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1.
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
2.
Czakis-Sulikowska D. Kałużna-Czaplińska J. 《Journal of Thermal Analysis and Calorimetry》2000,62(3):821-830
The compounds ML2(NCS)2, (M(II)=Mn, Co), FeL2(NCS)2×2H2O, NiL3 NCS)2×3H2O (L=2,2'-bipyridine, 2-bipy) MX2(NCS)2×2H2O (M(II)=Mn, Fe; X=4,4'-bipyridine, 4-bipy) have been prepared and their IR spectra and molar conductivity studied. The thermal decomposition
of the complexes was studied under non-isothermal conditions in air. During heating the hydrated complexes lose crystallization
water molecules in one or two steps and then decompose via different intermediate compounds to the oxides Mn3O4, Fe2O3, CoO, NiO.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
3.
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
4.
Czakis-Sulikowska D. Czylkowska A. Malinowska A. 《Journal of Thermal Analysis and Calorimetry》2002,67(3):667-678
New mixed-ligand complexes of general formulae Mn(4-bpy)(CCl3COO)2⋅H2O, Ni(4-bpy)2(CCl3COO)2⋅2H2O and Zn(4-bpy)2(CCl3COO)2⋅2H2O (where 4-bpy=4,4’-bipyridine) were obtained and characterized. The IR spectra, conductivity measurements and other physical properties
of these compounds were discussed. The central atoms M(II) form coordinate bonds with title ligands. The thermal behaviour
of the synthesized complexes was studied in air. During heating the complexes decompose via different intermediate products to Mn3O4, NiO and ZnO; partial volatilization of ZnCl2was observed. A coupled TG-MS system was used to the analysis of the principal volatile thermal decomposition products of
Mn(II) and Ni(II) complexes. The principal volatile mass fragments correspond to: H2O+, OH+, CO+
2, HCl+, Cl+
2, CCl+ and other.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
5.
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
6.
D. Czakis-Sulikowska J. Radwańska-Doczekalska M. Markiewicz 《Journal of Thermal Analysis and Calorimetry》2000,60(1):145-151
The mixed 2,4'-bipyridine-oxalato complexes of the formulae M(2,4'-bipy)2 C2 O4 2H2 O (M (II)=Mn, Co, Ni, Cu; 2,4'-bipyridine=2,4'-bipy or L ; C2 O2–
4 =ox) have been prepared and characterized. IR data show that the 2,4'-bipy coordinated with these metals(II) via the least
hindered (4')N atom; that oxalate group acts as bidentate chelating ligand. Room temperature magnetic moments are normal for
the orbital singlet states. The thermal decomposition of these complexes was investigated by TG, DTA and DTG in air. The endothermic
or exothermic character of the decomposition of ML2 (ox)2H2 O was discussed.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
7.
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
8.
New solid complexes of a herbicide known as dicamba (3,6-dichloro-2-methoxybenzoic acid) with Pb(II), Cd(II), Cu(II) and Hg(II)
of the general formula M(dicamba)2·xH2O (M=metal, x=0-2) and Zn2(OH)(dicamba)3·2H2O have been prepared and studied. The complexes have different crystal structures. The carboxylate groups in the lead, cadmium
and copper complexes are bidentate, chelating, symmetrical, in Hg(dicamba)2·2H2O - unidentate, and in the zinc salt - bidentate, bridging, symmetrical. The anhydrous compounds decompose in three stages,
except for the lead salt whose decomposition proceeds in four stages. The main gaseous decomposition products are CO2, CH3OH, HCl and H2O. Trace amounts of compounds containing an aromatic ring were also detected. The final solid decomposition products are oxychlorides
of metals and CuO.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
9.
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
10.
The triethanolamine complexes, [M(tea)2]sq·nH2O, (n=2 for Co(II), n=0 for Ni(II), Cu(II) and n=1 for Cd(II), tea=triethanolamine, sq2−=squarate), have been synthesized and characterized by elemental analyses, magnetic susceptibility and conductivity measurements,
UV-Vis and IR spectra, and thermal analyses techniques (TG, DTG and DTA). The Co(II), Ni(II) and Cu(II) complexes possess
octahedral geometry, while the Cd(II) complex is monocapped trigonal prismatic geometry. Dianionic squarate behaves as a counter
ion in the complexes. The thermal decomposition of these complexes takes place in three stages: (i) dehydration, (ii) release of the tea ligands and (iii) burning of organic residue. On the basis of the first DTGmax of the decomposition, the thermal stability of the anhydrous complexes follows the order: Ni(II), 289°C>Co(II), 230°C>Cu(II),
226°C>Cu(II), 170°C in static air atmosphere. The final decomposition products — the respective metal oxides — were identified
by FTIR spectroscopy. 相似文献
11.
P. Naumov V. Jordanovska O. Grupče B. Boyanov G. Jovanovski 《Journal of Thermal Analysis and Calorimetry》2001,65(1):59-67
The adducts of Co, Ni, Cu, Zn and Pb saccharinates with 2,2'-bipyridine were synthesized and their thermal behaviour in the 20–1000°C temperature interval in a static air atmosphere was investigated. Regardless of the coordination, the decomposition starts with dehydration and proceeds with removal of the bipyridine ligand(s). The resulting metal(II) saccharinates adopt characteristic two-step decomposition, the first step being the SO2 release. Their stability was found tobe metal-dependent. The thermal decomposition pathways were correlated with the existing structural data about the compounds.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
12.
The [Co(HOr)(H2O)2(im)2] (1), [Ni(HOr)(H2O)2(im)2] (2), [Zn(H2O)2(im)4](H2Or)2 (3) and [Cd(HOr)(H2O)(im)3] (4) complexes (H3Or: orotic acid, im: imidazole) were synthesized and characterized by elemental analysis, magnetic and conductance measurements,
UV-vis and IR spectra. The thermal behaviour of the complexes was also studied by simultaneous thermal analysis techniques
(TG, DTG and DTA). The orotate ligand (HOr2−) coordinated to the Co(II), Ni(II) and Cd(II) ions are chelated to the deprotonated pyrimidine nitrogen (N(3)) and the carboxylate oxygen, while do not coordinate to the Zn(II) ion is present as a counter-ion (H2Or−). The first thermal decomposition process of all the complexes is endothermic deaquation. This stage is followed by partially
(or completely) decomposition of the imidazole and orotate ligands. In the later stage, the remained organic residue exothermically
burns. On the basis of the first DTGmax, the thermal stability of the complexes follows order: 2, 176°C>1, 162°C>4, 155°C>3, 117°C in static air atmosphere. The final decomposition products which identified by IR spectroscopy were the corresponding
metal oxides. 相似文献
13.
Nickel(II) and cobalt(II) complexes with the commercial herbicides 2,4-dichlorophenoxyacetic acid (2,4D; C8H6O3Cl2) and 2-(2,4-dichlorophenoxy)-propionic acid (2,4DP; C9H8O3Cl2) were prepared and characterized. On the basis of the results of elemental analysis and Ni and Co determination, the following
molecular formulae were proposed for the obtained compounds: Ni(C8H5O3Cl2)2·6H2O, Co(C8H5O3Cl2)2·6H2O, Ni(C9H7O3Cl2)2·2H2O and Co(C9H7O3Cl2)2·2H2O. X-ray powder analysis was carried out. The IR, electronic (VIS) spectra and conductivity data were discussed. Water solubility
of the synthesized complexes at room temperature was examined. Thermal decomposition of the compounds was studied. Dehydration
processes occur during heating in air. The anhydrous compounds decompose via different intermediate products to oxides. TG/MS
studies indicate formation of gaseous mass fragments of decomposition including H2O+, OH+, CO2
+, HCl+, Cl2
+, CH3Cl+, CH2O+, C6H6
+ and other.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
14.
The thermal stabilities of 5-chloro-2-methoxybenzoates of Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) were studied in air and
nitrogen atmospheres. The complexes were obtained as mono-, di-, tetra-and pentahydrates with a metal to ligand ratio of 1:2
and with colours typical for M2+ ions (Mn-slightly pink, Co-pink, Ni-green, Cu-blue and Zn-white) and as polycrystalline compounds. When heated they dehydrate
to form anhydrous salts which nextare decomposed to the oxides of the respective metals in air while in nitrogen to the mixtures
of metal oxides and oxychlorides and carbon. The most thermally stable in air, nitrogen and argon atmospheres is 5-chloro-2-methoxybenzoate
of Cu(II) while the least thermally stable is that of Co(II).
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
15.
Complexes of Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) with 3-(2-pyridyl)-1-(2-hydroxy phenyl)-2-propen-1-one (PHPO), 3-(1-naphthyl)-1-(2-hydroxy
phenyl)-2-propen-1-one (NHPO) and 3-(3,4-dimethoxy phenyl)-1-(2-hydroxy phenyl)-2-propen-1-one (DMPHPO) have been synthesized
and characterized by analytical, conductivity, thermal, magnetic, infrared, electronic and electron spin resonance data. Based
on analytical data the stoichiometry of the complexes has been found to be 1 : 2. The conductivity data show that all these
complexes are non-electrolytes. The infrared spectral data indicate that the ligand PHPO acts as uninegative tridentately
towards Co(II) and Ni(II) and bidentately with Cu(II), Zn(II) and Cd(II). Ligands like NHPO and DMPHPO act as uninegative
bidentately with all the metal ions. The electronic spectral data suggest that all the Co(II) complexes and Ni(II) of PHPO
complex are octahedral and all the Cu(II) and Ni(II) of NHPO and DMPHPO complex are square-planar. The complex of Zn(II) and
Cd(II) are tetrahedral. ESR parameters of Cu(II) complexes have been calculated and relevant conclusions have been drawn with
respect to the nature of bonds present in them. 相似文献
16.
《Journal of Saudi Chemical Society》2020,24(5):381-392
Cobalt (II), nickel (II), copper (II) and manganese (II) complexes of dihydrazone derived from the condensation of oxaloyldihydrazide with 2-hydroxybenzaldehyde have been synthesized. The dihydrazone ligand/chelates were characterized on the basis of their elemental analyses, spectral (UV–Vis., FT-IR, mass, 1H NMR), magnetism, thermal (TGA) measurements and structures of the compounds have been established. The surface morphology of the desired complexes was studied by SEM. The ligand is coordinated to the Ni(II), Co(II), Mn(II) and Cu(II) centers in bi, tetra, penta and hexadentate way giving mono-nuclear complexes except in case of manganese and copper the bi-nuclear complexes were formed. The nickel complex has tetrahedral geometry while the other complexes are suggested to have octahedral configurations. The prepared samples have been assayed for their electrical activities. The electrical activity (DC and AC conductivity) for ligand and its metal complexes has been examined at different frequencies (1, 10, 100 kHz) in the temperature ranges 303–573 and 300–625 K, respectively. The DC and AC conductivity are viewed as thermally activated process at higher temperatures and a marked increment was seen in case of Mn(II) complex. The dielectric permittivity was determined in the temperature area of 300–625 K and diminished with augmentation of frequency proposing a typical behavior of dielectrics. 相似文献
17.
K. Kafarska D. Czakis-Sulikowska W. M. Wolf 《Journal of Thermal Analysis and Calorimetry》2009,96(2):617-621
New metal(II) complexes with empirical formulae Co(ibup)2·4H2O, Cd(ibup)2·3H2O, Co(nap)2·H2O, Cd(nap)2·3H2O (where ibup=(CH3)2CHCH2C6H4CH(CH3COO−) and nap=CH3O(C10H6)CH(CH3COO−)) were isolated and investigated. The complexes were characterized by elemental analysis, molar conductance, IR spectroscopy
and thermal decomposition. The thermal behavior was studied by TG, DTG, DTA methods under non-isothermal conditions in air
atmosphere. The hydrated complexes lose water molecules in first step. All complexes decompose via intermediate products to corresponding metal oxides CoO and CdO. A coupled TG-MS system was used to detect the principal
volatile products of thermolysis and fragmentation processes of Co(nap)2·H2O. The IR spectra of studied complexes revealed also absorption of the carboxylate group. Principal concern with the position
of asymmetric, symmetric frequencies. The value of their separation allow to deduce about type of coordination these groups. 相似文献
18.
K. Mészáros-Szécsényi E. Z. Ivegeš V. M. Leovac A. Kovács G. Pokol Ž. K. Jaćimović 《Journal of Thermal Analysis and Calorimetry》1999,56(2):493-501
Complexes represented by the general formula [MCl2L2] (M(II)=Zn, Mn, Co) and complexes of [Cu3Cl6L4] and CuSO4L2·4H2O, CoSO4L2·3H2O, [ZnSO4L3] where L stands for 3-amino-5-methylpyrazole were prepared. The complexes were characterized by elemental analysis, FT-IR
spectroscopy, thermal (TG, DTG, DSC and EGA) methods and molar conductivity measurements. Except for the Zn-complexes, the
magnetic susceptibilities were also determined.
Thermal decomposition of the sulphato complexes of copper(II) and cobalt(II) and the chloro complexes of cobalt(II) and manganese(II)
resulted in well-defined intermediates. On the basis of the IR spectra and elemental analysis data of the intermediates a
decomposition scheme is proposed.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
19.
Wiesława Ferenc Beata Bocian J. Sarzyński 《Journal of Thermal Analysis and Calorimetry》2006,84(2):377-383
Four new complexes of 2,3,4-trimethoxybenzoic acid
anion with manganese(II), cobalt(II), nickel(II) and copper(II) cations were
synthesized, analysed and characterized by standard chemical and physical
methods. 2,3,4-Trimethoxybenzoates of Mn(II), Co(II), Ni(II) and Cu(II) are
polycrystalline compounds with colours typical for M(II) ions. The carboxylate
group in the anhydrous complexes of Mn(II), Co(II) and Ni(II) is monodentate
and in that of Cu(II) monohydrate is bidentate bridging one. The anhydrous
complexes of Mn(II), Co(II) and Ni(II) heated in air to 1273 K are stable
up to 505–517 K. Next in the range of 505–1205 K they decompose
to the following oxides: Mn3O4,
CoO, NiO. The complex of Cu(II) is stable up to 390 K, and next in the range
of 390–443 K it loses one molecule of water. The final product of its
decomposition is CuO. The solubility in water at 293 K is of the order of
10–3 mol dm–3
for the Mn(II) complex and 10–4 mol dm–3
for Co(II), Ni(II) and Cu(II) complexes. The magnetic moment values of Mn2+,
Co2+, Ni2+ and Cu2+
ions in 2,3,4-trimethoxybenzoates experimentally determined in the range of
77–300 K change from 5.64–6.57 μB (for Mn2+),
4.73–5.17 μB (for Co2+), 3.26–3.35 μB
(for Ni2+) and 0.27–1.42 μB (for Cu2+).
2,3,4-Trimethoxybenzoates of Mn(II), Co(II) and Ni(II) follow the Curie–Weiss
law, whereas that of Cu(II) forms a dimer. 相似文献
20.
New metal complexes of Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) with salicylidine-2-aminobenzimidazole (SABI) are
synthesized and their physicochemical properties are investigated using elemental and thermal analyses, IR, conductometric,
solid reflectance and magnetic susceptibility measurements. The base reacts with these metal ions to give 1:1 (Metal:SABI)
complexes; in cases of Fe(III), Co(II), Cu(II), Zn(II) and Cd(II) ions; and 1:2 (Metal:SABI) complexes; in case of Ni(II)
ion. The conductance data reveal that Fe(III) complex is 2:1 electrolyte, Co(II) is 1:2 electrolyte, Cu(II), Zn(II) and Cd(II)
complexes are 1:1 electrolytes while Ni(II) is non-electrolyte. IR spectra showed that the ligand is coordinated to the metal
ions in a terdentate mannar with O, N, N donor sites of the phenloic -OH, azomethine -N and benzimidazole -N3. Magnetic and
solid reflectance spectra are used to infer the coordinating capacity of the ligand and the geometrical structure of these
complexes. The thermal decomposition of the complexes is studied and indicates that not only the coordinated and/or crystallization
water is lost but also that the decomposition of the ligand from the complexes is necessary to interpret the successive mass
loss. Different thermodynamic activation parameters are also reported, using Coats-Redfern method.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献