Synthesis and spectral characterization of bis(β-diketonato)zirconium(IV) and -hafnium(IV) phthalocyaninates

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.

2001 ◽  
Vol 05 (10) ◽  
pp. 717-720 ◽  
Author(s):  
M. S. AǦIRTAŞ ◽  
Ö. BEKAROǦLU

The synthesis of new metal-free and zinc(II), cobalt(II) phthalocyanines substituted with four 4-(2-N'-cyanoethyl)aminoethylsulfanyl groups is described. The new compounds have been characterized by elemental analysis and IR, 1 H NMR and UV-vis spectroscopy.


2017 ◽  
Vol 68 (10) ◽  
pp. 2436-2439
Author(s):  
Stefania Felicia Barbuceanu ◽  
Laura Ileana Socea ◽  
Constantin Draghici ◽  
Elena Mihaela Pahontu ◽  
Theodora Venera Apostol ◽  
...  

In the work we presented the behavior of 5-(4-(4-X-phenylsulfonyl)phenyl)-4-(n-propyl)-2H-1,2,4-triazole-3(4H)-thiones (X= Cl or Br) with some alkylation agents. Thus, new S-alkylated 1,2,4-triazole derivatives were synthesized by reaction of the corresponding 1,2,4-triazole-3-thione derivatives with different �-halogenated compounds (ethyl bromide, ethyl chloroacetate or phenacyl bromide), in basic medium. The structures of synthesized compounds were elucidated by spectral data (1H-NMR, 13C-NMR, mass spectrometry) and elemental analysis.


2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Md. Hasan Zahir

Reaction of Ce3+with p-tert-butylcalix[n]arene (n=4,6,8) yields purple crystalline complexes structurally as [Ce(p-tert-butylcalix[4]arene-3H)2(NO3)(DMF)x](2 −x)DMF (1), [Ce(p-tert-butylcalix[6]arene-4H)2(NO3)(DMF)x](3 −x)DMF (2), and [Ce(p-tert-butylcalix[8]arene-7H)2(NO3)(DMF)6] (3), whereDMF=N,N-dimethylformamide. The properties and coordination characteristics of the three calixarene complexes were determined by elemental analyses, electronic absorption, X-ray absorption spectroscopy (EXAFS), TG-DTA, FT-IR, SEM, and1H-NMR spectroscopy. The effect of various organic solvents on complexes1,2, and3has been discussed based on results from electronic absorption spectra. The polar protic solvents showed the most significant molar extinction coefficients in comparison with those of nonpolar and polar aprotic solvents. The Ce3+ions in the complexes are proved to combine with the ligand phenolic groups, oxygen atoms of DMF molecules, and/or OH−ions.


RSC Advances ◽  
2017 ◽  
Vol 7 (24) ◽  
pp. 14389-14394 ◽  
Author(s):  
Ling-Bao Xing ◽  
Fei Qiao ◽  
Zhao Yuan ◽  
Jing-Li Zhang ◽  
Rui-Ying Zhang ◽  
...  

New binuclear alkynylplatinum(ii) terpyridyl complexes with flexible bridges have been synthesized and characterized by 1H NMR, mass spectra and elemental analysis.


1980 ◽  
Vol 35 (7) ◽  
pp. 802-807 ◽  
Author(s):  
Michael Kopp ◽  
Luise R. Krauth ◽  
Richard Ratka ◽  
Klaus Weidenhammer ◽  
Manfred L. Ziegler

The reaction of cis-(C6H5CN)2PtCl2 and Na2PtCl4 with the dienes 1,4-pentadiene and 2,5-diphenyl-1,5-hexadiene yields the species cis-(1,4-pentadiene) PtCl2 and cis-(2,5-diphenyl-1,5-hexadiene)PtCl2, respectively. The compounds have been fully characterized by elemental analysis, IR, 1H-NMR, mass spectroscopy and by X-ray methods


2017 ◽  
Vol 41 (16) ◽  
pp. 7932-7937 ◽  
Author(s):  
Ilya A. Khodov ◽  
Olga V. Maltceva ◽  
Vladimir V. Klochkov ◽  
Oscar I. Koifman ◽  
Nugzar Zh. Mamardashvili

The complexation of 2-aza-21-carba-tetraphenylporphyrin and 2-aza-2-methyl-5,10,15,20-tetraphenyl-21-carbaporphyrin with nickel and zinc acetates in organic solvents has been investigated by UV-Vis spectroscopy and 1H NMR.


2016 ◽  
Vol 846 ◽  
pp. 706-711 ◽  
Author(s):  
Nurliana Roslan ◽  
Salasiah Endud ◽  
Zainab Ramli ◽  
Hendrik Oktendy Lintang

Synthetic metalloporphyrins have long been recognized either as functional models or mimics of the cytochrome P-450 enzymes and they are versatile compounds with potential use in drug delivery, catalysis and electronics. In the present study, the metalloporphyrin, (meso-tetra-(p-sulfonatophenyl)-porphyrinato)copper, CuTSPP was synthesized in the reaction between free-base porphyrin, meso-tetra (p-sulfonatophenyl)porphyrin, H2TSPP and copper(II) acetate monohydrate. The materials were characterized using Fourier Transform Infrared Spectroscopy (FTIR), Ultraviolet-Visible (UV-Vis) Spectroscopy, Proton Nuclear Magnetic Resonance (1H NMR) Spectroscopyand Mass Spectrometry (MS) analysis. The FTIR spectra of both free-base porphyrin and CuTSPP showed the appearance of three pronounced bands indicating the presence of the salt form (R-SO3Na) of the sulfonic acid group. Characterization of CuTSPP by UV-Vis spectroscopy confirmed that the insertion of copper into the free-base porphyrin was successful by the appearance of the Soret band and Q bands. The catalytic activity of CuTSPP was tested in the oxidation of 2,3,6-trimethylphenol (TMP) at 60 °C using hydrogen peroxide (H2O2) as oxidant. The reaction parameters including the reaction temperature and time have been optimized. The only product obtained by means of TMP oxidation with H2O2 using CuTSSP is 2,3,5-trimethylbenzoquinone (TMBQ), an important precursor for the industrial production of Vitamin E.


1997 ◽  
Vol 488 ◽  
Author(s):  
In Tae Kim ◽  
Ronald L. Elsenbaumer

AbstractA series of poly(N-alkylpyrrylene vinylenes)( alkyl = methyl(l), hexyl(2), dodecyl(3)) have been synthesized from the monomer, N-alkyl-2,5-bis(thiophenylmethylene)pyrrole, by base induced elimination and polymerization. The resulting deep purple conjugated polymers (2, 3) were soluble in a variety organic solvents. The electrical conductivities of the polymers lie in the range, 10−2 to 2.5 S/cm. The highest yield was obtained when the polymers were synthesized in refluxing THF with a monomer/ base mole ratio of 1/4. The optical band gap of the undoped polymers were 1.89 eV(1), 1.69 eV(2) and 1.65 eV(3). Characterization of the polymers includes IR, CV, 1H and 13C NMR, UV-vis spectroscopy, TGA and molecular weight studies.


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 ?).


2019 ◽  
Vol 23 (11n12) ◽  
pp. 1592-1602 ◽  
Author(s):  
Yumeela Ganga-Sah ◽  
Elahe Tajbakhsh ◽  
Rachel H. Platel ◽  
Wen Zhou ◽  
Daniel B. Leznoff

The preparation and structural characterization of a pair of scandium(III) phthalocyanine hydroxide complexes were achieved by reaction of PcScCl with alkali metal alkoxides, likely via hydrolysis of soluble PcSc-alkoxide intermediates. A Sc[Formula: see text]Li[Formula: see text]-OH)[Formula: see text] cubane supported by two distorted Pc rings of the form (PcSc)[Formula: see text]-OH)[Formula: see text]Li[Formula: see text](THF)(DME) was isolated from the reaction of PcScCl with LiO[Formula: see text]Pr, while a simpler alkali-metal-free [Pc[Formula: see text]Sc[Formula: see text]-OH)[Formula: see text](THF)] was obtained from addition of NaO[Formula: see text]Bu; both structures are reminiscent of bent metallocenes, with dihedral angles between the two Pc rings of 50.8 and 37.7[Formula: see text]respectively. A soluble PcScOH material can also be obtained directly via hydrolysis of insoluble PcScCl in approximately 95:5 THF:water. Reduction of the Pc ring of PcScCl using KC[Formula: see text] is reversible and generates Pc[Formula: see text] and Pc[Formula: see text]-containing materials that were characterized via UV-vis spectroscopy and, where appropriate EPR and [Formula: see text]H NMR spectroscopy; analogous reductions of the PcScOH-based species were irreversible. Exposure of the air-sensitive, reduced PcScCl-based species to ambient atmosphere generated PcScOH materials analogous to the direct hydrolysis route.


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