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1.
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
2.
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
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. 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
5.
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
6.
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
7.
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
8.
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
9.
《Journal of Coordination Chemistry》2012,65(6):1006-1015
Two new complexes, [Mn(H2bptc)(2,2′-bpy)2]?·?2H2O (1) and [Mn3(Hbptc)2(2,2′-bpy)3(H2O)8]?·?2H2O (2) (H4bptc?=?biphenyl-2,5,2′,5′-tetracarboxylic acid, 2,2′-bpy?=?2,2′-bipyridine), have been synthesized under hydrothermal conditions. Their structures have been characterized by single-crystal X-ray diffraction, elemental analyses, IR spectra, powder X-ray diffraction, and thermogravimetric analyses. Complexes 1 and 2 are both linked into 3-D supramolecular networks by non-covalent interactions (O–H?···?O, C–H?···?O, C–H?···?π, and π?···?π). Complexes 1 and 2 exhibit weak antiferromagnetic interactions. 相似文献
10.
D. Czakis-Sulikowska A. Czylkowska J. Radwańska-Doczekalska R. Grodzki E. Wojciechowska 《Journal of Thermal Analysis and Calorimetry》2007,90(2):557-564
New mixed-ligands complexes with empirical formulae: M(2,4′-bpy)2L2·H2O (M(II)Zn, Cd), Zn(2-bpy)3L2·4H2O, Cd(2-bpy)2L2·3H2O, M(phen)L2·2H2O (where M(II)=Mn, Ni, Zn, Cd; 2,4′-bpy=2,4′-bipyridine, 2-bpy=2,2′-bipyridine, phen=1,10-phenanthroline, L=HCOO−) were prepared in pure solid state. They were characterized by chemical, thermal and X-ray powder diffraction analysis, IR
spectroscopy, molar conductance in MeOH, DMF and DMSO. Examinations of OCO− absorption bands suggest versatile coordination behaviour of obtained complexes. The 2,4′-bpy acts as monodentate ligand; 2-bpy and phen as chelating ligands. Thermal studies were performed in static air atmosphere. When the temperature raised the dehydration
processes started. The final decomposition products, namely MO (Ni, Zn, Cd) and Mn3O4, were identified by X-ray diffraction. 相似文献
11.
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
12.
R. E. Lyon R. N. Walters S. I. Stoliarov 《Journal of Thermal Analysis and Calorimetry》2007,89(2):441-448
The present article describes the synthesis,
structural features and thermal studies of the complexes of the type [M(SB)2(H2O)2]·nH2O [where
HSB=pyridine-m-carboxaldene-o-aminobenzoic
acid and M=Mn(II), Co(II), Ni(II), Cu(II),
Zn(II) and Cd(II)]. The complexes have been characterized on the basis of
elemental analyses, magnetic susceptibility measurements, (FTIR and electronic)
spectra and thermal studies. The nature of the bonding has been discussed
on the basis of infrared spectral data. Magnetic susceptibility measurements
and electronic spectral data suggest a six-coordinated structure of these
complexes. The complexes of Mn(II), Co(II), Ni(II), Cu(II) are paramagnetic,
while Zn(II) and Cd(II) are diamagnetic in nature.
The thermal
decomposition of the complexes have been studied and indicates that not only
the crystallization and coordinated water are lost but also that the decomposition
of the ligand from the complexes is necessary to interpret the successive
mass losses. The kinetic parameters such as order of reaction (n)
and the energy of activation (E
a)
have been reported using Freeman–Carroll method. The entropy (S*), the pre-exponential factor (A),
the enthalpy (H*) and the Gibbs free energy
(G*) have been calculated. 相似文献
13.
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
14.
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
15.
Three types of metal complexes containing coordinated zwitterionic 8-Quinolinol(oxine) are isolated from the reaction ofMOx
2 (M=divalent Ni, Mn, or Mg; HO
x
=oxine) and haloacetic acidsRCO2H (R=CF3, CCl3, CHCl2, or CH2Cl) in benzene. These types are:M(O2CR)Ox·HOx forM=Ni,R=CCl3, CHCl2, and CH2Cl and forM=Mn,R=CHCl2.MOx(HOx) (RCO2)MOx·nH2O forM=Ni, Mn, or Mg,R=CF3 andn=1,1, and 4, respectively.MO
x
(HOx) (RCO2)2
MOx forM=Mn andR=CCl3. These types are compared with the simple mixed chelateMn(O2CCH2Cl)Ox. Interrelated reactions are suggested to explain the formation of these metal complexes and the contributing factors are discussed. The coordination of the zwitterion to the metal ion through its phenolate oxygen and the presence of the triatomic system+N–H...O in the three types of metal complexes are evidenced by typical infrared bands. Analytical and spectral data are in accordance with the suggested formulations.
Koordination von zwitterionischem 8-Chinolinol (Oxin) an gemischten Oxinat-Carboxylat-Komplexen des divalenten Nickel, Mangan und Magnesium
Zusammenfassung Drei Typen von Metallkomplexen mit koordiniertem zwitterionischem 8-Chinolinol (Oxin) wurden aus der Reaktion vonMOx 2 [M=Ni(II), Mn(II), Mg(II); HOx=Oxin] mit Halogen-essigsäurenRCOOH (R=CF3, CCl3, CHCl2, CH2Cl) in Benzol isoliert. Es werden Reaktionswege zur Bildung der Komplexe diskutiert. Die Koordination des Zwitterions über den phenolischen Sauerstoff und die Präsenz der Gruppierung+N–H...O in allen Typen der untersuchten Metallkomplexe wird auf Grund typischer IR-Banden nachgewiesen.相似文献
16.
《Journal of Coordination Chemistry》2012,65(23):4077-4087
Two complexes, [Cu2(TFSA)(2,2′-bpy)4]?·?TFSA?·?8H2O (1) and {[Cu(4,4′-bpy)(H2O)2]?·?TFSA?·?6H2O} n (2) (H2TFSA?=?tetrafluorosuccinic acid, 2,2′-bpy?=?2,2′-bipyridine, and 4,4′-bpy?=?4,4′-bipyridine), have been synthesized and structurally characterized by X-ray structural analyses. Complex 1 is a binuclear molecule bridged by TFSA ligands; 2 is a 1-D chain bridged by 4,4′-bpy ligands. The asymmetric units of the two complexes are composed of cationic complexes [Cu2(TFSA)(2,2′-bpy)4]2+ (1) and [Cu(4,4′-bpy)(H2O)2]2+ (2), free TFSA anion, and independent crystallization water molecules. A unique 2-D hybrid water–TFSA anionic layer by linkage of {[(H2O)8(TFSA)]2?} n fragments consisting of 1-D T6(0)A2 water tape and TFSA anionic units by hydrogen bonds in 1 was observed. Unique 2-D hybrid water–TFSA anionic layer generated by the linkage of {[(H2O)6(TFSA)]2?} n fragments consisting of cyclic water tetramers with appended water molecules and TFSA anionic units, and 1-D metal–water tape [Cu–H2O?···?(H2O)6?···?H2O?] n in 2 were found. 3-D supramolecular networks of the two complexes consist of cationic complexes and water–TFSA anionic assemblies connected by hydrogen bonds. 相似文献
17.
The 1,10-phenanthroline (phen) complexes of Co(II), Ni(II), Cu(II) and
Cd(II) orotates were synthesized and characterized by elemental analysis,
magnetic susceptibility, spectral methods (UV-vis and FTIR) and thermal analysis
techniques (TG, DTG and DTA). The Co(II), Ni(II), Cu(II) and Cd(II) ions in
diaquabis(1,10-phenanthroline)metal(II) diorotate octahedral complexes [M(H2O)2(phen)2](H2Or)2·nH2O
(M=Co(II), n=2.25; Ni(II), n=3;
Cu(II) and Cd(II), n=2) are coordinated
by two aqua ligands and two moles of phen molecules as chelating ligands through
their two nitrogen atoms. The monoanionic orotate behaves as a counter ion
in the complexes. On the basis of the first DTGmax,
the thermal stability of the hydrated complexes follows the order: Cd(II),
68°C 68°C 相似文献
18.
Homo and heterobinuclear complexes of arylidene- anthranilic acids with Cu(II), Ni(II) and Co(II) are prepared and characterised by chemical analysis, spectral and X-ray diffraction techniques as well as conductivity measurements. Two types of homo-binuclear complexes are formed. The first has the formula M2L2Cl2(H2O)n where M=Cu(II), Ni(II) and Co(II), L = p-hydroxybenzylideneanthranilic acid (hba), p-dimethylaminobenzylideneanthranilic acid (daba) and p-nitrobenzylideneanthranilic acid(nba) and n = 0–3. The second type has the formula M2LCl3(H2O)n in which M is the same as in the first type, L = benzylideneanthranilic acid (ba), (daba) (in cases of Cu(II) and Ni(II)); and n = 1–5. Heterobinuclear complexes having the formula (MLCl2H2O) MCl2(H2O)n are isolated by reaction of Cu(II) binary chelates with Ni(II) and/or Co(II) chlorides. These are also characterized and their structures are elucidated. 相似文献
19.
Mihaela Badea Rodica Olar Dana Marinescu Gina Vasile 《Journal of Thermal Analysis and Calorimetry》2008,92(1):209-214
A series of new complexes with mixed ligands of the type [ML(C3H3O2)2]·nH2O (((1)
M=Mn, n=1; (2)
M=Co(II), n=2; (3)
M=Ni(II), n=4; (4)
M=Cu(II), n=1.5; (5)
M=Zn(II), n=0; L=3-amino-1,2,4-triazole and (C3H3O2)=acrylate anion) were synthesized and characterised by chemical analysis and IR data. In all complexes the 3-amino-1,2,4-triazole
acts as bridge while the acrylate acts as bidentate ligand except for complex (5) where it is found as unidentate. The thermal behaviour steps were investigated in nitrogen flow. The thermal transformations
are complex processes according to TG and DTG curves including dehydration, acrylate ion and 3-amino-1,2,4-triazole degradation
respectively. The final products of decomposition are the most stable metal oxides, except for complex (4) that leads to metallic copper. 相似文献
20.
Marleen L. B. F. Hereygers H. O. Desseyn 《Journal of Thermal Analysis and Calorimetry》1996,47(1):143-150
Oxathioamidates (CSNR1
R
2COOKR
1=R
2=H (A),R
1=H andR
2=CH3 (B),R
1,=R
2=CH3 (C)) can act as O, S donors and form pentaatomic ring systems with divalent metals (M(II)=Mn, Fe, Co, Ni, Cu, Zn). Vibrational spectra and thermal analysis provide information on the amount and nature of associated water molecules. The dehydration of MA2(H2O)2 (M=Mn, Fe, Co, Ni) can be very well explained by the C.F.S.E. (crystal field stabilization energy) for weak field octahedral complexes. The complexes with ligand A and B decompose to form polymers by deprotonation on the thioamide group. The proposed structures are confirmed by the vibrational spectra. For ligand C no stable intermediates are formed during heating, degradation proceeds until metal sulphide remains.The N.F.W.O. is thanked for the financial support towards the spectroscopic and thermal equipment. The authors are very grateful to Ing. J. Janssens for the TG/DTA measurements. 相似文献