Electrochemical and spectral properties of tris[tetra(15-crown-5)phthalocyaninato]dilutetium(III)

2005 ◽  
Vol 09 (01) ◽  
pp. 1-6 ◽  
Author(s):  
Igor V. Zhukov ◽  
Lyudmila A. Lapkina ◽  
Yuliya G. Gorbunova ◽  
Vladimir E. Larchenko ◽  
Aslan Yu. Tsivadze
Keyword(s):  
Cyclic Voltammetry ◽  
Spectral Properties ◽  
Redox Properties ◽  
X Ray ◽  
H Nmr ◽  
Nmr Data ◽  
Physicochemical Studies ◽  
First Time

Tris[tetra(15-crown-5)phthalocyaninato]dilutetium(III) ( R 4 Pc )3 Lu 2, whose structure had been confirmed earlier by X-ray analysis, was further examined by physicochemical studies. The redox properties of this complex were investigated by cyclic voltammetry. The spectroelectrochemical study of this compound has been performed for the first time. Based on the results obtained and analysis of literature data, an electrochemical criterion related to double- and triple-decker structure of lanthanide phthalocyanines has been proposed. IR and 1 H NMR data are also reported.

Synthesis and characterization of meso-to-meso directly linked porphyrin-diazaporphyrin triads

2018 ◽  
Vol 22 (09n10) ◽  
pp. 814-820
Author(s):  
Yingying Jia ◽  
Ling Xu ◽  
Bangshao Yin ◽  
Mingbo Zhou ◽  
Jianxin Song
Keyword(s):  
Nickel Complex ◽  
High Resolution Mass Spectrometry ◽  
Dihedral Angles ◽  
X Ray Diffraction ◽  
Extinction Coefficients ◽  
X Ray ◽  
H Nmr ◽  
First Time ◽  
Molar Extinction Coefficients

Beginning with 5,10,15-triarylporphyrin-nickel complex, five meso-to-meso directly linked porphyrin-diazaporphyrin triads were successfully prepared for the first time through a series of reactions including formylation via Vilsmeier–Haack reaction, condensation with pyrrole, bromination with [Formula: see text]-Bromosuccinimide (NBS), oxidation with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), metal-templated cyclization of dibromodipyrrin-metal complexes with NaN[Formula: see text] and demetalization. All these triads were comprehensively characterized by [Formula: see text]H NMR, high-resolution mass spectrometry and UV-vis absorption. In addition, the structure of compound 6Ni was unambiguously determined by X-ray diffraction analysis, which showed that the two dihedral angles are both 86.65 (4)[Formula: see text] between each mean plane of porphyrin and that of central diazaporphyrin The UV-vis absorption spectra disclosed that the longest wavelengths of Soret bands and Q bands for these triads were observed at 429 and 642 nm, respectively. In contrast to diazaporphyrin-porphyrin dyads, diazaporphyrin dimers and diazaporphyrin monomers reported previously the molar extinction coefficients, particularly for triad 8Ni are much higher.

Bleispezies PbX und PbX2 als Brückenliganden in übergangsmetallorganisch geschützten Koordinationsverbindungen/ Leadspecies PbX and PbX2 as Bridging Ligands in Organometallic Protected Coordination Compounds

2002 ◽  
Vol 57 (1) ◽  
pp. 25-42 ◽  
Author(s):  
Peter Rutsch ◽  
Gottfried Huttner
Keyword(s):  
Coordination Compounds ◽  
Dynamic Behaviour ◽  
Disodium Salt ◽  
3D Nmr ◽  
Spectroscopic Techniques ◽  
The Novel ◽  
Bridging Ligands ◽  
X Ray ◽  
Nmr Data ◽  
First Time

The disodium salt Na2[{(CO)5Cr}2Pb(NO3)2], Na2·1, which contains a lead center in a (4+2) coordination mode, reacts with tetraphenylphosphonium halides [Ph4P]X to give the tetrahedral compounds [Ph4P]2[{(CO)5Cr}2PbX2] (X = Cl: 2a; X = Br: 2b; X = I: 2c). Substitution of the nitrate groups of Na2·1 by alcoxides leads to binuclear compounds of the type [{(CO)5Crg2Pb(μ2-OR)2Pb{Cr(CO)5}2]2- (R = Et: 3a; R = n -Pr: 3b; R = i-Pr: 3c; R = Allyl: 3d). NMR experiments show that these dimeric compounds are in equilibrium with the monomeric species [{(CO)5Cr}2PbR]- .Trialkylphosphanes react with Na2·1 to give the neutral phosphane complexes [{(CO)5Cr}2Pb(PR3)2] (R=Me: 4a; R=Et: 4b; R = n-Bu: 4c), which show dynamic behaviour in solution. All of the novel compounds have been characterized by X-ray analysis, as well as by the usual analytic and spectroscopic techniques. 207Pb-NMR data of Cr(CO)5- bound lead species are reported for the first time.

scholarly journals Keggin-Type Heteropoly Salts as Bifunctional Catalysts in Aerobic Baeyer-Villiger Oxidation

Materials ◽  
2018 ◽  
Vol 11 (7) ◽  
pp. 1208 ◽  
Author(s):  
Katarzyna Pamin ◽  
Jan Połtowicz ◽  
Mateusz Prończuk ◽  
Joanna Kryściak-Czerwenka ◽  
Robert Karcz ◽  
...  
Keyword(s):  
Oxidation Mechanism ◽  
Decomposition Reaction ◽  
Redox Properties ◽  
Lewis Acidity ◽  
Bifunctional Catalysts ◽  
X Ray ◽  
Ethanol Decomposition ◽  
Iron Salts ◽  
First Time ◽  
Villiger Oxidation

The cobalt, manganese, and iron salts of tungstophosphoric or molybdophosphoric acid with growing content of metals were applied for the first time as catalysts in the Baeyer-Villiger (BV) oxidation of cyclohexanone to ε-caprolactone with molecular oxygen. The catalysts were characterized with Fourier transform infrared spectroscopy (FTIR), X-ray fluorescence (XRF), and ethanol decomposition reaction. Introduction of transition metals into the heteropoly structure increases the activity of resulting heteropoly salts in comparison with parent heteropolyacids. It was shown that the most active catalysts are salts of the heteropoly salts with one metal atom introduced and one proton left (HMPX) type, (where M = Co, Fe, Mn, and X = W, Mo) with the metal to proton ratio equal one. Among all of the studied catalysts, the highest catalytic activity was observed for HCoPW. The effect indicates that both the acidic and redox properties are required to achieve the best performance. The Baeyer-Villiger (BV) oxidation mechanism proposed identifies the participation of heteropoly compounds in three steps of the investigated reaction: oxidation of aldehyde to peracid (redox function), activation of carbonyl group (Lewis acidity), and decomposition of the Criegee adduct to ε-caprolactone (Brønsted acidity).

Preparation of New Anti-Slip Flooring Coatings: Hydrophobic MMA Floor Coatings

2013 ◽  
Vol 721 ◽  
pp. 73-76
Author(s):  
Shu Le Lin ◽  
Hui Hua Cai
Keyword(s):  
Electronic Spectroscopy ◽  
Dynamic Contact ◽  
Contact Angles ◽  
Coating Properties ◽  
Hydrophobic Properties ◽  
X Ray ◽  
H Nmr ◽  
Potential Applications ◽  
Ft Ir ◽  
First Time

For the first time, hydrophobic MMA floor coatings were prepared based on the fluorine-containing methacrylic ester copolymers and applied as a new kind of anti-slip flooring coatings. The composition of the synthesized copolymers was characterized by FT-IR and 1H-NMR. The prepared hydrophobic MMA floor coatings were analyzed for their coating properties. The hydrophobic properties of the coatings were characterized by static and dynamic contact angles and X-ray photo-electronic spectroscopy (XPS). Results show that the newly prepared floor coatings are easy to apply and have excellent mechanical and hydrophobic properties, which indicates that the hydrophobic MMA floor coatings have great potential applications in anti-slip flooring coatings.

Preparation and characterization of some ruthenium(II) porphyrins containing tertiary phosphine axial ligands, including the crystal structure of (octaethylporphinato)bis(triphenylphosphine)ruthenium(II)

1984 ◽  
Vol 62 (4) ◽  
pp. 755-762 ◽  
Author(s):  
Sara Ariel ◽  
David Dolphin ◽  
George Domazetis ◽  
Brian R. James ◽  
Tak W. Leung ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Phosphine Ligands ◽  
Tertiary Phosphine ◽  
X Ray ◽  
Porphyrin Complex ◽  
H Nmr ◽  
Axial Ligands ◽  
Nmr Data ◽  
Phosphine Complex

The ruthenium(II) porphyrin complex Ru(OEP)(PPh3)2 (OEP = the dianion of octaethylporphyrin) has been prepared from Ru(OEP)(CO)EtOH, and the X-ray crystal structure determined; as expected, the six-coordinate ruthenium is situated in the porphyrin plane and has two axial phosphine ligands. Synthesized also from the carbonyl(ethanol) precursors were the corresponding tris(p-methoxyphenyl)phosphine complex, and the Ru(TPP)L2 (TPP = the dianion of tetraphenylporphyrin, L = PPh3, P(p-CH3OC6H4)3, P″Bu3) and Ru(TPP)(CO)PPh3 complexes. Optical and 1H nmr data are presented for the complexes in solution. In some cases dissociation of a phosphine ligand to generate five-coordinate species occurs and this has been studied quantitatively in toluene at 20 °C for the Ru(OEP)L2 and Ru(TPP)L2 systems.

Spectroscopic and X-Ray Investigation of Cobalt(III) Complexes with 2-Oximinocarboxylic Acids

1993 ◽  
Vol 48 (4) ◽  
pp. 409-417 ◽  
Author(s):  
Rostislav D. Lampeka ◽  
Zamira D. Uzakbergenova ◽  
Victor V. Skopenko
Keyword(s):  
Electronic Absorption Spectra ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Octahedral Structure ◽  
Space Group ◽  
X Ray ◽  
H Nmr ◽  
Nmr Data ◽  
R Factors

Mixed complexes of Co(III) with 2-oximinopropionic (H2A) or 2-oximino-3-phenylpropionic (H2B) acid and different amine (imidazole, benzimidazole, pyridine, β-picoline, γ-picoline) are reported. Characterization of the complexes was based upon elemental analysis, conductivity and JR, 1H NMR, and electronic absorption spectra, and X-ray diffraction analysis. The organic ligands behave as O,N donors via the carboxyl oxygen and the oxime nitrogen atoms. A trans-octahedral structure has been assigned to the bis(2-oximinocarboxylato)bis(amine)cobalt(III) on the basis of 1H NMR data.The crystal and molecular structures of the complexes trans-[bis(2-oximinopropionato)bis-(imidazole)]- (I) and trans-[bis(2-oximinopropionato)bis(pyridine)]cobalt(III) (II) were determined. I crystallizes in space group P2/n with a = 14.1 67(2), b = 8.774(1), c = 14.785(2) Å,β = 113.37(1)°, Z = 4, Dcalc = 1.568 g · cm-3. II crystallizes in space group P1̄ with a = 9.122(2), b = 10.038(2), c = 11.759(2) Å, α = 69.95(1)°, β = 67.47(2)°, γ = 69.49(2)°, Ζ = 2, Dcalc = 1.547 g cm-3. The structures were refined to unweighted R factors of 0.036 and 0.028, respectively. The coordination sphere around Co is pseudo-octahedral with the 2-oximinopropionato ligands occupying four equatorial positions, and the amines in axial positions.

N,N′-Bis(trimethylsilyl) benzamidinato-Komplexe von Vanadium(V), Niob(V) und Tantal(V)/ N,N′-Bis(trimethylsilyl)benzamidinato Complexes of Vanadium(V), Niobium(V) and Tantalum(V)

1999 ◽  
Vol 54 (11) ◽  
pp. 1396-1404 ◽  
Author(s):  
Fritz Preuss ◽  
Michael Scherer ◽  
Christoph Klingshirn ◽  
Gabriele Hornung ◽  
Monika Vogel ◽  
...  
Keyword(s):  
Diffraction Analysis ◽  
Mass Spectra ◽  
X Ray ◽  
H Nmr ◽  
Nmr Data

N,N′-Bis(trimethylsilyl)benzamidinato complexes of vanadium(V), niobium(V) and tantalum( V) have been prepared starting from tBuN=MCl3 · n py and tBuN=MCpCl2, respectively: tBuN=V[PhC(NSiMe3)2] nCl3-n (n = 1, 2); tBuN=M[RC(NSiMe3)2]Cl · py [M = Nb. Ta; R = C6H5, C6H4(4-CF3)]; tBuN=MCp[RC(NSiMe3)2]Cl [M = V. Nb, Ta; R = C6H5, C6H4- (4-CF3)]; tBuN=VCp[PhC(NSiMe3)2](OtBu). The syntheses of silylated tert-butylamido complexes tBuN=M[NtBu-SiMe2-NHtBu]Cl2 · py (M = Nb, Ta), tBuN=V[NtBu-SiMe2-OtBu]Cl2 and tBuN=M[NtBu-SiMe2-OtBu]Cl2 · py [M = Nb, Ta (20)] are also described. The compounds have been investigated by 1H NMR data,51V NMR data, mass spectra. X-ray data diffraction analysis.

The coordination compounds of nickel with glycine and with an N-N ligand

1988 ◽  
Vol 53 (3) ◽  
pp. 563-570 ◽  
Author(s):  
František Březina ◽  
Zdeněk Šindelář ◽  
Jiří Kameníček ◽  
Jan Lasovský
Keyword(s):  
Cyclic Voltammetry ◽  
Coordination Compounds ◽  
Spectral Properties ◽  
Chemical Oxidation ◽  
Redox Properties

The compounds [Ni(Gly)2N-N].nH2O (n = 1, 2; Gly = glycine anion; N-N – ethylenediamine 1,10-phenanthroline, α,α’-bipyridyl) and K[Ni(Gly)3].3H2O were prepared. On the basis of their magnetochemical and spectral properties, the compounds obtained can be characterized as octahedral nickel(II) complexes. Cyclic voltammetry was employed to study the redox properties of selected compounds and possible electrochemical and chemical oxidation were studied. The results obtained permitted comparison with the properties of nickel(II) complexes with dipeptides or tripeptides as ligands.

Structure of isosilerolide, relative and absolute configuration of silerolide and lasolide - Sesquiterpenic lactones of new stereoisomeric type of eudesmanolides

1986 ◽  
Vol 51 (4) ◽  
pp. 903-929 ◽  
Author(s):  
Miroslav Holub ◽  
Miloš Buděšínský ◽  
Zdenka Smítalová ◽  
David Šaman ◽  
Urszula Rychłewska
Keyword(s):  
Absolute Configuration ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Nmr Data ◽  
Chemical Correlation ◽  
The Absolute

On the basis of spectroscopic, particularly 1H NMR data, isosilerolide was assigned structure I, including the absolute configuration. The structure was confirmed by X-ray diffraction. Isosilerolide represents a new stereoisomeric type of natural eudesmanolides, characterized as 5βH, 6αH, 7αH, 10αCH3-eudesman-6,12-olide. As shown by the chemical correlation of isosilerolide (I) with silerolide (III) and lasolide (X), the latter two natural lactones belong to this stereoisomeric group of eudesmanolides. Analysis of models and 1H NMR data shows that structures of some eudesman-6,12-olides, published by other authors, should be corrected.

Reaktion von 1.4-Dienen mit Metallkomplexen, I Darstellung und Röntgenstrukturanalyse eines π-enyl-Komplexes der Zusammensetzung (C8H13PdCl)2/ Reaction of 1,4-Dienes with Metal Complexes, I Synthesis and X-ray Structure Determination of a π-enyl Complex of Composition (C8H18PdCl)2

1976 ◽  
Vol 31 (4) ◽  
pp. 455-462 ◽  
Author(s):  
Peter Feldhaus ◽  
Richard Ratka ◽  
Hermann Schmid ◽  
Manfred L. Ziegler
Keyword(s):  
Metal Complexes ◽  
Structure Determination ◽  
Three Dimensional ◽  
Fourier Methods ◽  
X Ray ◽  
H Nmr ◽  
Nmr Data ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

Reaction of (C6H5CN)2PdCl2 and 1,3-dimethylenecyclohexane led to an exocyclic π-enyl complex of formula (C8H13PdCl)2-bis(η3-2-methylene-6-methylcyclohexyl)(di-µ-chloro)-dipalladium. IR and 1H NMR data are in agreement with this formulation.The compound is monoclinic, with unit cell dimensions α = 499.97 ± 0.08, b =1342.26 ± 0.19, c =1379.60 ± 0.20 pm, β = 99.43 ± 0.02°, space group C5h2-P21/C, Ζ = 2, dX-ray = 1.83 g/cm3.The structure was determined from three-dimensional X-ray data by Patterson and Fourier methods. Least squares refinement by use of 1045 independent reflections has reached R1 = 5.6%.

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