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1.
Synthesis and some properties of light lanthanide complexes with 4,4′-bipyridine and dibromoacetates
A. Czylkowska 《Journal of Thermal Analysis and Calorimetry》2013,114(3):989-995
In this study, new complexes with formulae: Ce(4-bpy)(CHBr2COO)3·H2O, Ln(4-bpy)0.5(CHBr2COO)3·2H2O (where Ln(III) = Pr, Nd, Sm; 4-bpy = 4,4′-bipyridine) and Eu(4-bpy)(CHBr2COO)3·2H2O were prepared, and characterized by chemical and elemental analyses, and IR spectroscopy. The way of metal–ligand coordination was discussed. They are small crystalline. The complexes of Pr(III), Nd(III), and Sm(III) are isostructural in group. Conductivity studies (in methanol, dimethylformamide, and dimethylsulfoxide) were also performed and described. The thermal properties of complexes in the solid state were studied using TG–DTG techniques under dynamic flow of air atmosphere. TG–MS system was used to analyze principal volatile thermal decomposition and fragmentation products evolved during pyrolyses of Ce(III) and Sm(III) complexes in dynamic flow of air atmosphere. 相似文献
2.
Journal of Thermal Analysis and Calorimetry - New complexes with formulae: Ln(4-bpy)(CBr2HCOO)3·3H2O (where Ln(III) = Gd, Tb, Dy) and Er(4-bpy)1.5(CBr2HCOO)3·3H2O, were... 相似文献
3.
Agnieszka Czylkowska Danuta Czakis-Sulikowska Rafał Kruszyński Mirosława Markiewicz 《Structural chemistry》2010,21(2):415-423
A novel mixed-ligand complexes of Er(III), Yb(III) and Lu(III) with title ligands were prepared and characterized by chemical
and elemental analysis and IR spectroscopy, conductivity (in methanol, dimethyloformamide and dimethylsulphoxide). The thermal
properties of complexes in the solid state were studied. The mode of metal–ligand coordination was discussed. The title compounds
are isomorphic and isostructural in solid state. All atoms in studied compounds lie in general positions but occurrence of
inversion on the midpoint of the bond linking two pyridine rings leads to existence in asymmetric unit one complex molecule
and half of outer coordination sphere 4-bpy molecule. All chelating carboxylate groups are symmetrically bonded to the metal
cations. The molecules of studied compounds are connected to the three dimensional network via O–H···O and O–H···N intermolecular
hydrogen bonds. In the structures also exist C–H···O, C–H···Cl weak hydrogen bonds and π····π stacking interactions. 相似文献
4.
A. Czylkowska D. Czakis-Sulikowska A. Kaczmarek M. Markiewicz 《Journal of Thermal Analysis and Calorimetry》2011,105(1):331-339
A novel mixed-ligand complexes with empirical formulae: Ln(4-bpy)1.5(CCl3COO)3·nH2O (where Ln(III) = Pr, Sm, Eu, Gd, Tb; n = 1 for Pr, Sm, Eu and n = 3 for Gd, Tb; 4-bpy = 4,4′-bipyridine) were prepared and characterized by chemical, elemental analysis and IR spectroscopy.
Conductivity studies (in methanol, dimethylformamide and dimethylsulfoxide) were also described. All complexes are crystalline.
The way of metal–ligand coordination was discussed. The thermal properties of complexes in the solid state were studied under
non-isothermal conditions in air atmosphere. During heating the complexes decompose via intermediate products to the oxides:
Pr6O11, Ln2O3 (for Sm, Eu, Gd) and Tb4O7. TG-MS system was used to analyze principal volatile thermal decomposition and fragmentation products evolved during pyrolysis
of Pr(III) and Sm(III) compounds in air. 相似文献
5.
《Journal of Coordination Chemistry》2012,65(5):692-704
Two new complexes {[Tb(2-IBA)3 · 2,2′-bipy]2 · C2H5OH} (1) and [Tb(2-ClBA)3 · 2,2′-bipy]2 (2) (2-IBA = 2-iodobenzoate; 2-ClBA = 2-chlorobenzoate; 2,2′-bipy = 2,2′-bipyridine) were prepared and their crystal structures determined by X-ray diffraction. Complex 1 is composed of two types of binuclear molecules, [Tb(2-IBA)3 · 2,2′-bipy]2 (a) and [Tb(2-IBA)3 · 2,2′-bipy]2 (b), and an uncoordinated ethanol molecule. In molecule (a), two Tb3+ ions are linked by four 2-IBA groups, all bidentate-bridging. In molecule (b), two Tb3+ ions are held together by four 2-IBA groups in two coordination modes, bidentate-bridging and chelating-bridging. In the two molecules, each Tb3+ ion is further bonded to one chelating 2-IBA group and one chelating 2,2′-bipy molecule, resulting in coordination numbers of eight for (a) and nine for (b). The structural characteristics of 2 are similar to that of molecule (b) in 1. The two complexes, 1 and 2, both emit strong green fluorescence under ultraviolet light with the 5D4 → 7F j (j = 6–3) emission of Tb3+ ion observed. 相似文献
6.
D. Czakis-Sulikowska J. Radwańska-Doczekalska M. Markiewicz 《Monatshefte für Chemie / Chemical Monthly》1994,125(10):1075-1082
Summary New complexes of 2,2-dipyridyl and 4,4-dipyridyl with thulium salts TmX
3 (whereX=Cl–, Br–, NO
3
–
, NCS–, and ClO
4
–
) have been prepared and their solubilities in water at 21 °C were determined. The IR spectra of these compounds are discussed. The conditions of thermal decomposition of the complexes were also studied.
Synthese und Eigenschaften von 2,2-Dipyridyl- und 4,4-Dipyridylkomplexen mit Thuliumsalzen
Zusammenfassung Es wurden neue 2,2-Dipyridyl- und 4,4-Dipyridyl-Komplexen mit Thuliumsalzen TmX 3 (X=Cl–, Br– No 3 – , NCS–, ClO 4 – ) dargestellt und ihre Wasserlöslihkeit bei 21 °C bestimmt. Die IR-Spektren werden diskutiert. Das thermische Verhalten der erhaltenen Komplexe wurde untersucht.相似文献
7.
4,4′-Bipyridine belong to an important class of compounds with wide applications in different fields and since the formation charge transfer compounds give opportunity to improve the physical and chemical properties of different donors so charge transfer compounds of 4,4′-bipyridine (Bpy) with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), 2,5-dichloro-3,6-dihydroxy-1,4-benzoquinone [chloranilic acid] (CHA) and 2,3,5,6-tetrachloro-1,4-benzoquinone [choloranil] (CHL) were studied. The stoichiometries of the reactions were determined from photometric titration methods. Although the thermodynamic parameters [Gibbs free energy (ΔG°), enthalpy (ΔH°), and entropy change (ΔS°)] were calculated. The thermal decomposition of the complexes follows first order kinetics and thermodynamic parameters of the decomposition were calculated. The structural morphology was investigated by scanning electron microscopy (SEM) and Transmission Electron Microscopy (TEM) and show that these molecules are of nanosize. 相似文献
8.
A. Czylkowska 《Journal of Thermal Analysis and Calorimetry》2012,110(3):1299-1308
Novel mixed-ligand complexes with empirical formula Ln(4-bpy)2(CCl3COO)3·nH2O [where Ln(III)?=?Dy, Ho, Er, Tm, Yb, Lu; 4-bpy?=?4,4??-bipyridine] were prepared and characterized by chemical and elemental analysis, infrared spectroscopy, and conductivity measurements (in methanol, dimethylformamide, and dimethyl sulfoxide). X-ray powder diffraction patterns indicate that the complexes are small crystalline compounds. IR spectra of complexes show that all carboxylate groups and 4-bpy are engaged in coordination of lanthanide ions. The thermal behavior of complexes was studied by means of TG, DTG, DTA techniques in the solid state under nonisothermal conditions in air atmosphere. During heating, the complexes decompose via intermediate products to the oxide Ln2O3. The combined TG?CFTIR technique was employed to study the decomposition pathway of the Ho(III) and Tm(III) complexes in flowing argon atmosphere. 相似文献
9.
《Journal of Coordination Chemistry》2012,65(17):3045-3057
Three new diruthenium(III) complexes, [Ru2O(2-sb)2(2,2′-bipy)2(H2O)2]·2.5H2O (1), [Ru2O(3-sb)2(2,2′-bipy)2(H2O)2]·9H2O (2), and [Ru2O (4-sb)2(2,2′-bipy)2(H2O)2]·9H2O (3), where sb2? is sulfobenzoate dianion and 2,2′-bipy is 2,2′-bipyridine, were synthesized using hydrothermal methods and characterized by IR, elemental analysis, thermogravimetric analysis, UV–vis, and fluorescence spectra. The single crystal X-ray analysis showed that each of these complexes has a dinuclear core stabilized by two bridging carboxylates and one bridging O2?. Variable sb2? ligands (2-sb, 3-sb, and 4-sb) in these complexes lead to diverse electronic spectroscopic behavior. The efficiency of activating methyl phenyl sulfide oxidation utilizing H2O2 in 3 equiv. was studied at 23?±?2?°C. The effect of the amount of catalyst and solvents on activities was investigated. Under optimized reaction conditions, the major product was sulfoxide. Complex 1 gave significant conversion of 100 and 98% selectivity for sulfoxide after 4?h. 相似文献
10.
Agnieszka Czylkowska Mirosława Markiewicz 《Journal of Thermal Analysis and Calorimetry》2010,100(2):717-723
A novel mixed-ligand complexes with empirical formulae: Dy(4-bpy)(CCl2HCOO)3 · H2O and Ln(4-bpy)1.5(CCl3COO)3 · 2H2O (where Ln(III) = Ce, Nd) were prepared and characterized by chemical and elemental analysis and IR spectroscopy, conductivity
(in methanol, dimethyloformamide and dimethylsulfoxide). Analysis of the diffractograms showed that the obtained complexes
are crystalline. Way of metal-ligand coordination discussed. The thermal properties of complexes in the solid state were studied
under non-isothermal conditions in air atmosphere. During heating the complexes decompose via intermediate products to the oxides: Ln2O3 (Nd, Dy) and CeO2. TG-MS system was used to analyse principal volatile thermal decomposition and fragmentation products evolved during pyrolysis
of Dy(4-bpy)(CCl2HCOO)3 · H2O in air. 相似文献
11.
The reaction of [HN(n-C4H9)3]3[WV(CN)8]·4H2O, 4,4′-bipyridine dioxide(4,4′-dpdo), and MnCl2·4H2O or CuCl2·2H2O gives two new three-dimensional octacyanometalate-based bimetallic assemblies, {[Mn2 (4,4′-dpdo)(H2O)4] [WIV(CN)8]}·6H2O (1) and {[Cu2(4,4′-dpdo)(H2O)][W(CN)8]}·CH3OH·H2O (2). Compound 1 crystallizes in the orthorhombic system, space group P21212 with cell constants a=10.397(2) -, b= 11.321(2) -, c=12.295(3) - and Z=2, whereas 2 crystallizes in the monoclinic system, space group P21/c with cell con... 相似文献
12.
13.
Noha Said Bedowr Rosiyah Binti Yahya Nesrain Farhan 《Journal of Saudi Chemical Society》2018,22(3):255-260
This paper presents synthesis, structural characterization and spintronic applications of copper (II) tetradecanoate derived magnetic complexes. The complexes were prepared by a chemical reaction between [Cu2(CH3(CH2)12COO)4](EtOH)2 and 2,2′-bipyridine-4,4′-bipyridine ligands respectively. The complexes were further reacted between the product of the first reaction and 4,4′-bipyridine-2,2′-bipyridine respectively. The structural characterization techniques included elemental analysis, Fourier transformed infrared spectroscopy (FTIR), Ultra-violet–Visible (UV–Vis) spectroscopy, polarized optical microscopy, magnetic moment and thermogravimetric analysis. The structural and characterization results suggested that the synthesized complexes were binuclear and mononuclear covalent complexes of copper(II) with structural formulas [Cu2(η2-(OOCR)4](4,4′-bpy)2H2O] and [Cu(η1-(OOCR)2(2,2′-bpy) (4,4′-bpy)] respectively. 相似文献
14.
The three-dimensional complex {[Nd(bpdc)1.5(DMF)]·1.4DMF}n (DMF=N,N′-dimethylformamide, bpdc=biphenyl-4,4′-dicarboxylate) was synthesized using the solvothermal method. The crystal structure of the neodymium(III) complex has been determined by single-crystal X-ray diffraction method at 100(2) K. The polymeric structure consists of neodymium polyhedra bridged by bpdc ligands. Eight-coordinated Nd(III) atoms are surrounded by seven oxygen atoms from six bpdc moieties and one oxygen atom from the DMF molecule. The 3D structure of the complex contains two types of channels occupied by DMF molecules. Thermal analysis revealed that DMF molecules are lost in a stepwise manner. The infrared spectrum confirmed full deprotonation of acid and presence of DMF molecules in the structure. 相似文献
15.
《Journal of Coordination Chemistry》2012,65(12):2159-2169
Four new platinum(II) complexes (1–4) with N-benzoyl-L-amino acid and bipy were synthesized and characterized by elemental analysis, IR, UV, 1H NMR, and mass spectra. The crystal structure of 1 was determined by X-ray diffraction analysis. Cytotoxicities were measured by MTT and SRB assays. Complexes 1–4 exert cytotoxicity with selectivity against HL-60, Bel-7402, BGC-823, and KB cell lines. This suggests that amino acids and acylated groups have important effects on cytotoxicity; the cytotoxicity is also related to the species of tumor cells, but the IC50 values do not show definite correlation with the variation of amino acids and acylated groups. 相似文献
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17.
The reactions of AgNO3 with combinations of 1,2-bis(4-pyridyl)ethane(bpa)/4,4′-bipyridine (bpy), 4,4′-stilbenedicarboxylic acid (H2sda)/2,2′-diphenylaminedicarboxylic acid (H2dpadc)/2,6-naphthalenedicarboxylic acid (H2ndc) in aqueous alcohol/ammonia at room temperature produce block-like crystals of [Ag2(bpa)1.5(sda)0.5](sda)0.5·7H2O, [Ag2(bpa)2(H2O)3](dpadc), [Ag2(bpy)2](ndc)·4H2O. All three complexes consist of 1D infinite silver–ligand cationic chains, interspersed with organic carboxylate anions that provide charge compensation in the crystal structures. The lattice water molecules are situated among the framework of the crystal structure and show rich hydrogen-bonding interactions, which help to orientate the organic carboxylate anions in the crystal packing, and the presence of Ag···N and Ag···Ag contacts contributes to strengthen the frameworks. The luminescent properties and thermogravimetric analyses of the three complexes are also presented. 相似文献
18.
19.
《Journal of Saudi Chemical Society》2019,23(7):781-794
A new bioactive material of cobalt(II) with 5,10,15,20-tetrakis[4 (benzoyloxy)phenyl] porphyrin (TPBP) and bpy ligands ([CoII(TPBP)(bpy)2] 1) has been synthesized and characterized by Single-crystal X-ray diffraction (SCXRD), spectroscopic methods and quantum-chemistry calculations. In the crystalline structures of six coordinated Co(II) [CoII(TPBP)(bpy)2] 1, linear 1D polymeric chains were observed in which all the porphyrin units are aligned parallel to each other. The crystal packing is stabilized by inter-and intramolecular C–H⋯O and C–H⋯N hydrogen bonds, and by weak C–H⋯Cg π interactions. Interestingly, NBO–Second-order perturbation theory analysis, carried out at the UB3LYP/6-31G(d)/SDD DFT level of theory, demonstrated that a two-center bond between the nitrogen atoms and the cobalt ions (Co) was not found, the Co–Npy/bp interactions are coming from an electronic delocalization between the Npy/Nbp filled orbitals to the anti-bonding LP*(4) and LP*(5) metal NBOs. Mass spectroscopy, and elemental analysis were also investigated to confirm the molecular structure. The downfield shift and the peak broadening of the axial ligand resonances observed in the 1H NMR indicated the contiguity to the paramagnetic Co(II) center. Additionally, the photophysical properties have been evaluated by UV–visible absorption, and fluorescence emission spectroscopies. Finally, bioactivity investigations revealed that free porphyrin TPBP, CoIITPBP and complex 1 could be used as potential antioxidant agents. 相似文献
20.
Six new lanthanide complexes, with the formula [La(2,6-DMBA)3(5,5′-DM-2,2′-bipy)(H2O)]2 (1) and [Ln(2,6-DMBA)3(5,5′-DM-2,2′-bipy)]2 (Ln = Tb(2), Dy(3), Ho(4), Pr(5), Nd(6)) (2,6-DMBA = 2,6-dimethylbenzoate, 5,5′-DM-2,2′-bipy = 5,5′-dimethyl-2,2′-bipyridine) have been successfully synthesized and characterized. These title complexes have three different structural types. The structure of complex 1(type I) contains coordination water molecules, and the coordination number is 8. The coordination numbers of complexes 2–4 and 5–6 are 8 and 9, showing a distorted square antiprism geometry and distorted monocapped square anti-prismatic geometry, respectively. However they have the same general formula and they can be all assembled into the same 1D, 2D supramolecular structures via the C-H···O hydrogen bonding interactions, which is interesting in previous lanthanide complexes. The complexes were analyzed by TG-DSC/FTIR. In addition, the visible light luminescence experiments of Tb (III) complex was carried out, and the characteristic luminescence behavior of strong green color was shown. And the fluorescence lifetime and intrinsic quantum yield were calculated. The magnetic properties of complexes 2–4 were also studied, and the results showed that complex 3 and complexes 2, 4 have ferromagnetic interactions and antiferromagnetic interactions, respectively. 相似文献