Complexes of Di-2-pyridyl ketone. II. Some chelated nickel(II) products of metal-promoted reactions at the ketones

1970 ◽  
Vol 23 (10) ◽  
pp. 1997 ◽  
Author(s):  
MC Feller ◽  
R Robson

From reactions in aqueous solution between nickel(11) nitrate, di-2-pyridyl ketone (DPK), and the reagents MeNH2, NH3, pyrazole ( C3H4N2) , HS03-,PhNHNH2, and 82-, solid complexes with the following stoicheiometries were isolated: Ni(DPK)z(MeNH2)2(N03)z(H2O)x (x: = 1, 0), Ni(DPK)z(NH~)(H2O)(NO3)3, K~(DPK)z(C3H4NZ)2(NO3)Z(H2O)y(y = 3, O), Ni(DPK)Z(HSO4)Z(HZO), Ni(DPK)2- (PhNHNH2)2(N03)2, and Ni(DPK)2(H2O)2S. Magnetic and spectral data indicate pseudo-octahedral ligand fields in all cases. Except in the cases Ni(DPK)2(H20)2S and Ni(DPK)2(PhNHNH2)2(NO3)2, for which the evidence is ambiguous, elementary compositions and i.r. spectra indicate that the added nucleophile, HX, has condensed with at least one of the two DPK units per nickel ion, yielding tridentate products, (C5H4N)2(OH)X. I n the complexes of stoicheiometry Ni(DPK)2(C3H4N2)2(N03)2 and N~(DPK)z(M~NH~)z(NO~)Z both DPK units per nickel ion have condensed with the nucleophile yielding products bound to the cation as tridentate N3 ligands. U.V. spectral observations in aqueous solution indicate that with the reagents MeNH2, NH3, C ~ H ~ N Z , and HS03- attack upon DPK occurs slowly, if a t all, in the absence of nickel(11) a t room temperature, but in the presence of nickel(11) much more rapid condensation occurs. These reactions constitute new types of metal-ion promoted condensation. With cyanide ion as the nucleophile, attack occurs not a t the ketone but a t nickel yielding [Si(DPK)2]2+[Ni(CN)4]z- in w-hich the cation is octahedral, the anion square-planar, and some cyanide units are bridging.

2012 ◽  
Vol 12 (2) ◽  
pp. 146-151 ◽  
Author(s):  
Elfi Susanti VH ◽  
Sabirin Matsjeh ◽  
Tutik Dwi Wahyuningsih ◽  
Mustofa Mustofa ◽  
Tri Redjeki

Synthesis of flavones and their derivatives has attracted considerable attention due to their significant pharmaceutical effects. 7-hydroxy-3',4'-dimethoxyflavone has been synthesized and its antioxidant activity has been investigated. Flavone was synthesized by oxidative cyclization of chalcone. 2',4'-dihydroxy-3,4-dimethoxychalcone was prepared by Claisen-Schmidt condensation of 2,4-dihydroxyacetophenones with 3,4-dimethoxybenzaldehydes in the presence of aqueous solution of sodium hydroxide and ethanol at room temperature. Oxidative cyclization of 2',4'-dihydroxy-3,4-dimethoxychalcone was done by using I2 catalyst in DMSO to form 7-hydroxy-3',4'-dimethoxyflavone. The synthesized compounds were characterized by means of their UV-Vis, IR, 1H-NMR and 13C-NMR spectral data. The compound was tested for their antioxidant activities by DPPH method.


1969 ◽  
Vol 22 (1) ◽  
pp. 59 ◽  
Author(s):  
AR Nicholoson ◽  
GJ Sutton

Spin-free six-coordinate complexes of nickel(II) and the heterocyclic ligands 2-aminomethylpyridine, 2-methylaminomethylpyridine, 2-(2- aminoethyl)pyridine, and 2-aminomethyl-6-methylpyridine have been prepared and studied. Various hydrated and anhydrous nickel(II) complexes with the anions sulphate, nitrate, halide, and perchlorate were obtained with nickel ion to ligand stoicheiometric ratios of 1 : 1, 1 : 2, and 1 : 3, and in a number of instances water molecule and anion attachments to the coordination sphere are reported; the sulphate complexes are considered to be of the bridged type. Also, certain mixed-ligand solid complexes and mixed-ligand cationic species in aqueous solution were prepared. Physical measurements used to elucidate structures included molecular conductances in suitable solvents, solubility observations, infrared spectrophotometry, pyrolysis methods, and measurements of magnetic susceptibility. Complex cations in aqueous solution were characterized by visible and near-infrared spectrophotometry.


2017 ◽  
Vol 76 (7) ◽  
pp. 1895-1906 ◽  
Author(s):  
Sowmya Vilvanathan ◽  
S. Shanthakumar

The biosorption capability of Chrysanthemum indicum to remove nickel ions from aqueous solution in a fixed-bed column was examined in this study. Native C. indicum flower waste was improved for its biosorptive potential by pyrolysis to obtain its biochar form and, thereby, both raw (CIF-R) and biochar (CIF-BC) forms of the flower were used for Ni(II) removal. Fixed bed column studies were conducted to examine the influence of bed height (1.0–3.0 cm), flow rate (1.0–5.0 mL min−1) and initial metal ion concentration (25–75 mg L−1). The breakthrough curves (Cout/Cin vs time) were modelled using different dynamic adsorption models, viz. Adams-Bohart, Thomas and Yoon-Nelson model. Interpretation of the data revealed a favorable correlation with the Thomas model with higher R2 values and closer model-predicted and experimental biosorption capacity values. The equilibrium uptake capacity of CIF-R and CIF-BC for Ni(II) were found to be 14.02 and 29.44 mg g−1, respectively. Further, the column was regenerated using HCl as eluent, to desorb the adsorbed Ni(II) ions. The experimental results implied and affirmed the suitability of the biosorbents for nickel ion biosorption with its nature being favorable, efficient, and environmentally friendly.


2006 ◽  
Vol 2006 ◽  
pp. 1-9 ◽  
Author(s):  
Irena Kostova ◽  
Georgi Momekov ◽  
Tzvetomira Tzanova ◽  
Margarita Karaivanova

Complexes of lanthanum(III) with bis-coumarins: 3,3′-benzylidene-bis(4-hydroxy-2H-1-benzopyran-2-one) (H2L1) and bis(4-hydroxy-2-oxo-2H-chromen-3-yl)-(1H-pyrazol-3-yl)-methane (H2L2) were synthesized by reaction of lanthanum(III) salt and the ligands, in amounts equal to metal: ligand molar ratio of1:2. The complexes were prepared by adding an aqueous solution of lanthanum(III) salt to an aqueous solution of the ligand subsequently raising the pH of the mixture gradually to circa 5.0 by adding dilute solution of sodium hydroxide. The lanthanum(III) complexes with bis-coumarins were characterized by different physicochemical methods—elemental analysis, IR-,1H-, and13C-NMR-spectroscopies, and mass spectral data. The spectral data of lanthanum(III) complexes were interpreted on the basis of comparison with the spectra of the free ligands. This analysis showed that in theLa(III)complexes, the ligands coordinated to the metal ion through both deprotonated hydroxyl groups. On the basis of theν(C=O)red shift observed, participation of the carbonyl groups in the coordination with the metal ion was also suggested. In the present study, we performed a cytotoxic-effects screening of the lanthanum complexes withH2L1 andH2L2 in a panel of human tumor cell lines, using the standard MTT-dye reduction assay for cell viability. The panel consisted of the acute myeloid leukemia-derived HL-60 and the chronic myeloid leukemia-derived BV-173. Following a 24- hour treatment of BV-173 cells with lanthanum complex ofH2L1 at 100 or 200μM led to a DNA-laddering. The findings suggest that the observed cytotoxicity of the lanthanum complex ofH2L1 on BV-173 is at least partly mediated through induction of programmed cell death.


1972 ◽  
Vol 27 (3) ◽  
pp. 304-307 ◽  
Author(s):  
R. K. Mehta ◽  
V. C. Singhi

The Schiff base, N-hydroxyethylnaphthalideneimine forms solid complexes with Mn (II) , Co (II), Ni (II), Cu (II), Zn (II), Cd (II), Pd (II) and UO2 (II). The structures of these compounds have been discussed on the basis of their elemental analysis, magnetic moment values and electronic spectral data. These studies have conclusively proved that UO2 (II) and Mn (II) complexes are octahedral in shape whereas the Cu (II) complex molecule displays a square planar or tetragonally distorted octahedral configuration. Co (II) , Ni (II) , Zn (II) and Cd (II) complexes are tetrahedral in structures while the Pd (II) compound is square planar.


1969 ◽  
Vol 47 (14) ◽  
pp. 2699-2706 ◽  
Author(s):  
G. J. Erskine

Palladium(II) complexes of cis- and trans-1,2-bis(dimethylarsino)ethylene, 1 and 2, respectively, in the metal: ligand ratios 1:1 and 1:2 are described. Their structures are discussed in terms of nuclear magnetic resonance, infrared, conductivity, and analytical data, and by comparison with the corresponding platinum(II) complexes (1). The cis-isomer, cis-ED, is a strong chelating ligand and forms the complexes Pd(cis-ED)X2, 9 (X = Cl−, Br−), and Pd(cis-ED)2X2•3H2O, 8 (X = Cl−, Br−, ClO4−, PF6−). The trans-isomer, trans-ED is a bridging ligand and forms the dimeric complexes, [Pd(trans-ED)X2]2, 10 (X = Cl−, Br−), and Pd2(trans-ED)4X4•3H2O, 7 (X = Cl−, Br−, ClO4−, PF6−). All these complexes contain 4-coordinate, square planar palladium(II). The anhydrous form of 7 (X = Cl−) shows evidence for a Pd—Cl bond, suggesting 5-coordination in the solid state. Room temperature irradiation (with ultraviolet light) of 7 (X = Cl−), in non-aqueous solvents, causes isomerization of the ligand and the formation of complex 8 (X = Cl−). No change occurs under these conditions in aqueous solutions. Contrary to the original suggestion for the corresponding platinum(II) derivative, 10 (M = Pt(II), ref. 1) far infrared evidence supports a cis-configuration about the metal ion rather than the trans-configuration, 6.


2013 ◽  
Vol 78 (7) ◽  
pp. 947-957 ◽  
Author(s):  
Ionela Alan ◽  
Angela Kriza ◽  
Olguta Dracea ◽  
Nicolae Stanica

The new N,N?-bis-(3-methoxy-saliciliden)-3,3?-dimetilbenzidine (H2L) Schiff base and complexes with Co(II), Ni(II) and Cu(II) of type [M(HL)Cl(H2O)] (M=Co(II), Cu(II)) [M2L(H2O)4]X2 (M=Co(II), X=ClO4 and M=Cu(II), X=NO3) and [M2L(CH3COO)2] (M=Co(II), Ni(II), Cu(II)) were synthesised. The ligand and complexes were characterized by elemental analysis, conductibility measurements, magnetic moments at room temperature, IR, NMR, UV-VIS-NIR, EPR spectra and thermogravimetric analysis. A molar ratio of 1:1 or 1:2 between ligand and metal was determined from the elemental analysis. Except for perchlorate complex that behave as electrolyte, the rest of complexes are non-electrolytes. The spectral data suggest a tetrahedral, pseudo-tetrahedral or square-planar stereochemistry respectively, data confirmed by magnetic behaviour of complexes. The antimicrobial tests indicate a fungicide effect both for ligand and complexes.


2011 ◽  
Vol 8 (2) ◽  
pp. 541-546 ◽  
Author(s):  
S. Sridhar ◽  
S. C. Dinda ◽  
Y. Rajendra Prasad

A series of new chalcones(3a-g)were prepared by Claisen-Schmidt condensation of 3-acetyl-2,5-dimethylfuran with various substituted aromatic aldehydes in presence of aqueous solution of potassium hydroxide and ethanol at room temperature. The synthesized chalcones were characterized by means of their IR,1H NMRspectral data and elemental analyses. When these chalcones were evaluated for antimicrobial and anti-inflammatory activities, some of them were found to possess significant activity, when compared to standard drugs.


2008 ◽  
Vol 2008 ◽  
pp. 1-8 ◽  
Author(s):  
Sahar I. Mostafa ◽  
Constantina Papatriantafyllopoulou ◽  
Spyros P. Perlepes ◽  
Nick Hadjiliadis

The new complexes[M2O5L2(H2O)2]⋅H2O (M=Mo,1;M=W,2),[RuL2(H2O)2]⋅H2O (3),[ML3]⋅xH2O (M=Rh,x=2,4;M=Ir,x=1,5),[RhL2(PPh3)2](ClO4)⋅2H2O (6),[PdL2]⋅2H2O (7),[PdL(phen)]Cl⋅H2O (8),[Re⁡OL2(PPh3)]Cl (9)and[UO2L2] (10)are reported, where LH is 4,6-diamino-1-hydro-5-hydroxy-pyrimidine-2-thione. The complexes were characterized by elemental analyses, physical techniques (molar conductivity, room-temperature magnetic susceptibility), and spectroscopic (IR, Raman, UV/VIS/ligand field, NMR, mass) methods. The ligandL−is in its thione form and behaves as a bidentate chelate with the deprotonated (hydroxyl) oxygen and the nitrogen of one amino group as donor atoms. Oxobridged dinuclear(1, 2)and various mononuclear(3–10)structures are assigned for the complexes in the solid state. The metal ion coordination geometries are octahedral(1–6, 9, 10)or square planar(7, 8). The free ligand LH and complexes1,4,7, and8were assayed in vitro for antimicrobial activity against two bacterial and two fungal cultures.


1987 ◽  
Vol 19 (3-4) ◽  
pp. 439-448 ◽  
Author(s):  
Jeppe S. Nielsen ◽  
Steve E. Hrudey ◽  
Frederick F. Cantwell

Batch isotherm studies using spiked sewage samples containing a range of total soluble nickel concentrations typical of municipal sewage strongly suggested that it is the free (i.e. uncomplexed) nickel ion that is sorbed by activated sludge. Equations relating nickel uptake by activated sludge to free nickel ion concentrations and the extent of complexation in untreated sewage were developed and applied. Predicted and measured nickel removals generally agreed to within ± 30%.


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