scholarly journals Colorimetric detection of hydrogen peroxide by dioxido-vanadium(V) complex containing hydrazone ligand: synthesis and crystal structure

2018 ◽  
Vol 5 (3) ◽  
pp. 171471 ◽  
Author(s):  
Sunshine D. Kurbah ◽  
Ibanphylla Syiemlieh ◽  
Ram A. Lal

Dioxido-vanadium(V) complex has been synthesized in good yield, the complex was characterized by IR, UV–visible and 1 H NMR spectroscopy. Single crystal X-ray crystallography techniques were used to assign the structure of the complex. Complex crystallized with monoclinic P 2 1 /c space group with cell parameters a (Å) = 39.516(5), b (Å) = 6.2571(11), c (Å) = 17.424(2), α (°) = 90, β (°) = 102.668(12) and γ (°) = 90. The hydrazone ligand is coordinate to metal ion in tridentate fashion through –ONO– donor atoms forming a distorted square pyramidal geometry around the metal ion.

2011 ◽  
Vol 8 (4) ◽  
pp. 1900-1910 ◽  
Author(s):  
Vinayak M. Naik ◽  
Nirmalkumar B. Mallur

A few eight coordinated complexes of lanthanide(III) nitrate with 2-benzimidazolyl mercaptoaceto hydrazone ligand (LH2) with the general formula [Ln(LH)2NO2]H2O (where Ln = La, Pr, Nd, Sm and Gd) have been synthesized and characterized by elemental analysis, magnetic susceptibility, molar conductance, UV-Visible, IR and1H NMR spectral studies. The experimental data sustain stoichiometry of 1:2 (metal/ligand) for the complexes. The spectral data shows that the ligand reacts in keto form and behaves as monobasic terdentate in nature. The nitrate appears to coordinate in the bidentate fashion to the metal ion. The thermal stabilities of the complexes have been studied by TGA and their kinetic parameters were calculated using Coats-Redfern and MKN methods. The antimicrobial activity studies have been under taken and results are discussed.


2021 ◽  
Vol 76 (3-4) ◽  
pp. 193-199
Author(s):  
Muhammad Said ◽  
Sadia Rehman ◽  
Muhammad Ikram ◽  
Hizbullah Khan ◽  
Carola Schulzke

Abstract Three guanidine-derived tri-substituted ligands viz. N-pivaloyl-N′,N″-bis-(2-methoxyphenyl)guanidine (L1), N-pivaloyl-N′-(2-methoxyphenyl)-N″-phenylguanidine (L2) and N-pivaloyl-N′-(2-methoxyphenyl)-N″-(2-tolyl)guanidine (L3) were reacted with Cu(II) acetate to produce the corresponding complexes. The significance of the substituent on N″ for the resulting molecular structures and their packing in the solid state has been studied with respect to the structural specifics of the corresponding Cu(II) complexes. The key characteristic of the guanidine-based metal complexation with Cu(II) is the formation of an essentially square planar core with an N2O2 donor set. As an exception, in the complex of L1, the substituent’s methoxy moiety also interacts with the Cu(II) center to generate a square-pyramidal geometry. The hydroxyl groups of the imidic acid tautomeric forms of L1–L3, in addition to N″, are also bonded to Cu(II) in all three complexes rather than the nitrogen donor of the guanidine motif.


2000 ◽  
Vol 78 (9) ◽  
pp. 1214-1221 ◽  
Author(s):  
John E Drake ◽  
Jincai Yang

O-alkyl monothiocarbonate (monoxanthate) derivatives of tin were obtained by the reaction of a sodium salt of the monothiocarbonic acid with an organotin chloride to give Ph3Sn[SCO2R], Ph2Sn[SCO2R]2, and Me3Sn[SCO2R], where R = Me and i-Pr. The compounds have been characterized by infrared, Raman, 1H NMR, and 13C NMR spectroscopy, as well as mass spectrometry, and in two cases by X-ray crystallography. Ph3Sn[SCO2Me] (1) and Ph3Sn[SCO2(i-Pr)] (2), crystallize in the triclinic space group P[Formula: see text] (no. 2) with cell parameters a = 10.218(4), b = 10.568(6), c = 9.366(7) Å, α = 106.73(5), β = 96.99(5), γ = 85.55(4)°, V = 960(1) Å3, and Z = 2 for 1; and a = 14.793(2), b = 17.856(3), c = 9.813(3) Å, α = 103.86(5), β = 98.36(5), γ = 106.85(4)°, V = 2343(1) Å3, and Z = 2 for 2. The latter has two molecules in the asymmetric unit. The immediate environment about tin in both 1 and 2 is that of the expected distorted tetrahedron. However, the orientation of the monothiocarbonate group is such that there is an Sn-O intramolecular interaction of 3.040(8) for 1 and 3.05(2) Å on average for 2. Thus, the considerable distortion is consistent with a tendency to form a five-coordinate, trigonal bipyramidal species with one of the O-Sn-C angles approaching 180o (153.4(4) for 1 and an average of 157.1(6) for 2). Estimations of the Pauling partial bond orders suggest this weak Sn-O interaction is slightly stronger than the corresponding Ge-O interaction in the analogous germanium derivative, Ph3Ge[SCO2Me].Key words: structure, tin, methyl, phenyl, isopropyl, monothiocarbonates.


2014 ◽  
Vol 2014 ◽  
pp. 1-7
Author(s):  
Gauri D. Bajju ◽  
Altaf Ahmed ◽  
Deepmala Gupta ◽  
Ashu Kapahi ◽  
Gita Devi

The synthesis and spectroscopic characterization of new axially ligated indium(III) porphyrin complexes were reported. Chloroindium(III) porphyrin (TPPIn-Cl) was obtained in good yield by treating the corresponding free base with indium trichloride. The action of the different phenols on chloroderivatives (TPPIn-Cl) led to the corresponding phenolato complexes (TPPIn-X). These derivatives were characterized on the basis of mass spectrometry,1H-NMR, IR, and UV-visible data. The separation and isolation of these derivatives have been achieved through chromatography. The spectral properties of free base porphyrin and its corresponding metallated and axially ligated indium(III) porphyrin compounds were compared with each other. A detailed analysis of UV-Vis,1H-NMR, and IR suggested the transformation from free base porphyrin to indium(III) porphyrin. Besides,13C-NMR and fluorescence spectra were also reported and interpreted. The stability of these derivatives has also been studied through thermogravimetry. The complexes were also screened for anticancerous activities. Among all the complexes, 4-MePhO-InTPP shows highest anticancerous activity. The title complexe, TPPIn-X (where X = different phenolates), represents a five-coordinate indium(III) porphyrin complex in a square-pyramidal geometry with the phenolate anion as the axial ligand.


2017 ◽  
Vol 70 (12) ◽  
pp. 1269
Author(s):  
Steven Gareth Williams ◽  
Mohan Bhadbhade ◽  
Roger Bishop ◽  
Alison Thavary Ung

The reaction of (–)-β-pinene with KCN under a mild bridged Ritter reaction gave (1S,5R,6S)-2,2,6-trimethyl-3-aza-bicyclo[3.3.1]non-3-en-6-yl acetate that subsequently reacted to provide an unexpected (1S,4R,5R,6S)-4-cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonane-6-yl acetate. The structure of the compound was determined by high-resolution mass spectrometry, and IR and NMR spectroscopy and confirmed by single crystal X-ray crystallography. The compound crystallises in the monoclinic P21 space group, with unit cell parameters a 8.6120 (17), b 7.4570 (15), c 11.189 (2) Å, and β 110.16 (3)°.


2015 ◽  
Vol 19 (10) ◽  
pp. 1107-1113 ◽  
Author(s):  
Qiong Yu ◽  
Wei-Xia Xu ◽  
Ya-Hong Yao ◽  
Zeng-Qi Zhang ◽  
Shu Sun ◽  
...  

One novel porphyrin 5,10,15-tris(phenyl)-20-[4-(2-(2-methyl-5-nitro-imidazolyl)ethoxyl)phenyl] porphyrin and its zinc(II) metalloporphyrin were synthesized and characterized by IR, UV-vis, 1H NMR, MS and elemental analysis. The single crystal structure of zinc(II) porphyrin shows that the Zn(II) ion is coordinated with four nitrogen atoms of porphyrin ring and one oxygen atom of ethanol from axial, forming a five-coordinated square pyramidal geometry. Their cytotoxicity and photodynamic activity against breast cancer cells were studied. The results indicate that both of the porphyrins display high phototoxicity to the breast cancer cells with the negligible dark toxicity. In addition, the photodynamic activity of zinc(II) porphyrin was obviously higher than that of the free porphyrin.


RSC Advances ◽  
2016 ◽  
Vol 6 (68) ◽  
pp. 63837-63847 ◽  
Author(s):  
Nayan Roy ◽  
Surjatapa Nath ◽  
Abhijit Dutta ◽  
Paritosh Mondal ◽  
Pradip C. Paul ◽  
...  

A new coumarin based Schiff-base chemosensor was synthesized and evaluated. Based on Job’s plot,1H NMR titration, ESI-MS and B-H plot, the structure of ligand and its metal ion is 1 : 1 stoichiometry. It also exhibits a binary logic function.


2007 ◽  
Vol 11 (01) ◽  
pp. 42-49 ◽  
Author(s):  
B. Narayana Achar ◽  
T. M. Mohan Kumar

A novel series of nitrone-substituted, metal phthalocyanine complexes (the central metal ion being Co , Ni and Cu , respectively) were synthesized for the first time in pure state with quantitative yield. These complexes were characterized using elemental analysis, UV-visible, IR-spectroscopy, magnetic susceptibility, X-ray crystallography, and thermogravimetry. All three complexes had a monoclinic structure with different crystal lattice constants. Horowitz-Metzger, Coats-Redfern and Broido's relations were employed to calculate the kinetic and activation parameters associated with the thermal decomposition of the above complexes. Electrical conductivity studies were undertaken for all three complexes using a two-probe technique in the temperature range 30-200°C. They showed an improvement of 103-105 times the electrical conductivity at room temperature, compared to the corresponding unsubstituted metal phthalocyanines.


2014 ◽  
Vol 70 (a1) ◽  
pp. C1831-C1831
Author(s):  
Lo Kong Mun ◽  
Chew Shin Thung ◽  
Tan Kong Wai

A series of copper(II) complexes containing phosphonium substituted hydrazone, (L) with the formulations [CuL]Cl and [Cu(L')L]Cl, where L = doubly deprotonated hydrazone; L' = 1,10'-phenanthroline, 2,2'-bipyridine, 4,4-bipyridine and 5,5'-dimethyl-2,2'-bipyridine has been synthesized. The compounds were characterized by elemental analysis, IR and NMR spectroscopic methods and in the case of crystalline products by X-ray crystallography. The crystal structure of [CuL]Cl and the extent of distortion from ideal square pyramidal geometry for CuL')(l)]Cl will be discussed. The cytotoxicity and topoisomerase I (topo I) inhibition activities of these compounds were also studied. It is noteworthy that the addition of N,N-ligands to the copper(II) complex lead to the enhancement in the cytotoxicity of the compounds, especially against human prostate adenocarcinoma cell line (PC-3). The complexes can also inhibit topo I through the binding to DNA and the enzyme.


Author(s):  
Meriem Saidi ◽  
Michel Giorgi ◽  
Leila Boukli-hacene

The title complex, [(CH3)2NH2][Cr(C6H10NO4)2Cl]·H2O, was synthesized sonochemically. The complex anion consists of a chromium(II) ion ligated by two 3-carboxy-2-(dimethylamino)propanoate anions. They coordinate in a bidentate manner, with a carboxylate oxygen atom and the nitrogen atom cis to each other in the equatorial plane, while the apical position is occupied by a Cl− ion. Hence, the chromium(II) ion is five-coordinate with a quasi-ideal square-pyramidal geometry; τ5 parameter = 0.01. The complex crystallizes as a monohydrate and in the crystal, the water molecule and the dimethylammonium counter-ion link the complex cations via N—H...O, N—H...Cl, Owater—H...O, O—H...Owater and O—H...O hydrogen bonds, forming a supramolecular framework. There are also a number of C—H...O hydrogen bonds present that reinforce the framework structure. The crystal studied was refined as a racemic twin.


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