scholarly journals Complexes of light lanthanides with 2,3-dimethoxybenzoic acid

2001 ◽  
Vol 66 (8) ◽  
pp. 543-553 ◽  
Author(s):  
Wieslawa Ferenc ◽  
Agnieszka Walków-Dziewulska
Keyword(s):  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
Magnetic Measurements ◽  
Magnetic Moments ◽  
Intermediate Formation ◽  
Carboxylate Group ◽  
X Ray ◽  
Light Lanthanides ◽  
Thermogravimetric Studies ◽  
Low Symmetry

The complexes of light lanthanides with 2,3-dimethoxybenzoic acid of the formula: Ln(C9H9O4)3, where Ln = La(III), Ce(III), Pr(III), Nd(III), Sm(III), Eu(III) and Gd(III) have been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric studies, as well as X-ray and magnetic measurements. The complexes have colours typical for Ln3+ ions (La, Ce, Eu, Gd-white, Sm-cream, Pr-green, Nd-violet). The carboxylate group in these complexes is a bidentate, chelating ligand or a tridentate chelating and bridging one. They are crystalline compounds characterized by low symmetry. On heating in air to 1173 K, the 2,3-dimethoxybenzoates of the light lanthanides decompose in various ways. The complexes of Ce(III), Pr(III), Sm(III), Eu(III) and Gd(III) decompose directly to oxides of the respective metals while those of La(III) and Nd(III) via the intermediate formation of La2O2CO3 and Nd2O2CO3. The solubilities of the 2,3-dimethoxybenzoates of the light lanthanides in water at 293Kare in the orders of 10-3-10-2 mol dm-3. The magnetic moments were determined in the range 4.2-298 K and the complexes are found to obey the Curie-Weiss law.

scholarly journals Complexes of light lanthanides with 2,4-dimethoxybenzoic acid

2000 ◽  
Vol 65 (1) ◽  
pp. 27-35 ◽  
Author(s):  
Wieslawa Ferenc ◽  
Agnieszka Walków-Dziewulska
Keyword(s):  
Ir Spectroscopy ◽  
Intermediate Formation ◽  
Carboxylate Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
One Step ◽  
Light Lanthanides ◽  
Thermogravimetric Studies ◽  
Hydrated Complexes ◽  
Two Stages

The complexes of light lanthanides with 2,4-dimethoxybenzoic acid of the formula: Ln(C9H9O4)3.nH2O where Ln = La(III), Ce(III), Pr(III), Nd(III), Sm(III), Eu(III), Gd(IIII), and n = 3 for La(III), Gd(III), n = 2 for Sm(III), Eu(III), and n = 0 for Ce(III), Pr(III), Nd(III) have been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric studies and X-ray diffraction measurements. The complexes have colours typical for Ln 3+ ions (La, Ce, Eu, Gd-white, Sm-cream, Pr-green, Nd-violet). The carboxylate group in these complexes is a symmetrical, bidentate, chelating ligand. They are crystalline compounds characterized by various symmetry. On heating in air to 1273 K the 2,4-dimethoxybenzoates of the light lanthanides decompose in various ways. The hydrated complexes decompose in two or three steps while those of anhydrous ones only in one or two. The trihydrate of lanthanum 2,4-dimethoxybenzoate first dehydrates to form the anhydrous salt, which then decomposes to La2O3 via the intermediate formation of La2O2CO3. The hydrates of Sm(III), Eu(III), Gd(III) decompose in two stages. First, they dehydrate forming the anhydrous salts, which then decompose directly to the oxides of the respective metals. The anhydrous complexes of Ce(III), Pr(III) decompose in one step, while that of Nd(III) in two. The solubilities of the 2,4-dimethoxybenzoates of the light lanthanides in water and ethanol at 293 K are in the order of: 10 -3 mol dm -3 and 10 -4.10 -3 mol dm-3, respectively.

Complexes of Light Lanthanides with 3,4-Dimethoxybenzoic Acid

2000 ◽  
Vol 65 (2) ◽  
pp. 179-191 ◽  
Author(s):  
Wiesława Ferenc ◽  
Agnieszka Walków-Dziewulska
Keyword(s):  
Magnetic Moments ◽  
Intermediate Formation ◽  
Lanthanide Ions ◽  
Ligand Field ◽  
X Ray Diffraction ◽  
Magnetic Studies ◽  
X Ray ◽  
Light Lanthanides ◽  
Polycrystalline Solids ◽  
Van Vleck

The complexes of light lanthanides with 3,4-dimethoxybenzoic acid, Ln(C9H9O4)3·4 H2O, where Ln = La(III), Ce(III), Pr(III), Nd(III), Sm(III), Eu(III) and Gd(III), have been synthesized as polycrystalline solids and characterized by elemental analysis, IR spectroscopy, thermogravimetric and magnetic studies and X-ray diffraction measurements. The complexes possess colours typical of Ln(III) ions (La, Ce, Eu, Gd white, Pr greenish, Nd violet and Sm cream). The carboxylate group in these complexes binds as a symmetrical, bidentate chelating ligand. On heating in air to 1 273 K the 3,4-dimethoxybenzoates of Ce(III), Pr(III), Sm(III), Eu(III) and Gd(III) first dehydrate to anhydrous salts that further decompose to oxides of the respective metals. The 3,4-dimethoxybenzoates of La(III) and Nd(III) decompose in three steps. Firstly, they dehydrate to anhydrous salts that further decompose to the oxides with the intermediate formation of oxycarbonates. The solubilities of the studied complexes in water at 293 K is in the order of 10-4-10-3 mol dm-3. Their magnetic moments were determined in the temperature range 77-298 K and found to obey the Curie-Weiss law. The values of μeff calculated for the all compounds (except that for Eu) are close to those obtained for Ln(III) by Hund and van Vleck. The results show that there is no influence of the ligand field on 4f electrons of the lanthanide ions in these polycrystalline compounds; 4f electrons probably do not participate in the formation of the Ln-O bonds.

scholarly journals Spectral and thermal behaviors of rare earth element complexes with 3,5-dimethoxybenzoic acid

2003 ◽  
Vol 68 (10) ◽  
pp. 751-763 ◽  
Author(s):  
Wieslawa Ferenc ◽  
Agnieszka Walkóv-Dziewulska ◽  
Janusz Chrusciel
Keyword(s):  
Rare Earth ◽  
Rare Earth Elements ◽  
Rare Earth Element ◽  
Earth Element ◽  
Magnetic Measurements ◽  
Quantitative Composition ◽  
Carboxylate Group ◽  
X Ray ◽  
Thermogravimetric Studies ◽  
Hydrated Complexes

The conditions for the formation of rare earth element 3,5-dimethytoxybenzoates were studied and their quantitative composition and solubilities in water at 293 K were determined. The complexes are anhydrous or hydrated salts and their solubilities are of the orders of 10-5 ? 10-4 mol dm-3. Their FTIR, FIR and X-ray spectra were recorded. The compounds were also characterized by thermogravimetric studies in air and nitrogen atmospheres and by magnetic measurements. All complexes are crystalline compounds. The carboxylate group in these complexes is a bidentate chelating ligand. On heating in air to 1173 K, the 3,5-dimethoxybenzoates of rare earth elements decompose in various ways. The hydrated complexes first dehydrate to form anhydrous salts which then decompose in air to the oxides of the respective metals while in nitrogen to mixtures of carbon and oxides of the respective metals. The complexes are more stable in air than in nitrogen.

scholarly journals Magnetic, thermal and spectral characterization of 2,6-dimethoxybenzoates of Co(II), Ni(II) and Cu(II)

2006 ◽  
Vol 31 (2) ◽  
pp. 17-24 ◽  
Author(s):  
W. Ferenc ◽  
A. Walków-Dziewulska ◽  
J. Sarzynski
Keyword(s):  
Elemental Analysis ◽  
Magnetic Moments ◽  
Chelating Ligands ◽  
Carboxylate Group ◽  
X Ray Diffraction ◽  
Acid Anion ◽  
Magnetic Studies ◽  
X Ray ◽  
Polycrystalline Solids

The complexes of 2,6-dimethoxybenzoic acid anion with ions of Co(II), Ni(II), and Cu(II) have been synthesized as polycrystalline solids, and characterized by elemental analysis, spectroscopy, magnetic studies, and also by X-ray diffraction and thermogravimetric measurements. The analysed complexes have following colours: pink for Co(II), green for Ni(II), and blue for Cu(II) compounds. The carboxylate group binds as monodentate, and bidentate bridging and chelating ligands. On heating in air to 1173 K the complexes decompose in four, three or two steps. At first, they dehydrate in one or two steps to anhydrous salts, that next decompose to oxides of the respective metals. The solubility of the investigated dimethoxybenzoates in water at 293 K is of the order of 10-2 mol/dm3. Their magnetic moments were determined in the temperature range of 76-303 K. The results reveal the compounds of Co(II) and Ni(II) to be high-spin complexes and that of Cu(II) to form dimer.

scholarly journals Magnetic, thermal and spectroscopic properties of lanthanide(III) 2-(4-chlorophenoxy) acetates, Ln(C8H6ClO3)3•nH2O

2013 ◽  
Vol 78 (9) ◽  
pp. 1335-1349 ◽  
Author(s):  
Wiesława Ferenc ◽  
Beata Cristóvão ◽  
Jan Sarzyński
Keyword(s):  
Magnetic Moments ◽  
Intermediate Formation ◽  
Spectroscopic Properties ◽  
Ligand Field ◽  
X Ray Diffraction ◽  
Magnetic Susceptibilities ◽  
X Ray ◽  
Gaseous Products ◽  
Carboxylate Groups ◽  
Thermogravimetric Studies

4-Chlorophenoxyacetates of lanthanides(III) were synthesized as polycrystalline hydrated solids with the general formulae: Ln(C8H6ClO3)3?2H2O (Ln = La(III), Pr(III), Sm(III), Eu(III) and Tb(III)), Ln(C8H6ClO3)3?H2O (Ln = Dy(III)) and Ln(C8H6ClO3)3?3H2O (Ln = Er(III), Tm(III), Yb(III) and Lu(III) and characterized by elemental analysis, FTIR spectroscopy, magnetic and thermogravimetric studies and also by X-ray diffraction (XRD) measurements. The complexes have colours typical for lanthanide(III) ions. The carboxylate groups bind as bidentate chelating. On heating to 1273 K in air the complexes decompose in three steps. At first they dehydrate in one stage to form anhydrous salts that next decompose to the oxides of respective metals with the intermediate formation of their oxychlorides. The gaseous products of compound thermal decomposition in nitrogen were also determined and the magnetic susceptibilities were measured over the ranges 76-303K and 1.8-303K, and their magnetic moments were calculated. The results show that 4-chlorophenoxyacetates of lanthanides(III) are high-spin complexes with weak ligand field.

[Zn(phen)2(CX3COO)]+, X = H orCl; Influence of X on the Coordination Mode of the Carboxylate Group (phen = 1,10-Phenanthroline)

2005 ◽  
Vol 60 (10) ◽  
pp. 1049-1053 ◽  
Author(s):  
Zeanab Talaei ◽  
Ali Morsali ◽  
Ali R. Mahjoub
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Mode ◽  
Bidentate Ligand ◽  
Carboxylate Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Coordinate Geometry ◽  
C Nmr

Two new ZnII(phen)2 complexes with trichloroacetate and acetate anions, [Zn(phen)2(CCl3COO)- (H2O)](ClO4) and [Zn(phen)2(CH3COO)](ClO4), have been synthesized and characterized by elemental analysis, IR, 1H NMR, 13C NMR spectroscopy. The single crystal X-ray data of these compounds show the Zn atoms to have six-coordinate geometry. From IR spectra and X-ray crystallography it is established that the coordination of the COO− group is different for trichloroacetate and acetate. The former acts as a monodentate whereas the latter acts as a bidentate ligand.

scholarly journals Synthesis and structure of macrocyclic dinickel(II) complex with 5-(4-pyridyl)tetrazolate as coligand

2021 ◽  
pp. 3-10
Author(s):  
Sergei V. Voitekhovich ◽  
Berthold Kersting ◽  
Oleg A. Ivashkevich
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Dinuclear Complex ◽  
X Ray Diffraction ◽  
X Ray

The dinuclear nickel(II) complex [Ni2LmClO4] + , where Lm represents a 24-membered macrocyclic hexaaza-dithiophenolate ligand, reacts with 5-(4-pyridyl)tetrazole (PyrCN4H) to give the dinuclear complex [Ni2Lm(PyrCN4)]+ . The new complex was both isolated as perchlorate or tetraphenylborate salts and characterised by elemental analysis and IR spectroscopy. The structure of [Ni2Lm(PyrCN4)]BPh4 ⋅ MeCN was determined by single crystal X-ray diffraction, showing that tetrazolate units are in a N2,N3-bridging mode to generate dioctahedral N3Ni(µ-S)2(µ-N4CPyr)NiN3 core.

1,3,5-Tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane

2016 ◽  
Vol 71 (1) ◽  
pp. 81-84 ◽  
Author(s):  
Eugen Weisheim ◽  
Hans-Georg Stammler ◽  
Norbert W. Mitzel
Keyword(s):  
Mass Spectrometry ◽  
Ir Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

AbstractThe reaction of 1,3,5-triethynyl-1,3,5-trimethyl- 1,3,5-trisilacyclohexane with (dimethylamino)trimethylstannane afforded 1,3,5-tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane with tin-functionalised ethynyl groups. The compound was characterized by single-crystal X-ray diffraction, elemental analysis, mass spectrometry, NMR and FT-IR spectroscopy.

scholarly journals Coordination Polymers of Scandium(III) and Thiophenedicarboxylic Acid

2021 ◽  
Vol 47 (9) ◽  
pp. 593-600
Author(s):  
A. A. Lysova ◽  
V. A. Dubskikh ◽  
K. D. Abasheeva ◽  
A. A. Vasileva ◽  
D. G. Samsonenko ◽  
...  
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Coordination Polymers ◽  
Elemental Analysis ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
Phase Purity ◽  
X Ray ◽  
Metal Organic

Abstract Three new metal−organic frameworks based on scandium(III) cations and 2,5-thiophenedicarboxylic acid (H2Tdc) are synthesized: [Sc(Tdc)(OH)]·1.2DMF (I), [Sc(Tdc)(OH)]·2/3DMF (II), and (Me2NH2)[Sc3(Tdc)4(OH)2]·DMF (III) (DMF is N,N-dimethylformamide). The structures of the compounds are determined by single-crystal X-ray structure analysis (CIF file CCDC nos. 2067819 (I), 2067820 (II), and 2067821 (III)). The chemical and phase purity of compound I is proved by elemental analysis, thermogravimetry, X-ray diffraction analysis, and IR spectroscopy.

scholarly journals Synthesis, characterization, electrochemical studies and X-ray structures of mixed-ligand polypyridyl copper(II) complexes with the acetate

2016 ◽  
Vol 81 (11) ◽  
pp. 1251-1262 ◽  
Author(s):  
Oluwafunmilayo Adekunle ◽  
Ray Butcher ◽  
Oladapo Bakare ◽  
Olusegun Odunola
Keyword(s):  
Room Temperature ◽  
Magnetic Measurements ◽  
Magnetic Moments ◽  
Copper Ion ◽  
X Ray Diffraction ◽  
Visible Spectroscopy ◽  
X Ray ◽  
Elemental Analyses ◽  
Structural Details ◽  
Uv Visible

[Cu(phen)2(CH3COO)](ClO4).2H2O (1) and [Cu(bipy)2(CH3COO)]-(ClO4).H2O (2) {phen = 1,10-phenanthroline, bipy = 2,2?-bipyridine}were synthesized and characterized. The complexes were characterized by employying elemental analyses, infrared and UV-Visible spectroscopy, room temperature magnetic measurements and the crystal structures elucidated using X-ray diffraction experiment. The redox properties of the complexes were also investigated. Both structures have a square pyramidal CuN4O chromophore which exhibit significant distortions due to long Cu-O [2.217(3) ? for (1) and 2.179 (1) for (2)] and Cu-N [2.631(2) ? for (1) and 2.714(1) ? for (2)] bonds. This distortion if further shown by the O-Cu-N bond angles [147.71(8) o for (1) and 153.40(5) o for (2)]. The elemental analyses further support the structural details unveiled by the single crystal X-ray diffraction analysis. The infrared spectra shows the acetate vibrational frequencies at 1587 cm-1,1428 cm-1, 1314 cm-1 for (1) and 1571 cm-1, 1441 cm-1, 1319c m-1 for (2) and the perchlo-rate bands at 1059 cm-1, 720 cm-1 (1) and 1080 cm-1,768 cm-1 (2). The broad d-d bands for the copper ion at 14,514 cm-1(1) and 14,535 cm-1(2) support the adoption of square pyramid geometries. The magnetic moments for the two complexes are 1.83 B.M for (1) and 1.72 B.M for (2). The peak to peak values of the two complexes show that the electrode reactions are quasi-reversibile with ?Ep = 0.023V (1) and 0.025V for (2). In both structures, there are ?-? intermolecular interactions in addition to hydrogen bonding between the units.

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