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1.
The thermal properties and gas Chromatographie behaviour of manganese(II) and manganese(III) trifluoroacetylacetonates (TFA) were investigated by using the ligand vapour technique. The two chelates, Mn(TFA); and Mn(TFA)3, can be quantitatively eluted on a mixed-liquid phase (1.9% OV-17 ÷ 0.1% PEG-20M) at column temperatures above 210°C and 130–150°C, respectively; Mn(TFA)3 is completely converted to Mn(TFA)2 by thermal dissociation at column temperatures above 180°C and completely eluted as Mn(TFA)2 above 210°C. The chelates can be determined separately within errors of about 1% after a preliminary extraction. 相似文献
2.
TG, DTA and other analytical methods were applied to investigate the thermal behaviour and structures of the compounds Mg(ClAc)2(Py)2·2H2O (I), Mg(Cl2Ac)2(Py)·H2O (II), Mg(Cl3Ac)2(Py)·6H2O (III) and Mg(SCN)2(Py)3·2H2O (IV), where ClAc=ClCH2COO−, Cl2Ac=Cl2CHCOO−, Cl3Ac=Cl3CCOO− and Py=Pyridine. The compositions of the complexes and the solid-state intermediates and products of thermolysis were identified
by means of elemental analysis. Possible schemes of destruction of the complexes are suggested. The final products of the
thermal decompositions were MgO (I–III) and MgS (IV). The IR data suggest unidentate coordination of the carboxylate ions
to Mg(II) in complexes I–III. Py is coordinated to the Mg(II) through the nitrogen atom of its heterocyclic ring.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
3.
V. V. Ramakrishna S. K. Patil L. Krishna Reddy A. S. Reddy 《Journal of Radioanalytical and Nuclear Chemistry》1978,47(1-2):57-76
Extraction of Tm(III), from thiocyanate media, by different sulfoxides (R2SO) has revealed that the extractable complex is Tm(SCN)3·4 R2SO. When mixtures of DPSO and HTTA are used for the extraction of Tm(III) from thiocyanate or perchlorate media, synergistic
enhancement of the extraction of Tm(III) results. The complexes responsible for the enhanced extraction are Tm(TTA)3·DPSO and Tm(TTA)3·2 DPSO when perchlorate media were employed for the extraction and Tm(SCN)(TTA)2·2 DPSO and Tm(SCN)2(TTA)·3 DPSO, in addition to the above two when a thiocyanate medium was employed for the extraction. Values of equilibrium
constants for some equilibria encountered in the extraction of Am(III) and Tm(III) by mixtures of DPSO and HTTA are given. 相似文献
4.
Yi‐Wen Chen Hai‐Xia Wei Xiu‐Guang Wang Prof. Dr. Dong‐Zhao Gao Ya‐Qiu Sun Guo‐Ying Zhang Yan‐Yan Xu 《无机化学与普通化学杂志》2012,638(9):1328-1334
Three new one‐dimensional (1D) chain metal–nitroxide complexes {[Cu(NIT4Py)2(suc)(H2O)] · 3H2O}n ( 1 ), {[Cd(NIT4Py)2(suc)(H2O)] · [Cd(NIT4Py)2(suc)(H2O)2] · 3H2O}n ( 2 ), and {[Zn(NIT4Py)(glu)(H2O)] · H2O}n ( 3 ) [NIT4Py = 2‐(4′‐pyridyl)‐4, 4, 5, 5‐tetramethylimidazoline‐1‐oxyl‐3‐oxide, suc = succinate anion and glu = glutarate anion] were synthesized and structurally characterized. Single‐crystal X‐ray analyses indicate that the three complexes crystallize in neutral 1D chains in which the metal‐nitroxide units are linked by flexible dicarboxylate anions. The succinate anions only adopt trans configuration in complexes 1 and 2 , whereas the glutarate anion has gauche/anti conformation in complex 3 . Magnetic measurements show that complex 1 exhibits weak antiferromagnetic interactions between the copper ions and the nitroxides. 相似文献
5.
The IR. spectra of α-thenoyl-trifluoroacetone (HTTA) and seventeen of its chelates with metal(II) and -(III) ions of the first transition series have been determined. Three series of complexes are represented: the anhydrous metal(II) species, [M(TTA)2]n (M ? Ca, Mn, Co, Ni, Cu, Zn); metal(II) dihydrates, [M(TTA)2(H2O)2] (M ? Mn, Fe, Co, Ni, Zn); and the metal(III) chelates, [M(TTA)3] (M ? Sc, V, Cr, Mn, Fe, Ga). For each metal(II) complex, the spectra of the anhydrous and hydrated compounds are practically identical, suggesting that the anhydrous complexes have the polynuclear octahedral structure established for the corresponding acetylacetonates. Magnetic moment determinations reveal that complexes of the 3d4?3d7 ions all have spin-free configuration. Several vibrational bands with frequencies < 700 cm?1 are found to exhibit a frequency variation with d-orbital population which is consistent with the order of crystal field stabilization energies and hence with their assignment as coupled metal-oxygen stretching modes. Unique features of the spectra of [Cu(TTA)2] and [Mn(TTA)3] are ascribed to structural differences arising from Jahn-Teller distortion. Tentative assignments for the majority of the ligand vibrations are given. 相似文献
6.
Dong-Zhao Gao Dai-Zheng Liao Zong-Hui Jiang Shi-Ping Yan 《Transition Metal Chemistry》2008,33(1):107-112
Two hetero-spin metal–radical complexes [Cu(NIT2Py)2Cl] · ClO4 · H2O (
1
) and [Co(NIT2Py)2(H2O)(CH3OH)] · (ClO4)2
(
2
) (NIT2Py = 2-(2′-pyridinyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide), were synthesized and characterized structurally
and magnetically. The two complexes crystallize in mononuclear structures where two radical ligands coordinate to the metal
ion through the nitroxide oxygen atoms directly via the bidentate chelating mode. The magnetic measurements show that two
complexes exhibit strong antiferromagnetic interactions between the metal ions and the nitroxide radicals. 相似文献
7.
Studies on the fractional sublimation of various metal β-diketone chelates have been extended to include the chelates of thenoyltrifluoroacetone (TTA). Many of the common metal chelates were found to be stable, to sublime readily, and to form well-defined zones in the vacuum fractional sublimator. Of the 17 chelates reported only those of manganese (II) and iron(II) were not volatile. The chelates of UO2(II), Zr(IV), Pb(II), and Cr(III) partially decomposed during sublimation and their recovery was incomplete. The recovery of the sublimed chelates of Ni(II), Mg(II), Al(III), Pd(II), Co(II), Cu(II). Fe(III), Tl(III), Zn(II) and Be(II) ranged from 87 to 100%, with most recoveries being quantitative. The sublimation recrystallization zone temperatures of the various chelates are compared to those of the metal acetylacetonates and the benzoyltrifluoroacetonates; in general, the metal chelates of TTA sublime more readily than those of benzoyltrifluoroacetone but are potentially less useful for fractional sublimation separations than the corresponding metal acetylacetonates. Even so, a quantitative separation of iron(III) from Ni(II), Al(III), Mn(II), and Fe(II) is proposed that depends upon the fractional sublimation of the TTA chelates. 相似文献
8.
Fluorescence microscopy observation of self-organized microstructure formed by a rare earth compound
The morphologies of monolayers containing Eu(TTA)3Phen (TTA=thenoyltrifluoroace-tone, Phen = 1, 10-phenanthroline) were studied at the air/liquid interface on different subphases by fluorescence microscopy (FM). The composite subphase was the basic premise for the stable existence of the rare earth compound at air/liquid interface. The process that rare earth compound phase changes from liquid expanded state to liquid condensed state corresponded to a plateau in the π-A isotherm. In the pure Eu(TTA)3Phen monolayer, rod domains of Eu(TTA)3Phen formed and packed with no order. In the mixed monolayers with stearic acid (SA), phase transition of SA occurred first and formed domains with an electric gradient field, which induced the rare earth compound to form luminescent ring domains. Influence of intermolecular interaction on the self-organized microstructure was revealed. 相似文献
9.
Yuan‐Yuan Gao Yue Ma Ya‐Li Wang Yu‐Zhang Tong Ming‐Fang Yang Qing‐Lun Wang Li‐Cun Li Dai‐Zheng Liao 《无机化学与普通化学杂志》2013,639(6):1015-1020
Two heterospin complexes [Cu(NIT3Py)(cda)H2O] · H2O ( 1 ) and [Cu(NIT2Py)(cda)H2O] · H2O · CH3OH ( 2 ) with CuII ions and pyridyl‐substituted nitronyl nitroxide radicals (NITxPy = 2‐(x′‐pyridyl)‐4,4,5,5‐tetramethyl‐imidazoline‐1‐oxyl‐3‐oxide, x = 3, 2; H2cda = 4‐hydroxy‐pyridine‐2,6‐dicarboxylic acid) were synthesized and characterized structurally and magnetically. The single crystal structures show that the two complexes are both two‐spin complexes, in which the different radicals make the two complexes have different hydrogen bonding interactions to form 2D and 1D supramolecular network for complexes 1 and 2 , respectively. The magnetic measurements indicate that complexes 1 and 2 both exhibit antiferromagnetic interactions between CuII and radicals. 相似文献
10.
I. V. Kalinovskaya I. A. Tkachenko A. G. Mirochnik V. E. Karasev V. Ya. Kavun 《Russian Journal of Physical Chemistry A, Focus on Chemistry》2010,84(8):1452-1454
The luminescence and magnetic properties of mixed-ligand europium trifluoroacetates with nitrogen- and phosphorus-containing
neutral ligands [Eu(TFA)3 · 3H2O]2 and Eu(TFA)3 · 2D · nH2O were studied (here TFA is the trifluoroacetic acid anion, and D is Phen (1,10-phenanthroline), n = 1; DMF (dimethylformamide), n = 1; or TPPO (triphenylphosphine oxide), n = 3). The molar magnetic susceptibility increased in the series of complex compounds Eu(TFA)3 · 2Phen · H2O < [Eu(TFA)3 · 3H2O]2 < Eu(TFA)3 · 2DMF · H2O < Eu(TFA)3 · 2TPPO · 3H2O. Correlations were found between the luminescent and magnetic characteristics of the complex compounds. 相似文献
11.
《Journal of Coordination Chemistry》2012,65(10):913-921
The influence of amide ligands on the photoluminescent behavior of tris(thenoyltrifluoroacetonate)- europium(III) in the solid state is reported. Elemental analysis showed that these compounds have the following formulas [Eu(TTA)3·(ANL)2] and [Eu(TTA)3·PZA], where ANL = acetanilide and PZA = pyrazinamide. The photoluminescence spectra of the complexes recorded in the range 420-720 nm at 77 K show narrow bands arising from the 5D0 → 7F J transitions (where J = 0-4), under excitation at 394 nm. Based on the emission spectra and luminescence decay curves the intensity parameters (Ωλ), lifetime (τ) and emission quantum efficiency (η) were determined. The Ω2 values indicate that the Eu3+ion in these complexes is in a highly polarizable chemical environment. The higher value of η (60%) obtained for the complex with the ANL ligand, in comparison with the complex with the PZA ligand (30%), indicates a more efficient deactivation of the Eu3+ion in the [Eu(TTA)3·PZA] complex. 相似文献
12.
G. -C. Xu L. Zhang L. Liu G. -F. Liu D. -Z. Jia 《Journal of Thermal Analysis and Calorimetry》2007,89(2):547-553
Thermal behaviors of two mixed-ligand complexes, [Ni(PMPP-SAL)(Py)3] and [Cu(PMPP-SAL)Py]·MeOH, (PMPP-SAL=1-phenyl-3-methyl-4-(salicylidene hydrazide)-propenylidene-pyrazolone-5, Py=pyridine),
were studied by TG-DTG-DTA in dynamic air atmosphere. The complexes show the loss of pyridine molecule is followed by the
decomposition of the PMPP-SAL anion and give respective metal oxides as residues. Meanwhile, the Ozawa-Flynn-Wall model-free
analyses and multivariate non-linear regressions were applied to perform single and overall steps optimization. Kinetic parameters
were given and the most probable mechanism functions were suggested in this study. 相似文献
13.
Yi‐Wen Chen Hong‐Dao Li Dong‐Zhao Gao Xiu‐Guang Wang Zhong‐Yi Liu Ya‐Qiu Sun Guo‐Ying Zhang Yan‐Yan Xu 《无机化学与普通化学杂志》2013,639(5):746-753
Three new metal–nitroxide complexes {[Ni(NIT4Py)2(obb)(H2O)2] · 1.5H2O}n ( 1 ), {[Co(NIT4Py)2(obb)(H2O)2] · 2H2O}n ( 2 ), and [Co(IM4Py)2(obb)2(H2O)2][Co(IM4Py)2(H2O)4] · 10H2O ( 3 ) with the V‐shaped 4,4′‐oxybis(benzoate) [NIT4Py = 2‐(4′‐pyridyl)‐4,4,5,5‐tetramethylimidazoline‐1‐oxyl‐3‐oxide, IM4Py = 2‐(4′‐pyridyl)‐4,4,5,5‐tetramethylimidazoline‐1‐oxide, and obb = 4, 4′‐oxybis(benzoate) anion] were synthesized and structurally characterized. Single‐crystal X‐ray analyses indicate that complexes 1 and 2 crystallize in neutral one‐dimensional (1D) zigzag chains, in which the nitroxide–metal–nitroxide units are linked by the V‐shaped 4,4′‐oxybis(benzoate) anions, whereas complex 3 consists of isolated mononuclear [Co(IM4Py)2(obb)2(H2O)2]2– anions and [Co(IM4Py)2(H2O)4]2+ ions. Magnetic measurements show that complexes 1 and 2 both exhibit weak antiferromagnetic interactions between the metal ions and the nitroxides. 相似文献
14.
15.
D. M. Petrovic A. F. Petrovic V. M. Leovac S. R. Lukic 《Journal of Thermal Analysis and Calorimetry》1994,41(5):1165-1170
The thermal decomposition of copper(II) complexes with salicylaldehyde S-methylthiosemicarbazone of general formula Cu(HL)X·nH2O (X=Py+NO3, NCS, 0.5SO4) and [Cu(L)NH3]·H2O was investigated in air atmosphere in the interval from room temperature to 1000°C. Decomposition of the complexes occurred in several successive endothermic and exothermic processes, and the residue was in all cases CuO. 相似文献
16.
I. V. Kalinovskaya V. V. Kon’shin V. E. Karasev E. N. Chernykh 《Russian Journal of Inorganic Chemistry》2011,56(2):273-275
The ligand substitution in Eu(AA)3 · Phen-CDCl3-TFA systems, where AA is acetylacetone, Phen is 1,10-phenanthroline, and TFA is trifluoroacetic acid was studied at various
molar ratios (m) of competing ligands (m = TFA/AA) using NMR (1H, 19F) and luminescence spectroscopy. The formation of mixed Eu(AA)2(TFA) · Phen and Eu(AA)(TFA)2 · Phen complexes in the resultant solutions was attested. The luminescence spectra were studied. The competitive capacity
of TFA was ascertained to be higher than that of AA. Depending on the m value, the substitution of acido ligands was shown to occur successively according equations Eu(AA)3 · Phen + (TFA)
n
= Eu(AA)3 − n
(TFA)
n
· Phen + (AA)
n
(n = 1, 2, 3). 相似文献
17.
Pyridinium Chlorometallates of Lanthanoid Elements. Crystal Structures of [HPy]2[LnCl5(Py)] mit Ln = Eu, Er, Yb und von [H(Py)2][YbCl4(Py)2] · Py The pyridinium chlorometallates [HPy]2[LnCl5(Py)] with Ln = Eu, Er and Yb, as well as [H(Py)2][YbCl4(Py)2]·Py have been obtained by the reaction of diacetone alcohol with solutions of the corresponding metal trichlorides in pyridine at 100 °C. According to the crystal structure determinations the anions [LnCl5(Py)]2— are linked by bifurcated Cl···H···Cl bridges with the protons of the [HPy]+ cations forming chains along [001]. The anions of [H(Py)2][YbCl4(Py)2]·Py form discrete octahedrons with trans‐positions of the pyridine ligands. [HPy]2[EuCl5(Py)] ( 1a ): Space group Pnma, Z = 4, lattice dimensions at —80 °C: a = 1874.4(2), b = 1490.2(2), c = 741.5(1) pm, R1 = 0.0466. [HPy]2[ErCl5(Py)] ( 1b ): Space group Pnma, Z = 4, lattice dimensions at —80 °C: a = 1864.3(1), b = 1480.7(2), c = 739.7(1) pm, R1 = 0.0314. [HPy]2[YbCl5(Py)] ( 1c ): Space group Pnma, Z = 4, lattice dimensions at —80 °C: a = 1858.9(2), b = 1479.0(1), c = 736.8(1) pm, R1 = 0.0306. [H(Py)2][YbCl4(Py)2]·Py ( 2 ·Py): Space group Ia, Z = 4, lattice dimensions at —80 °C: a = 1865.5(1), b = 827.5(1), c = 1873.4(1) pm, ß = 103.97(1)°, R1 = 0.0258. 相似文献
18.
H. F. Aly M. M. El-Dessouky M. Raieh S. Mohamed 《Journal of Radioanalytical and Nuclear Chemistry》1978,43(1):7-14
Synergic extraction of trivalent iron and cobalt with thenoyltriflouroacetone (HTTA) and the synergic bases (B) benzylamine
(BA), dibenzylamine (DBA) and tribenzylamine (TBA) was studied. The extracted adducts proved to have the general formula M(TTA)3·B for all the amines investigated. The formation constants of the mixed-ligand complexes decrease in the order DBA>TBA>BA.
While equilibrium constant β3,1 for the Co(TTA)3·DBA complex is higher than the corresponding iron adduct, β3,1 for the iron adducts with BA and TBA are higher than those for cobalt. 相似文献
19.
Lu Zhenrong Ding Yuanchen Xu Ying Chen Shuhua Yu Yunpeng 《Journal of Thermal Analysis and Calorimetry》2003,73(1):333-340
The thermal behaviors of [1,1,1-trifluro-3-(2-thenoyl)-acetonato]copper(II) Cu(TTA)2 and its adducts with pyridine Cu(TTA)2(Py)2, 2,2'-bipyridine Cu(TTA)2(Bpy), quinoline Cu(TTA)2(Ql)2, and dimethyl sulfoxide Cu(TTA)2(DMS) in a nitrogen atmosphere were studied under the non-isothermal conditions by simultaneous TG-DTG-DSC technique. The
results showed that the evolution of the solvent molecules generally proceeded before the release of TTA in different ways
according to their structures. The Cu(TTA)2(Bpy) exhibited a unique decomposition pattern due to its distinctive structure. The dependences of activation energy on extent
of reaction for all the stage of each compound were determined by using an isoconversional method, Flynn-Wall-Ozawa equation,
which show E values varied with reaction progress, indicating the complexity of these decomposition reactions. In addition,
the values of activation energy E for TTA molecules evolution are generally higher than that for the solvent molecules release.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
20.
S. K. Patil V. V. Ramakrishna M. S. Sajun R. Thiagarajan 《Journal of Radioanalytical and Nuclear Chemistry》1979,54(1-2):159-169
Synergistic extraction of Th(IV) from perchlorate medium by mixtures of HTTA and TBP was studied. These studies include the
effect of the ionic strength, temperature and the diluents on the extraction. Ionic strength was found to influence the extraction
of Th(TTA)4 and Th(TTA)4·TBP whereas the adduct formation in the organic phase was almost unaffected. Increase of temperature resulted in a decrease
of the extraction of Th(IV). The stability of the adduct was found to decrease in the order, cyclohexane > benzene > chloroform. 相似文献