Crystallographic Study on Metal(II) Complexes with N-(2-Nitrophenylsulfonyl)glycine

1999 ◽  
Vol 52 (8) ◽  
pp. 741 ◽  
Author(s):  
Daniela Iacopino ◽  
Ledi Menabue ◽  
Monica Saladini

The interaction of MII ions (MII =Mn II, CoII, NiII, CuII, ZnII, CdII, PbII) with N-(2-nitrophenylsulfonyl)- glycine (NO2psglyH2) leads to the formation at acidic pH of the complex carboxylate-type M(NO2psgly- O)2.x H2O species. At higher pH the deprotonation reaction of the sulfonamide nitrogen takes place, leading to the formation of the M(NO2psgly-N,O).x H2O species where the ligand acts as a chelating agent toward the metal ion through the carboxylic oxygen and the deprotonated sulfonamide nitrogen. In ternary systems the addition of 2,2′-bipyridine (bpy) allows the deprotonation of the sulfonamide nitrogen also in presence of metal ions such as ZnII, CoII and NiII, which were inactive in the binary system, and the solid compounds isolated are in the M/bpy/L molar ratio 1 : 1 : 1 (MII = CuII , ZnII ) or 1 : 2 : 1(MII = CoII , NiII, CdII). Here we describe the crystal and molecular structures of NO2psglyH2 (1), [Pb(NO2psgly-N,O)]n (2), [Cd(bpy)2(NO2psgly-N,O)].H2O (3) and [Cu(bpy)(NO2psgly-N,O)(H2O)] (4).

2003 ◽  
Vol 68 (9) ◽  
pp. 1647-1662 ◽  
Author(s):  
Valeria Amendola ◽  
Massimo Boiocchi ◽  
Yuri Diaz Fernandez ◽  
Carlo Mangano ◽  
Piersandro Pallavicini

The bis-bidentate ligand R,S-1,2-diphenyl-N,N'-bis(2-quinolinemethylidene)ethane-1,2-diamine (ligand 4), containing two (iminomethyl)quinoline moieties separated by a cis-1,2-diphenylethylene spacer, forms stable complexes with both CuI and CuII. With CuII, the monomeric 1:1 complex [CuII(4)]2+ is obtained both in CH3CN and CH2Cl2. With CuI and overall 1:1 metal/ligand molar ratio, an equilibrium mixture is obtained in CH3CN, consisting of [CuI(4)2]+, [CuI2(4)2]2+ and [CuI2(4)(CH3CN)4]2+. The preponderant species is the two-metal one-ligand "open" complex [CuI2(4)(CH3CN)4]2+, in which each Cu+ cation is coordinated in a tetrahedral fashion by one (iminomethyl)quinoline unit and by two CH3CN molecules. Precipitation from the equilibrium mixture yields only crystals of [CuI2(4)(CH3CN)4](ClO4)2·2CH3CN, whose crystal and molecular structures have been determined. On the other hand, in the poorly coordinating CH2Cl2 solvent, only the dimeric helical [CuI2(4)2]2+ complex is obtained, when the overall metal/ligand 1:1 molar ratio is chosen. Addition of large quantities of acetonitrile to solutions of [CuI2(4)2]2+ in dichlorometane results in the formation of [CuI2(4)(CH3CN)4]2+, i.e. in the solvent-driven disassembling of the CuI helicate. While electrochemistry in CH3CN is poorly defined due to the presence of more than one CuI species, cyclic voltammetry experiments carried out in CH2Cl2 revealed a well defined behavior, with irreversible oxidation of [CuI2(4)2]2+ and irreversible reduction of [CuII(4)]2+ taking place at separate potentials (∆E ≈ 700 mV). Irreversibility and separation of the redox events are due to the self-assembling and disassembling processes following the reduction and oxidation, respectively.


1982 ◽  
Vol 35 (11) ◽  
pp. 2193 ◽  
Author(s):  
GL Roberts ◽  
BW Skelton ◽  
AH White ◽  
SB Wild

The potentially tridentate chelating agent bis(6-methylquinolin-8-yl)phenylarsine (AsN2) and quadridentate tris(6-methylquinolin-8-yl)arsine (AsN2) have been prepared from 6-methyl-8-lithio-quinoline and dichlorophenylarsine or arsenic trichloride, respectively. Both ligands behave as bidentates in complexes of the type [PdX2(AsN2)] and [PdX2(AsN2)] (where X = Cl or I) and as tridentates in [Mo(CO)3(AsN2)] and [Mo(CO)3(AsN2)]. The crystal and molecular structures of [PdCl2(AsN2)],CH2Cl2 and [PdI2(AsN2)] have been determined by single-crystal X-ray analysis. The dichloro complex crystallizes in space group P1 (Ci1; No.2) with a 9.963(3), b 8.555(3), c 16.102(7) �; α 86.64(3), β 82.13(3), γ 85.84(3)�; U 1354.3(9) �3 and Z = 2. The structure was solved by heavy-atom methods and refined by least squares to R 0.044 for 2530 'observed' reflections with 1>3σ(I). The coordination geometry of the palladium(II) atom is pseudo-square-planar in which the potentially tridentate AsN2 is behaving as a bidentate only. There is no evidence of interaction of the remaining 6-methylquinolin-8-yl group with the metal centre, although a weak interaction between the solvent of crystallization and the metal may be present. The diiodo complex similarly crystallizes in the centrosymmetric triclinic space group P1 (Cil ; No.2) with a 13.590(5), b 10.035(2), c 9.435(2) �; α 102.68(2), β 90.10(2), γ 92.99(2)�; U 1253.5(6) �3 and Z = 2. Least- squares refinement led to a convergence with R 0.038 for 3461 'observed' reflections. The structure of this complex was similar to that of the dichloro analogue.


F1000Research ◽  
2021 ◽  
Vol 10 ◽  
pp. 1140
Author(s):  
IKHOU Djamila ◽  
M'hamed Kaid ◽  
ZIANI Hanane ◽  
Didier Villemein

This study has investigated the solvent extraction of cadmium and lead ions from an aqueous solution in nitrate medium using aminooctyldiphosphonic acid (AODPA) as extractant in chloroform. In order to establish spectrophotometrically the concentration of metal ion in the aqueous phase before and after extraction, the Arsenazo III method was used. The effects of several extraction parameters on the extraction of these metals ions  including volume ratio between the aqueous and organic phases (1–5), extraction kinetic time (0–30 min), molar ratio Q (1–5), addition of HNO3 (pH =2–6), addition of KNO3 (0.01 – 1M), temperature (10–40°C) and the synergetic effect by adding TOPO (solvating agent) were evaluated. Thermodynamic parameters including the Gibbs free energy (ΔG0),enthalpy (ΔH0), and entropy (ΔS0) were calculated. Performed experiments showed that Pb (II) can be extracted till 73% when Cd (II) can be recovered completely after two cycles. The extraction of both metallic ions was spontaneous, endothermic and with a slight randomness.  Positive synergetic effect was observed at  a chelating agent/TOPO ratio of 3. It is a very encouraging result which can lead us to recover cadmium and lower the concentration of lead from wastewater.


2010 ◽  
Vol 2010 ◽  
pp. 1-6 ◽  
Author(s):  
Mehrdad Balandeh ◽  
Sirous Asgari

LiNiO2powders were synthesized with acrylic acid, citric acid, oxalic acid, and triethanolamine (TEA) as a chelating agent. CrystallizedLiNiO2was synthesized in air at a calcinations temperature of 500∘Cfor 12 hours, when the molar ratio of chelating agents to total metal ion (RPM) was 1.0. The TEA-assisted method had the highest intensity ratio of (003)/(104) peaks of X-ray diffraction (XRD) spectrum. The transmission electron microscopy (TEM) analysis indicates that the sample prepared with triethanolamine obtained the smallest particle size with average particle size of only 12 nm. The results indicate that chelating agents have an important role in the intensity ratio of (003)/(104) peaks of XRD spectrum, size and shape of powders.


2021 ◽  
Vol 60 (7) ◽  
pp. 5014-5020
Author(s):  
Yuji Tada ◽  
Atsushi Sunada ◽  
Riki Watanabe ◽  
Makoto Kanazawa ◽  
Keiichiro Utsumi

Sign in / Sign up

Export Citation Format

Share Document