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1.
Complexes of the general formulae Mn(2-bpy)2(CCl3COO)2, Co(2-bpy)2(CCl3COO)2·H2O and Ni(2-bpy)2(CCl3COO)2·2H2O (where: 2-bpy=2,2'-bipyridine) have been prepared and characterized by VIS and IR spectroscopy, conductivity and magnetic measurements.
The thermal properties of complexes in the solid state were studied under non-isothermal conditions in air atmosphere. During
heating the complexes decompose via different intermediate products to the oxides Mn3O4, CoO and NiO. A coupled TG-MS system was used to detection the principal volatile products of thermal decomposition and fragmentation
processes of obtained compounds. The principal volatile products of thermal decomposition of complexes are: H2O+, CO2
+, Cl2
+ and other.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
2.
New mixed-ligand complexes with empirical formulae M(4-bpy)L2·1.5H2O (M(II)=Mn, Co), Ni(4-bpy)2L2 and Cu(4-bpy) L2·H2O (where: 4-bpy=4,4'-bipyridine, L=CC L2HCOO-) have been isolated in pure state. The complexes have been characterized by elemental analysis, ir spectroscopy, conductivity
(in methanol, dimethylformamide and dimethylsulfoxide solutions) and magnetic and x-ray diffraction measurements. The Mn(II)
and Co(II) complexes are isostructural. The way of metal-ligand coordinations discussed. the ir spectra suggest that the carboxylate
groups are bonded with metal(II) in the same way (Ni, Cu) or in different way (Mn, Co). The solubility in water is in the
order of 19.40·10-3÷1.88·10-3ł mol dm-3ł. During heating the hydrate complexes lose all water in one step. The anhydrous complexes decompose to oxides via several
intermediate compounds. A coupled TG-MS system was used to analyse the principal volatile products of obtained complexes.
The principal volatile products of thermal decomposition of complexes in air are: H2O2
+, CO2
+, HCl+, Cl2
+, NO+ and other.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
3.
Czakis-Sulikowska D. Czylkowska A. Malinowska A. 《Journal of Thermal Analysis and Calorimetry》2001,65(2):505-513
The new mixed ligand complexes with formulae Co(4-bpy)2L2⋅2H2O (I), Cu(4-bpy)2L2⋅H2O (II) and Cd(4-bpy)L2⋅H2O (III) (4-bpy=4,4'-bipyridine, L=CCl3COO–) were prepared. Analysis of the IR spectra indicate that 4-bpy is coordinated with metal ions and carboxylates groups bond
as bidentate chelating ligands. The electronic spectra are in accordance with pseudo-octahedral environment around the central
metal ion in the Co(II) and Cu(II) complexes. The thermal decomposition of the synthesized complexes was studied in air. A
coupled TG-MS system was used to analyse the principal volatile thermal decomposition products of Co(II) and Cu(II) complexes.
Corresponding metal oxides were identified as a final product of pyrolysis with intermediate formation of metal chlorides.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
4.
Summary The new mixed-ligand complexes of d-electron metals (M(II)=Mn, Ni, Cu) with 2,2'-bipyridine (2-bpy) and mono- or dichloroacetates were prepared as crystalline solids. The general
formulae of the synthetized complexes are: Cu(2-bpy)2(CClH2COO)2·2H2O, Mn(2-bpy)2(CCl2HCOO)2, M(2-bpy)2(CCl2HCOO)2·2H2O (M(II)=Ni, Cu). The compounds were characterized by chemical analysis, IR and VIS spectroscopy. Their magnetic, molar conductivity
and thermal properties also were studied. During heating in air complexes decompose via different intermediate products to
metal oxides. A coupled TG-MS system was used to analyse the principal volatile thermal decomposition (or fragmentation) products
of 2,2'-bipyridine-chloroacetato complexes. 相似文献
5.
D. Czakis-Sulikowska J. Radwańnska-Doczekalska M. Markiewicz M. Pietrzak 《Journal of Thermal Analysis and Calorimetry》2008,93(3):789-794
New mixed ligand complexes of the following stoichiometric formulae: M(2-bpy)2(RCOO)2·nH2O, M(4-bpy)(RCOO)2·H2O and M(2,4’-bpy)2(RCOO)2·H2O (where M(II)=Zn, Cd; 2-bpy=2,2’-bipyridine, 4-bpy=4,4′-bipyridine, 2,4′-bpy=2,4′-bipyridine; R=C2H5; n=2 or 4) were prepared in pure solid-state. These complexes were characterized by chemical and elemental analysis, IR and
conductivity studies.
Thermal behaviour of compounds was studied by means of DTA, DTG, TG techniques under static conditions in air. The final products
of pyrolysis of Cd(II) and Zn(II) compounds were metal oxides MO. A coupled TG/MS system was used to analyse of principal
volatile products of thermal decomposition or fragmentation of Zn(4-bpy)(RCOO)2·H2O under dynamic air and argon atmosphere.
The principal species correspond to: C+, CH+, CH3
+, C2H2
+, HCN+, C2H5
+ or CHO+, CH2O+ or NO+, CO2
+, 13C16O2
+ and 12C16O18O+ and others; additionally CO+ in argon atmosphere. 相似文献
6.
D. Czakis-Sulikowska J. Radwańska-Doczekalska A. Czylkowska M. Markiewicz A. Broniarczyk 《Journal of Thermal Analysis and Calorimetry》2006,86(2):327-335
New mixed-ligand complexes with empirical
formulae: Mn(2-bpy)1.5L2·2H2O,
M(2-bpy)2L2·3H2O
(M(II)=Co, Cu), Ni(2-bpy)3L2·4H2O
and M(2,4’-bpy)2L2·2H2O
(where 2-bpy=2,2’-bipyridine, 2,4’-bpy=2,4’-bipyridine; L=HCOO– ) have been
obtained in pure solid-state. The complexes were characterized by chemical
and elemental analysis, IR and VIS spectroscopy, conductivity (in methanol
and dimethylsulfoxide). The way of metal-ligand coordination discussed. The
formate and 2,4’-bpy act as monodentate ligands and 2-bpy as chelate
ligand. The new complexes with ligand isomerism were identified. During heating
the complexes lose water molecules in one or two steps. Thermal decomposition
after dehydration is multistage and yields corresponding metal oxides as final
products. A coupled TG-MS system was used to analysis principal volatile thermal
decomposition (or fragmentation) products of Ni(2,4’-bpy)2(HCOO)2·2H2O under dynamic air or argon atmosphere. 相似文献
7.
Czakis-Sulikowska D. Radwańska-Doczekalska J. Czylkowska A. Gołuchowska J. 《Journal of Thermal Analysis and Calorimetry》2004,78(2):501-511
The new mixed ligand complexes with formulae M(4-bpy)(C2H5COO)2·2H2O (where M(II)=Mn, Co, Ni; 4,4'-bpy or 4-bpy=4,4'-bipyridine) and Cu(4-bpy)0.5(C2H5COO)2·H2O were prepared and characterized by VIS (for solid compounds of Co(II), Ni(II), Cu(II) in Nujol), IR spectroscopy, X-ray
powder diffraction and molar conductance in MeOH, DMF or DMSO. Thermal behaviour of complexes was studied under static conditions
in air atmosphere. Corresponding metal oxides were identified as final products of pyrolysis. A coupled TG-MS system was used
to analysis of principal volatile thermal decomposition and fragmentation products of isolated complexes under dynamic air
and argon atmosphere. The principal species correspond to: C+, OH+, H2O+, NO+, CO2
+ and other; additionally CO+ in argon atmosphere.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
8.
Czakis-Sulikowska D. Czylkowska A. Radwańska-Doczekalska J. 《Journal of Thermal Analysis and Calorimetry》2000,63(2):387-395
The complexes with the empirical formula M(4-bipy)(ClCH2COO)2 ×nH2O (where: 4-bipy=4,4'-bipyridine, L=ClCH2 COO–, M (II)=Mn, Co, Ni, Cu) were prepared and characterized via the IR and electronic (VIS) spectra and conductivity measurements.
Thermal decomposition of these compounds was studied. During heating in air dehydration processes occur. The anhydrous compounds
decompose at high temperature to oxides. The principal volatile mass fragments correspond to: H2O, CO2, CH3Cl, HCl, Cl2 and other.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
9.
Four new mixed ligand complexes were prepared by the reaction of title metal dichloroacetates and 2,4'-bipyridine. The general
formulae of synthesized compounds are M(2,4'-bpy)2(CCl2HCOO)2·nH2O (where M(II)=Mn, Co, Ni, Cu; 2,4'-bpy=2,4'-bipyridine, n=2 or 4). The complexes have been isolated from aqueous media and characterized by chemical analysis, molar conductance (in
MeOH, DMSO and DMF), magnetic, IR and VIS spectral studies. The nature of metal(II)-ligand coordination is discussed. The
thermal behaviour of obtained complexes was studied by thermal analysis and TG-MS techniques in air. IR, X-ray powder diffraction
and thermoanalytical data were used for the determination of solid intermediate products of the thermal decomposition. The
principal volatile products of thermal decomposition of complexes were proved by mass spectroscopy: H2O+, CO+
2, HCl+
2, Cl+
2, NO+ and other.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
10.
The complexes of 4-chloro-2-methoxybenzoic acid anion with Mn2+,
Co2+, Ni2+, Cu2+
and Zn2+ were obtained as polycrystalline solids
with general formula M(C8H6ClO3)2·nH2O and colours typical for M(II) ions (Mn – slightly pink, Co –
pink, Ni – slightly green, Cu – turquoise and Zn – white).
The results of elemental, thermal and spectral analyses suggest that compounds
of Mn(II), Cu(II) and Zn(II) are tetrahydrates whereas those of Co(II) and
Ni(II) are pentahydrates. The carboxylate groups in these complexes are monodentate.
The hydrates of 4-chloro-2-methoxybenzoates of Mn(II), Co(II), Ni(II), Cu(II)
and Zn(II) heated in air to 1273 K are dehydrated in one step in the range
of 323–411 K and form anhydrous salts which next in the range of 433–1212
K are decomposed to the following oxides: Mn3O4,
CoO, NiO and ZnO. The final products of decomposition of Cu(II) complex are
CuO and Cu. The solubility value in water at 293 K for all complexes is in
the order of 10–3 mol dm–3.
The plots of χM
vs.
temperature of 4-chloro-2-methoxybenzoates of Mn(II), Co(II), Ni(II) and Cu(II)
follow the Curie–Weiss law. The magnetic moment values of Mn2+,
Co2+, Ni2+ and Cu2+
ions in these complexes were determined in the range of 76−303 K and
they change from: 5.88–6.04 μB for Mn(C8H6ClO3)2·4H2O, 3.96–4.75
μB for Co(C8H6ClO3)2·5H2O, 2.32–3.02 μB for Ni(C8H6ClO3)2·5H2O and 1.77–1.94
μB for Cu(C8H6ClO3)2·4H2O. 相似文献
11.
The reaction products of Cu(II) 2-chlorobenzoate and the imidazole (1), and of Cu(II) 2,6-dichlorobenzoate and the imidazole
(2) formulated as CuL’2⋅2imd⋅2H2O and CuL”2⋅2imd⋅2H2O (L’=C7H4ClO2
−, L”=C7H3Cl2O2
−, imd=imidazole), were prepared and characterized by means of spectroscopic measurements and thermochemical properties. The blue
(1) and green (2) complexes were obtained as solids with a 1:2:2 molar ratio of metal to carboxylate ligand to imidazole.
When heated at a heating rate of 10 K min−1 the hydrated complexes, (1) and (2), lose some of the crystallization water molecules and then decompose to gaseous products.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
12.
Czakis-Sulikowska D. Malinowska A. Łuczak A. 《Journal of Thermal Analysis and Calorimetry》2004,78(2):461-471
Two lactates and four new mixed ligand complexes with formulae Co(lact)2·2H2O, Ni(lact)2·3H2O, Co(4-bpy)(lact)2, Co(2,4'-bpy)2(lact)2, Ni(4-bpy)(lact)2·2H2O and Ni(2,4'-bpy)2(lact)2 (where 4-bpy=4,4'-bipyridine, 2,4'-bpy=2,4'-bipyridine, lact=CH3CH(OH)COO-) were isolated and investigated. The thermal behaviour of compounds was studied by thermal analysis (TG, DTG, DTA). In the
case of hydrated complexes thermal decomposition starts with the release of water molecules. The compounds decompose at high
temperature to metal(II) oxides in air. A coupled TG-MS system was used to analyse the principal volatile products of thermolysis
and fragmentation processes of obtained complexes.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
13.
Conditions for the preparation of Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II)3,3-dimethylglutarates were investigated
and their quantitative composition, solubility in water at 293 K and magnetic moments were determined. IR spectra and powder
diffraction patterns of the complexes prepared with general formula MC7H10O4⋅nH2O (n=0−2) were recorded and their thermal decomposition in air were studied. During heating the hydrated complexes of Mn(II),Co(II),
Ni(II) and Cu(II) are dehydrated in one step and next all the anhydrous complexes decompose to oxides directly (Mn, Co, Zn)
or with intermediate formation free metal (Ni,Cu) or oxocarbonates (Cd). The carboxylate groups in the complexes studied are
bidentate. The magnetic moments for the paramagnetic complexes of Mn(II), Co(II), Ni(II) and Cu(II)attain values 5.62, 5.25,
2.91 and 1.41 M.B., respectively.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
14.
New Y(III) and La(III) complexes with 4-bpy (4,4??-bipyridine) and trichloro- or dibromoacetates with the formulae: Y(4-bpy)2(CCl3COO)3·H2O I, La(4-bpy)1.5(CCl3COO)3·2H2O II, Y(4-bpy)1.5(CHBr2COO)3·3H2O III, and La(4-bpy)(CHBr2COO)3·H2O IV were prepared and characterized by chemical, elemental analysis, and IR spectroscopy. Conductivity studies (in methanol, dimethyloformamide, and dimethylsulfoxide) were also described. They are small, crystalline substances. The way of metal?Cligand coordination was discussed. The thermal properties of complexes in the solid state were studied by TG-DTG techniques under dynamic flowing air atmosphere. TG-FTIR system was used to analyze principal volatile thermal decomposition and fragmentation products evolved during pyrolysis in dynamic flowing argon atmosphere for La(III) compounds. 相似文献
15.
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
16.
A series of new manganese(I) and ruthenium(II) monometallic and bimetallic complexes made of 2,2′-bipyridine and 1,10-phenanthroline ligands, [Mn(CO)3(NN)(4,4′-bpy)]+, [{(CO)3(NN)Mn}2(4,4′-bpy)]2+ and [(CO)3(NN)Mn(4,4′-bpy)Ru(NN)2Cl]2+ (NN = 2,2′-bipyridine, 1,10-phenanthroline; 4,4′-bpy = 4,4′-bipyridine) are synthesized and characterized, in addition to already known ruthenium(II) complexes [Ru(NN)2Cl(4,4′-bpy)]+ and [Cl(NN)2Ru(4,4′-bpy)Ru(NN)2Cl]2+. The electrochemical properties show that there is a weak interaction between two metal centers in Mn–Ru heterobimetallic complexes. The photophysical behavior of all the complexes is studied. The Mn(I) monometallic and homobimetallic complexes have no detectable emission. In Mn–Ru heterobimetallic complexes, the attachment of Mn(I) with Ru(II) provides interesting photophysical properties. 相似文献
17.
Erika Szunyogová Dagmar Mudroňová Katarína Györyová Radomíra Nemcová Jana Kovářová Lenka Piknová-Findoráková 《Journal of Thermal Analysis and Calorimetry》2007,88(2):355-361
Spectroscopic (IR), thermoanalytical (TG/DTG, DTA) and biological methods
were applied to investigate physicochemical and biological properties of seven
zinc(II) complex compounds of the following formula Zn(HCOO)2·2H2O
(I), Zn(HCOO)2·tph (II), Zn(CH3COO)2·2H2O (III), Zn(CH3COO)2·tph
(IV), Zn(CH3COO)2·2phen
(V), Zn(CH3CH2COO)2·2H2O
(VI), Zn(CH3CH2CH2COO)2·2H2O (VII), where tph=theophylline, phen=phenazone. The formation of various
intermediates during thermal decomposition suggests the dependence on the
length of aliphatic carboxylic chain and type of N-donor ligand (tph, phen).
The final product of the thermal decomposition was ZnO. The antimicrobial
activity of these complexes were tested against G+
and G– bacteria. Strong inhibitive effect
was observed towards E. coli, salmonellae
and Staph. aureus. 相似文献
18.
S. C. Mojumdar 《Journal of Thermal Analysis and Calorimetry》2001,64(2):629-636
Thermogravimetry (TG), differential thermal analysis (DTA) and other analytical methods have been applied to the investigation
of the thermal behaviour and structure of the complexes Mg(pc)(na)3⋅3H2O (I), Mg(pc)(py)2⋅2H2O (II),Mg(pc)(pic)2⋅2H2O (III) and Mg(pc)(caf)2⋅4H2O (IV), where pc=2,6- pyridinedicarboxylate, na=nicotinamide,py=pyridine, pic=γ-picoline and caf=caffeine. The thermal decomposition of these compounds is multi-stage processes. The chemical composition of the complexes,
the solid intermediates and the resultant products of thermolysis have been identified by means of elemental analysis and
complexometric titration. Schemes of destruction of these complexes are suggested. Heating of these compounds first resulted
in a release of water molecules. In complexes I, II and IV the loss of the molecular ligands (na, py and caf) occur (on the
TG curves) in one step (-2na, -2py and -2caf) and in complex III in two steps (-pic, -pic). The final product of the thermal
decomposition was MgO. The thermalstability of the complexes can be ordered in the sequence: IV<I<III<II. Nicotinamide, pyridine,
γ-picoline and caffeine were co-ordinated to Mg(II) through the N atom of the respective heterocyclic ring. IR data suggested
a unidentate co-ordination of carboxylates to Mg(II) in complexes I–IV.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
19.
Zong-Hui Jiang Chao-Li Deng Dai-Zheng Liao Shi-Ping Yan Geng-Lin Wang 《Transition Metal Chemistry》1993,18(3):345-347
Summary Four new trinuclear copper(II) complexes, [Cu(phen)-(NBzIm)] (ClO4) (1), [Cu(bpy)(NBzIm)](ClO4) (2), [Cu-(Me2-bpy)(NBzIm)](Ac)·1/2H2O (3) and [Cu(Me2-bpy)-(Im)](ClO4)·1/2H2O (4) (phen = 1, 10-phenanthroline, bpy = 2,2-bipyridine, NBzIm = 6-nitrobenzimidazolate ion, Im=imidazolate ion) have been prepared and characterized by variable temperature magnetic susceptibility measurements. A weak antiferromagnetic spin exchange interaction operates between copper(II) ions, exchange integrals evaluated as J =-23.82 cm-1 for (1); and J=-21.91 cm-1 for (2). 相似文献
20.
Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) 3-methylglutarates were prepared as solids with general formula MC6 H8 O4 ×n H2 O, where n =0–8. Their solubilities in water at 293 K were determined (7.0×10−2 −4.2×10−3 mol dm−3 ). The IR spectra were recorded and thermal decomposition in air was investigated. The IR spectra suggest that the carboxylate
groups are mono- or bidentate. During heating the hydrated complexes lose some water molecules in one (Mn, Co, Ni, Cu) or
two steps (Cd) and then mono- (Cu) or dihydrates (Mn, Co, Ni) decompose to oxides directly (Mn, Cu, Co) or with intermediate
formation of free metals (Co, Ni). Anhydrous Zn(II) complex decomposes directly to the oxide ZnO.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献