scholarly journals Synthesis and Spectroscopic Characterization of Lead(II)bis{O,O'-ditolyldithiophosphates} and their Adducts with 2,2'-Bipyridyl and 1,10-Phenanthroline

2011 ◽  
Vol 8 (s1) ◽  
pp. S113-S118
Author(s):  
Disha Jain Alok Chaturvedi ◽  
R.K. Upadhayay

The reaction of lead(II) dichloride with ammonium salts ofO,O'-ditolyldithiophosphoric acid have been carried out in 1:2 molar ratio by refluxing in benzene. These compounds have been further used to synthesize the adduct of the type lead(II)bis{O,O'-ditolyldithiophosphates}.2,2'-bipyridyl and lead(II)bis {O,O'-ditolyldithiophosphates}.1,10-phenanthroline by the reaction of lead(II)bis{O,O'-ditolyldithiophosphates} and 2,2'-bipyridyl and 1,10-phenanthro-line in the presence of unimolar dichloromethane and ethanol. All these complexes have been characterized by spectroscopic techniques such as IR,1H NMR and31P NMR. On the basis of spectroscopic studies tetracoordinated nature of lead atom in ditolyldithiophosphates complexes and hexacoordinated nature in their adducts have been established.

2013 ◽  
Vol 2013 ◽  
pp. 1-10
Author(s):  
Gauri D. Bajju ◽  
Deepmala ◽  
Sunil Kumar Anand ◽  
Sujata Kundan ◽  
Narinder Singh

A series of aluminium(III)-p-methyl-meso-tetraphenylporphyrin (p-CH3TPP-Al(III)) containing axially coordinated salicylate anion [p-CH3TPP-Al-X)], where X = salicylate (SA), 4-chlorosalicylate (4-CSA), 5-chlorosalicylate (5-CSA), 5-flourosalicylate (5-FSA), 4-aminosalicylate (4-ASA), 5-aminosalicylate (5-ASA), 5-nitrosalicylate (5-NSA), and 5-sulfosalicylate (5-SSA), have been synthesized and characterized by various spectroscopic techniques including ultraviolet-visible (UV-vis), infrared (IR) spectroscopy, proton nuclear magnetic resonance (1H NMR) spectroscopy,13C NMR, and elemental analysis. A detailed study of electrochemistry of all the synthesized compounds has been done to compare their oxidation and reduction mechanisms and to explain the effect of axial coordination on their redox properties.


2019 ◽  
Vol 17 (1) ◽  
pp. 571-580 ◽  
Author(s):  
Nevin Turan ◽  
Kenan Buldurun ◽  
Naki Çolak ◽  
İsmail Özdemir

AbstractThis study describes synthesis, spectroscopic characterization and catalytic activities of Fe(II), Ru(II), Pd(II) and Zn(II) complexes with a novel Schiff base ligand (L) derived from methyl 2-amino-5,5,7,7-tetramethyl-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate and terephthalaldehyde. We used spectroscopic techniques including IR, UV-Vis, 1H-NMR, 13C-NMR, elemental analysis and also mass analysis and magnetic susceptibility measurements to identify the products. The Pd(II) complex was used as a potential catalyst for Suzuki-Miyaura coupling reaction of some aryl halides under optimized conditions. The effect of various bases such as NaOH, KOH, and KOBut was investigated in transfer hydrogenation (TH) of ketones by isopropyl alcohol as the hydrogen source. Ru(II) and Pd(II) complexes showed catalytic activity while Zn(II) and Fe(II) metal complexes failed to do that.


1979 ◽  
Vol 34 (4) ◽  
pp. 579-584 ◽  
Author(s):  
Richard Ratka ◽  
Manfred L. Ziegler ◽  
Gerhard Schilling

Abstract The mechanism of formation of the exocyclic dimeric π-enyl complex (C8H13PdCl)2 by reaction of 1,3-dimethylenecyclohexane, C8H12 with trans-PdCl2(C6H5CN)2 is discussed. Through UV, 1H NMR (90 MHz, 360 MHz) and 13C spectroscopic studies it was possible to show that the dimer is formed by the disproportionate of C8H12 to C8H14 and m-xylene, and further that it consists of diastereomeric products. The reaction of (-) R-3-methyl-1-methylencyclohexane, C8H14, with the Pd-salt confirms that during the reaction between C8H12 and trans-PdCl2(C6H5CN)2 no free C8H14 is formed in solution.Studies on cleavage reactions of the dimer are also described in this paper.


2020 ◽  
Vol 45 (5) ◽  
Author(s):  
V.O. Uduah ◽  
J.J. Gongden ◽  
M.L. Kagoro ◽  
K.K. Gurumyen ◽  
Y.N. Lohdip ◽  
...  

This work presents a dry synthesis of Iron (III) complex with urea isolated from human urine and Fe (III) obtained from iron rust particles. Iron (III), PI (Purified iron rust), was isolated from iron rust in 10% hydrochloric acid, HCl and distilled water respectively. The complex was synthesized via dry-synthesis method using the melted urea as reaction medium. The isolated Fe (III) was characterized by elemental analysis which was done using XRF Cu-Zn method. The complex was prepared in a 1:4 metal to ligand (M-L) ratio. The stoichiometry of reaction indicate a 1:3 ratio of M-L (Fe-U). The complex was characterized by FT-IR, UV-vis, XRF and XRD spectroscopic techniques. The Fe (III) isolate and Fe-U complex shows percentage yields of 35.7% and ~92% respectively. The elemental and oxide composition of Fe and Fe2O3 (i.e., PI) were 40.387% and 57.753% respectively. The results obtained from the characterization of the iron-urea complex, IUC, indicate FT-IR result as symmetric and asymmetric frequencies with peaks of a combination band of Vs (NH) and Vas (NH), C=O and V (C-N) all stretched, XRD showed the crystal to be amorphous. The elemental and oxide composition of the Fe and Fe2O3 in IUC were 40.007 and 44.201 respectively. The results obtained revealed that useful complexes can be synthesized easily from waste materials, such as urine and iron rust particles, which complement Green chemistry.


2016 ◽  
Vol 13 (2) ◽  
pp. 105-114
Author(s):  
Baghdad Science Journal

New metal ion complexes were synthesized with the general formula; K[PtLCl4], [ReLCl4] and K[ML(Cl)2] where M = Pd(II), Cd(II), Zn(II) and Hg(II), from the Azo ligand (HL) [2-Hydroxy-3-((5-mercapto-1,3,4-thiadiazol-2-yl)diazenyl)-1-naphth aldehyde] (HL) the ligand was synthesized from (2-hydroxy-1-naphthaldehyde) and (5-amino-1,3,4-thiadiazole-2-thiol). The ligand and its metal complexes are characterized by phisco- chemical spectroscopic techniques (FT.IR, UV-Vis and Mass spectra, elemental analysis, molar conductivity, Atomic Absorption, Chloride contain and magnetic susceptibility). The spectral data suggest that the (HL) behaves as a bidentate ligand in all complexes. These studies revealed tetrahedral geometries for all metal complexes, except square planar for Pd(II) complex and except octahedral geometry for Pt(IV) and Re(V) complexes. The study of complexes formation via molar ratio of (M:L) as (1:1). Theoretical treatment of this ligand and its metal complexes in gas phase using Hyper chem.8 was preformed.


Polymers ◽  
2019 ◽  
Vol 11 (9) ◽  
pp. 1498 ◽  
Author(s):  
Abdul Hafeez ◽  
Zareen Akhter ◽  
John F. Gallagher ◽  
Nawazish Ali Khan ◽  
Asghari Gul ◽  
...  

Bis-aldehyde monomers 4-(4′-formyl-phenoxy)benzaldehyde (3a), 3-methoxy-4-(4′-formyl-phenoxy)benzaldehyde (3b), and 3-ethoxy-4-(4′-formyl-phenoxy)benzaldehyde (3c) were synthesized by etherification of 4-fluorobenzaldehyde (1) with 4-hydroxybenzaldehyde (2a), 3-methoxy-4-hydroxybenzaldehyde (2b), and 3-ethoxy-4-hydroxybenzaldehyde (2c), respectively. Each monomer was polymerized with p-phenylenediamine and 4,4′-diaminodiphenyl ether to yield six poly(azomethine)s. Single crystal X-ray diffraction structures of 3b and 3c were determined. The structural characterization of the monomers and poly(azomethine)s was performed by FT-IR and NMR spectroscopic techniques and elemental analysis. Physicochemical properties of polymers were investigated by powder X-ray diffraction, thermogravimetric analysis (TGA), viscometry, UV–vis, spectroscopy and photoluminescence. These polymers were subjected to electrical conductivity measurements by the four-probe method, and their conductivities were found to be in the range 4.0 × 10−5 to 6.4 × 10−5 Scm−1, which was significantly higher than the values reported so far.


2007 ◽  
Vol 79 (11) ◽  
pp. 2039-2046 ◽  
Author(s):  
Maiko Okajima-Kaneko ◽  
Masateru Ono ◽  
Kiyotaka Kabata ◽  
Tatsuo Kaneko

We extracted polysaccharides (PS) from Aphanothece sacrum using a hot alkaline solution which degraded other biopolymers such as proteins and nucleotides. The spectroscopy and elemental analyses indicated the PS contain carboxyls and sulfate groups. The degree of sulfation was estimated as about 10 mol %. 1H NMR studies demonstrated that the PS of A. sacrum had a dimethylated fucose unit. The combination of sulfate group and fucose in the prokaryotic PS was first evidenced by the direct spectroscopic studies. The PS showed efficient gelation behavior, binding to metal ions abundant in soil, and the swelling volume of the gel was approximately 250 times the dry volume. These results imply that PS of A. sacrum, which has been mass cultivated in Japan for a long time, may have potential as an environmentally benign water absorbent.


Author(s):  
Marta Siczek ◽  
Marcin Zawadzki ◽  
Miłosz Siczek ◽  
Agnieszka Chłopaś-Konowałek ◽  
Paweł Szpot

Abstract Purpose The aim of the study was to present the spectroscopic characteristics and crystal structure of the etazene—a benzimidazole opioid, which appeared on the illegal drug market in Poland in the last weeks. Methods The title compound was analyzed by X-ray crystallography as well as gas and liquid chromatography combined with mass spectrometry. Spectroscopic techniques have also been used, such as nuclear magnetic resonance, infrared and ultraviolet-visible spectroscopies. Results We presented the identification and the broad chemical characterization of etazene, a synthetic opioid that has recently been introduced on the illegal drug market. Conclusions In this paper, we described single-crystal X-ray, chromatographic and spectroscopic characterization of a synthetic opioid that emerged on the new psychoactive substance (NPS) market in Poland. To the best of our knowledge, this is the first full characterization of etazene. Analytical data presented in the work can be helpful in identification and detection of the NPS in forensic and clinical laboratories.


2002 ◽  
Vol 06 (03) ◽  
pp. 198-202 ◽  
Author(s):  
José L. Sosa-Sánchez ◽  
Alberto Galindo ◽  
Dino Gnecco ◽  
Sylvain Bernès ◽  
George R. Fern ◽  
...  

The synthesis and spectroscopic characterization of a new soluble silicon(IV) phthalocyanine complex is presented. The compound shows an increased solubility compared to its SiPcCl 2 precursor and this allowed solution 1 H NMR characterization. The assignment of the 1 H NMR signals for the axial ligands is greatly facilitated due to the anisotropic high ring current effects from the macrocycle. In addition, good quality crystals were grown from this more soluble material for molecular structure determination by single-crystal X-ray diffraction analysis. The molecular structure determination shows that the complex crystallizes in a non-centrosymmetric space group due to the inherent chirality of the naproxene ligands. Bond lengths and angles fit well to other analogous compounds previously reported.


2013 ◽  
Vol 2013 ◽  
pp. 1-26 ◽  
Author(s):  
Ricardo Tucceri ◽  
Pablo Maximiliano Arnal ◽  
Alberto Néstor Scian

This paper refers to spectroscopic studies carried out to identify the products ofo-aminophenol electro-oxidation and elucidate the structure of electrochemically synthesized poly(o-aminophenol) (POAP) films. Spectroscopic studies of the redox conversion of POAP are also reviewed.


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