiff Base Ligands: The Crystal Structure of Bis[N-(4-methylphenyl)salicylaldiminato]zinc(II)

1988 ◽  
Vol 43 (5) ◽  
pp. 611-615 ◽  
Author(s):  
T. Sogo ◽  
J. Romero ◽  
A. Sousa ◽  
A. de Blas ◽  
M. L. Durán ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Schiff Base ◽  
Schiff Bases ◽  
Electrochemical Synthesis ◽  
Chemical Properties ◽  
Zinc Atom ◽  
Schiff Base Ligands ◽  
Space Group ◽  
X Ray ◽  
Physico Chemical

Abstract The electrochemical synthesis and physico-chemical properties of neutral zinc(II) complexes of bidentate Schiff bases derived from salicylaldehydes are presented together with the X-ray structure of bis[N-(4-methylphenyl)salicylaldiminato]zinc(II). The crystal is monoclinic, a = 21.877(3), b = 8.801(2), c = 12.027(5) Å, β = 96.55(3)°, space group C2/c. The complex is a monomer, and the zinc atom is tetrahedrally coordinated.

1-Allylgermatrane. Synthesis, Structure and Reaction with Diazomethane

1997 ◽  
Vol 52 (1) ◽  
pp. 30-34 ◽  
Author(s):  
Galina S. Zaitseva ◽  
Sergey S. Karlov ◽  
Elena S. Alekseyeva ◽  
Leonid A. Aslanov ◽  
Evgeni V. Avtomonov ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Structure Study ◽  
Quantitative Yield ◽  
High Yield ◽  
Crystalline Solid ◽  
Conformational Disorder ◽  
X Ray ◽  
C Nmr

Reaction of allyltribromogermane (2), readily available from dibromo(1,4-dioxane)germanium(II) (1) and allylbromide, with tris(2-tributylstannoxyethyl)-amine (4) gives 1-allylgermatrane (3) in almost quantitative yield. 3 crystallizes from n-pentane as a colourless crystalline solid which was characterized by 1H and 13C NMR spectroscopy and by an X-ray crystal structure study. The “atrane” skeleton shows a strong conformational disorder; the Ge-N distance of 2.208(3) Å suggests the presence of a coordinative Ge-N bond. Treatment of 1-allylgermatrane (3) with CH2N2 in the presence of catalytic amounts of Pd(OAc)2 affords 1-cyclopropylmethylgermatrane (5) in high yield

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