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1.
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
2.
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
3.
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
4.
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
5.
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
6.
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
7.
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
8.
Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) 2,5-dichlorobenzoates were prepared and their compositions and solubilities in water
at 295 K were determined. The IR spectra and X-ray diffractograms of the obtained complexes were recorded. The complexes of
Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) were obtained as solids with a 1:2 molar ratio of metal to organic ligand and different
degrees of hydration. When heated at a heating rate of 10 K min-1, the hydrated complexes lose some (Co, Zn) or all (Ni, Cu, Cd) of the crystallization water molecules and then decompose
to oxide MO (Co, Ni) or gaseous products (Cu, Zn, Cd). When heated at a heating rate of 5 K min-1, the complexes of Ni(II) and Cu(II) lose some (Ni) or all (Cu) of the crystallization water molecules and then decompose
directly to MO.
This revised version was published online in July 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.
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
11.
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
12.
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
13.
2,4'-Bipyridyl (2,4'-bipy or L) complexes of Mn(II) with the formulae MnL2X2·2H2O (X–=Cl, Br, NCS, NO3), MnLSO4·5H2O and MnL4(ClO4)2·2H2O were synthesized and characterized via the IR spectra and magnetic, and conductivity measurements. The nature of the Mn(II)-ligand coordination is discussed. The thermal decompositions of these compounds were studied in air atmosphere. The mode of decomposition depends on the anion present, but the final product in all cases is Mn3O4. Some of the intermediates (MnL2Cl2, MnLCl2, MnL2Br2, MnL2(NCS)2 and MnLSO4) formed during the pyrolysis are isomeric with 2,2'-bipy and 4,4'-bipy complexes.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
14.
Conditions for the preparation of Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) 4-methylphthalates were investigated and
their composition, solubility in water at 295 K and magnetic moments were determined. IR spectra and powder diffraction patterns
of the complexes prepared with molar ratio of metal to organic ligand of 1.0:1.0 and general formula: M [ CH3C6H3(CO2)2]·nH2o (n=1-3) were recorded and their decomposition in air were studied. During heating the hydrated complexes are dehydrated in one
(Mn, Co, Ni, Zn, Cd) or two steps (Cu) and next the anhydrous complexes decompose to oxides directly (Cu, Zn), with intermediate
formation of carbonates (Mn, Cd), oxocarbonates (Ni) or carbonate and free metal (Co). The carboxylate groups in the complexes
studied are mono- and bidentate (Co, Ni), bidentate chelating and bridging (Zn) or bidentate chelating (Mn, Cu, Cd). The magnetic
moments for paramagnetic complexes of Mn(II), Co(II), Ni(II) and Cu(II) attain values 5.92, 5.05, 3.36 and 1.96 M.B., respectively.
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.
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
17.
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
18.
Merdivan M. Karipcin F. Kulcu N. Aygun R. S. 《Journal of Thermal Analysis and Calorimetry》1999,58(3):551-557
The thermal decompositions of the complexes of N,N-dialkyl-N'-benzoylthioureas with Cu(II), Ni(II), Pd(II), Pt(II), Cd(II), Ru(III) and Fe(III) were studied by TG and DTA techniques. These metal complexes decompose in two stages: elimination of dialkylbenzamide, and total decomposition to metal sulphides or metals. The influence of the alkyl substituents in these benzoylthiourea chelates on the thermal behaviour of the metal complexes was investigated.This revised version was published online in November 2005 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.
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