Synthesis and Properties of Tetrakis(trimethylsilyl)-phthalocyaninatoruthenium(II)

Author(s):  
KAI DÜRR ◽  
MICHAEL HANACK

Tetrakis(trimethysilyl)phthalocyaninatoruthenium(II) (5) has been synthesized via the biaxially coordinated (( CH 3)3 Si )4 PcRu (3- Clpy )2 (2) complex by thermal decomposition of the axial ligands of 2. (( CH 3)3 Si )4 PcRu (5) was characterized by NMR, IR and UV-vis spectroscopy and elemental analysis. The trisubstituted (( CH 3)3 Si )3 PcRu (3- Clpy )2 (3) and disubstituted (( CH 3)3 Si )2 PcRu (3- Clpy )2 (4) complexes, formed as side products during the thermolysis of 2, could be isolated and characterized.

2011 ◽  
Vol 7 (2) ◽  
pp. 1338-1347
Author(s):  
Tarek Ali Fahad ◽  
Shaker.A.N. AL-Jadaan

Two new heterocyclic Organmercury compounds   were prepared from the reaction of Sulfamethaxazole and Sulfadiazine with 4-acetaminophenol as a coupler and separated as solids with characteristic colors. these compounds were characterized by F.T.IR-spectroscopy 1H-NMR , Micro-elemental Analysis and UV-Vis spectroscopic techniques . The work involves a study of acid – base properties compounds at different pH values, the ionization and protonation constants were calculated. The thermal behavior of these two compounds   were investigated on the basis of thermogravimetric (TGA) and differential thermogravimetric (DTG) analyses, Thermal decomposition of these compounds is multi-stage processes.


2002 ◽  
Vol 06 (02) ◽  
pp. 114-121 ◽  
Author(s):  
L. A. Tomachynski ◽  
V. Ya. Chernii ◽  
S. V. Volkov

The reaction of PcMCl 2 ( M = Zr , Hf ) with β-diketones is reported. 1 H NMR and elemental analysis suggest the substitution of two Cl atoms for two β-diketone fragments takes place as a result of this reaction and the complexes PcM(β-dik)2 are formed. All obtained complexes are stable and highly soluble in most organic solvents. The data from 1 H and 19 F NMR, and UV-vis spectroscopy suggest the coordination of two β-diketone ligands in a cis geometry about the central atom of the macrocycle. It was shown bis(β-diketonato)zirconium(IV) and hafnium(IV) phthalocyanines containing β-diketones with donor or acceptor groups or with bulky substituents can be obtained.


2018 ◽  
Vol 38 ◽  
pp. 02019
Author(s):  
Yong-xin Zhao ◽  
Ying-qiang Zhang

Highly transparent silicone resin with self-crosslinking structure was prepared using phenyltrimethoxysilane, diphenyldimethoxysilane, 1,3,5,7-cyclotetra(methyl siloxane) and bisvinyltetramethyldisiloxane as main raw materials. The structure of silicone resin was determined by Fourier Transform Infrared Spectroscopy (FT-IR). The light transmittance was measured by UV-Vis spectroscopy. Thermogravimetric analysis (TGA) was used to study the thermal decomposition process. The microstructure of cured self-crosslinking silicone resin is more uniform, resulting in better light transmittance up to 100% in the range of 400nm ~ 800nm. The cured has relatively good heat resistance, the initial thermal decomposition temperature of the cured could be up to 315.8 °C. SEM observations show that the self-crosslinking silicone has a uniform, textured structure, higher transparency compared with the existing condensation silicone material, and can be used as advanced architectural translucent materials and optics packaging materials.


2013 ◽  
Vol 49 (2) ◽  
pp. 275-283 ◽  
Author(s):  
André Luis Máximo Daneluti ◽  
Jivaldo do Rosário Matos

Phytic acid is a natural compound widely used as depigmenting agent in galenic cosmetic emulsions. However, we have observed experimentally that phytic acid, when heated to 150 ºC for around one hour, shows evidence of thermal decomposition. Few studies investigating this substance alone with regard to its stability are available in the literature. This fact prompted the present study to characterize this species and its thermal behavior using thermal analysis (TG/DTG and DSC) and to associate the results of these techniques with those obtained by elemental analysis (EA) and absorption spectroscopy in the infrared region. The TG/DTG and DSC curves allowed evaluation of the thermal behavior of the sample of phytic acid and enabled use of the non-isothermal thermogravimetric method to study the kinetics of the three main mass-loss events: dehydration I, dehydration II and thermal decomposition. The combination of infrared absorption spectroscopy and elemental analysis techniques allowed evaluation of the intermediate products of the thermal decomposition of phytic acid. The infrared spectra of samples taken during the heating process revealed a reduction in the intensity of the absorption band related to O-H stretching as a result of the dehydration process. Furthermore, elemental analysis results showed an increase in the carbon content and a decrease in the hydrogen content at temperatures of 95, 150, 263 and 380 °C. Visually, darkening of the material was observed at 150 °C, indicating that the thermal decomposition of the material started at this temperature. At a temperature of 380 °C, thermal decomposition progressed, leading to a decrease in carbon and hydrogen. The results of thermogravimetry coupled with those of elemental analysis allow us to conclude that there was agreement between the percentages of phytic acid found in aqueous solution. The kinetic study by the non-isothermal thermogravimetric method showed that the dehydration process occurred in two stages. Dehydration step I promoted a process of vaporization of water (reaction order of zero), whereas dehydration step II showed an order of reaction equal to five. This change in reaction order was attributed to loss of chemically bonded water molecules of phytic acid or to the presence of volatile substances. Finally, the thermal decomposition step revealed an order of reaction equal to one. It was not possible to perform the kinetic study for other stages of mass loss.


2004 ◽  
Vol 69 (12) ◽  
pp. 1053-1061 ◽  
Author(s):  
Josef Husárek ◽  
Richard Pstorek ◽  
Michal Malon ◽  
Zedenek Sindalar ◽  
Marek Pavlícek

A series of new Ni(II) dithiocarbamate compounds of the composition [NiX(cetdtc)(PR3)](X = Cl, Br, I, NCS; cetdtc = cyclohexylethyldithiocarbamate; R = phenyl, n-butyl) has been synthesized. All the isolated complexes have been characterized by elemental analysis, IR and UV/VIS spectroscopy, 31P{1H}-NMR spectroscopy, thermal analysis magnetochemical and conductivity measurements. On the basis of the results of the physico-chemical study, all complexes are diamagnetic, non-electrolytes with a square-planar NiS2PX chromophore.


2021 ◽  
Vol 68 (4) ◽  
pp. 1008-1015
Author(s):  
Yong Yuan ◽  
Xi-Kun Lu ◽  
Gao-Qi Zhou ◽  
Xiao-Yang Qiu

Three new copper(II) complexes, [Cu(LH)2]Br2 (1), [Cu(LH)2]NCS2 (2), and [Cu(LH)2](NO3)2 (3), where LH is the zwitterionic form of 2-bromo-6-((2-(isopropylamino)ethylimino)methyl)phenol (HL), were synthesized and characterized by elemental analysis, IR and UV-vis spectroscopy. The structures of the complexes were further confirmed by single crystal X-ray structure determination. All compounds are mononuclear copper(II) complexes. The Cu atoms in the complexes are coordinated by two imino N and two phenolate O atoms from two LH ligands, forming square planar coordination. The compounds were assayed for their antimicrobial activities.


2011 ◽  
Vol 396-398 ◽  
pp. 2485-2488
Author(s):  
Bao Hua Zhu ◽  
Guo Hua Xu ◽  
Zhi Wei Xia

One new Ruthenium and one known Iron bimetallic carbonyl clusters containing triphos (1,1,1-tris(diphenylphosphinomethyl)ethane) ligand have been prepared as catalyst to study the reduction of amide to amine. All clusters were characterized by elemental analysis, 1HNMR, 31PNMR and IR spectroscopy. The reduction of N,N-dimethylbenzamide and N,N-diethyl-(3-methyl) benzamide catalyzed by Ru and Fe carbonyl clusters were investigated at 100 ~ 110 °C for 24 ~ 28h, polymethylhydrogensiloxane (PMHS) as reduction agent. The products were analysized using GC-MS, IR and UV-vis spectroscopy and an excellent yield (97%) of N,N-diethyl- (3-methyl)benzamine was obtained when using 3 mol% of bimetallic ruthenium carbonyl cluster as catalyst. The data of IR and UV-vis show that the frameworks of clusters are not changed remarkably during the reaction.


2005 ◽  
Vol 498-499 ◽  
pp. 535-539
Author(s):  
Crislene Rodrigues da Silva Morais ◽  
Wilton Silva Lopes ◽  
A.G. de Souza ◽  
P.D. Santa-Cruz

This work deals with the synthesis and thermal decomposition of complexes of general formula: Ln(ß-dik)3L (where Ln=Tb+3, ß-dik=4,4,4-trifluoro-1-phenyl-1,3- butanedione(btfa) and L=1,10-fenantroline(phen) or 2,2-bipiridine(bipy). The powders were characterized by melting point, FTIR spectroscopy, UV-visible, elemental analysis, scanning differential calorimeter(DSC) and thermogravimetry(TG). The TG/DSC curves were obtained simultaneously in a system DSC-TGA, under nitrogen atmosphere. The experimental conditions were: 0.83 ml.s-1 carrier gas flow, 2.0±0.5 mg samples and 10°C.min-1 heating rate. The CHN elemental analysis of the Tb(btfa)3bipy and Tb(btfa)3phen complexes, are in good agreement with the expected values. The IR spectra evinced that the metal ion is coordinated to the ligands via C=O and C-N groups. The TG/DTG/DSC curves of the complexes show that they decompose before melting. The profiles of the thermal decomposition of the Tb(btfa)3phen and Tb(btfa)3bipy showed six and five decomposition stages, respectively. Our data suggests that the thermal stability of the complexes under investigation followed the order: Tb(btfa)3phen < Tb(btfa)3bipy.


2013 ◽  
Vol 749 ◽  
pp. 521-526
Author(s):  
Si Jiao Wang ◽  
Xiang Rong Liu ◽  
Chao Chao Song ◽  
Shun Shen Zhao ◽  
Lan Ying Yan ◽  
...  

The 2-carboxybenzaldehyde-1H-benzotriazol-1-aceylhydrazone (C16H13N5O3) has been synthesized and used in preparing thirteen novel rare earth complexes. The complexes were characterized by elemental analysis, FT-IR, and UV-Vis, and the formula is RE (C16H11N5O3)·NO3·xH2O·yC2H5OH (RE=La, Ce, Pr, Nd, Sm, Eu, Tb, Ho, Er, Yb) and RE(C16H12N5O3)2·NO3·5H2O (RE=Gd, Dy, Y) .The thermal decomposition processes of the thirteen complexes were studied by thermal gravimetric technology and their apparent activation energy values were calculated by Kissingers and Ozawass method.


2011 ◽  
Vol 76 (6) ◽  
pp. 865-877 ◽  
Author(s):  
Ljiljana Vojinovic-Jesic ◽  
Vukadin Leovac ◽  
Mirjana Lalovic ◽  
Valerija Cesljevic ◽  
Ljiljana Jovanovic ◽  
...  

The first two complexes of dioxovanadium(V) with salicylaldehyde thiosemicarbazone (SALTSC), of the coordination formulas [VO2(SALTSC-H)]?H2O (1) and NH4[VO2(SALTSC-2H] (2), were synthesized and characterized by elemental analysis, conductometric measurements, IR and UV-vis spectroscopy and X-ray analysis. The complexes were obtained in the reaction of an aqueous ammoniacal solution of NH4VO3 and SALTSC. The results of the characterization showed that SALTSC was coordinated in the usual ONS tridentate mode as monoanion in complex 1 and dianion in complex 2. In both complexes, the vanadium atom is in a deformed square-pyramidal environment and is slightly shifted towards the apical oxo-ligand (? 0.52 ?).


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