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1.
Brzyska W. Bartyzel A. Zieniewicz K. Zwolińska A. 《Journal of Thermal Analysis and Calorimetry》2000,63(2):493-500
Rare earth element 3-methyladipates were prepared as crystalline solids with general formula Ln2(C7H10O4)3⋅nH2O, where n=6 for La, n=4 for Ce,Sm–Lu, n=5 for Pr, Nd and n=5.5 for Y. Their solubilities in water at 293 K were determined (2⋅10–3–1.5⋅10–4 mol dm–3). The IR spectra of the prepared complexes suggest that the carboxylate groups are bidentate chelating. During heating the
hydrated 3-methyladipates lose all crystallization water molecules in one (Ce–Lu) or two steps (Y) (except of La(III) complex
which undergoes tomonohydrate) and then decompose directly to oxides (Y, Ce) or with intermediate formation of oxocarbonates
Ln2O2CO3 (Pr–Tb) or Ln2O(CO3)2 (Gd–Lu). Only La(III) complex decomposes in four steps forming additionally unstable La2(C7H10O4)(CO3)2.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
2.
Synthesis And Characterization Of Complexes Of Rare Earth Elements With 1,1-Cyclobutanedicarboxylic Acid 总被引:1,自引:0,他引:1
The complexes of yttrium and lanthanide with 1,1-cyclobutanedicarboxylic acid of the formula: Ln2(C6H6O4)3⋅nH2O, where n=4 for Y, Pr–Tm, n=5 for Yb,Lu, n=7 for La, Ce have been studied. The solid complexes have colours typical of Ln3+ ions. During heating in air they lose water molecules and then decompose to the oxides, directly (Y, Ce, Tm, Yb) or with
intermediate formation. The thermal decomposition is connected with released water (313–353 K), carbon dioxide, hydrocarbons(538–598
K) and carbon oxide for Ho and Lu. When heated in nitrogen they dehydrate to form anhydrous salt and next decompose to the
mixture of carbon and oxides of respective metals. IR spectra of the prepared complexes suggest that the carboxylate groups
are bidentate chelating.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
3.
《Journal of Coordination Chemistry》2012,65(10):1784-1794
Two d10 metal complexes, {[Zn(Hbtc)(bmt)]·DMF·5H2O} n (1) and {[Cd(Hbtc)(bmt)]·0.5DMF·0.5H2O} n (2) (H3btc?=?1,3,5-benzenetricarboxylic acid, bmt?=?2-((benzoimidazol-yl)methyl)-1H-1,2,4-triazole), have been synthesized under solvothermal conditions by employing bmt and H3btc. Single-crystal X-ray diffraction shows that Zn(II) ions are connected by bmt with bidentate-bridging coordination and by 1,3,5-benzenetricarboxylate with bis-monodentate coordination leading to the 2D structure of 1. Complex 2 exhibits a 2D layer structure, in which bmt coordinate tridentate-bridging to Cd(II) and 1,3,5-benzenetricarboxylates coordinate to Cd(II) unidentate/chelating. Photoluminescence and thermogravimetric analyses of the two complexes are investigated. 相似文献
4.
Z. Rzączyńska A. Kula J. Sienkiewicz-Gromiuk A. Szybiak 《Journal of Thermal Analysis and Calorimetry》2011,103(1):275-281
The complexes of rare earth elements with 2,3-naphthalenedicarboxylic acid of the formula: Ln2(C12H6O4)3·nH2O, where Ln = La(III)-Lu(III) and Y(III); n = 3 for La(III), Ce(III); n = 6 for Pr(III)-Yb(III) and Y(III) and n = 5 for Lu(III) have been synthesized and characterized by elemental analysis, IR spectroscopy, thermal analysis (TG, DTG,
DTA and TG-FTIR) and X-ray analysis. They are sparingly soluble in water and stable at room temperature. During heating in
air atmosphere, they lose all water molecules in several steps, generally in two or three steps, except for the La(III) and
Ce(III) complexes which lose all water molecules in one step. The anhydrous compounds are stable up to about 773 K and then
decompose to corresponding oxides. The thermal decomposition is connected with the release of water molecules (443 K), carbon
dioxide (713 K) and hydrocarbons. 相似文献
5.
Summary Complexes of heavy lanthanide(III) (Gd-Lu) and Y(III) with 4-chlorophthalic acid were prepared and their IR spectra, solubility
in water at 295 K and thermal decomposition were investigated. When heated the complexes with general formula Ln2[ClC6H3(CO2)2]3·nH2O where n=6 for Tb, Dy(III), n=4 for Gd, Ho and Er(III), n=2 for Tm-Lu(III) and n=3 for Y(III) decompose to the oxides Ln2O3, Tb4O7 with intermediate formation of oxochlorides LnOCl. 相似文献
6.
W. Ferenc A. Dziewulska-Kułaczkowska J. Sarzyński B. Paszkowska 《Journal of Thermal Analysis and Calorimetry》2008,91(1):285-292
4-Chloro-2-methoxybenzoates of heavy lanthanides(III) and yttrium(III) were obtained as mono-, di-, tri-or tetrahydrates with
metal to ligand ratio of 1:3 and general formula Ln(C8H6ClO3)3·nH2O, where n=1 for Ln=Er, n=2 for Ln=Tb, Dy, Tm, Y, n=3 for Ln=Ho and n=4 for Yb and Lu. The complexes were characterized by elemental analysis, FTIR spectra, TG, DTA and DSC curves, X-ray diffraction
and magnetic measurements.
The carboxylate group appears to be a symmetrical bidentate chelating ligand. All complexes are polycrystalline compounds.
The values of enthalpy, ΔH, of the dehydration process for analysed complexes were also determined. The solubilities of heavy lanthanide(III) 4-chloro-2-methoxybenzoates
in water at 293 K are of the order of 10−4 mol dm−3. The magnetic moments were determined over the range of 76–303 K. The results indicate that there is no influence of the
ligand field of 4f electrons on lanthanide ions and the metal ligand bonding is mainly electrostatic in nature. 相似文献
7.
A. Kula 《Journal of Thermal Analysis and Calorimetry》2004,75(1):79-86
Complexes of lanthanides(III) (La-Lu) and Y(III) with 3,4,5-trihydroxybenzoic acid (gallic acid) were obtained and their thermal decomposition, IR spectra and solubility in water have been investigated. When heated, the complexes with a general formula Ln(C7H5O5)(C7H4O5)·nH2O (n=2 for La-Ho and Y: n=0 for Er-Lu) lose their crystallization water and decompose to the oxides Ln2O3, CeO2, Pr6O11, and Tb4O7, except of lanthanum and neodymium complexes, which additionally form stable oxocarbonates such as Ln2O2CO3. The complexes are sparingly soluble in water (0.3·10–5–8.3·10–4 mol dm–3).This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
8.
The complexes of yttrium and heavy lanthanides with 3,4-dimethoxybenzoic acid of the formula: Ln(C9 H9 O4 )3 ×n H2 O, where Ln =Y(III), Tb(III), Dy(III), Ho(III), Er(III), Tm(III), Yb(III) and Lu(III), and n =4 for Tb(III), Dy(III), n =3 for Ho(III), and n =0 for Er(III), Tm(III), Yb(III), Lu(III) and Y(III) have been prepared and characterized by elemental analysis, IR spectroscopy,
thermogravimetric and magnetic studies and X-ray diffraction measurements. The complexes have colours typical of Ln3+ ions (Ho - cream, Tb, Dy, Yb, Lu, Y - white, Er - salmon). The carboxylate group in these complexes is a symmetrical, bidentate,
chelating ligand. They are crystalline compounds characterized by various symmetry. On heating in air to 1273 K the hydrated
3,4-dimethoxybenzoates decompose in two steps while those of anhydrous only in one stage. The tetrahydrates of Tb and Dy and
trihydrate of Ho 3,4-dimethoxybenzoates are firstly dehydrated to form anhydrous salts that next are decomposed to the oxides
of the respective metals. The complexes of Er, Tm, Yb, Lu and Y are directly decomposed to the oxides of the appropriate elements.
The solubility in water at 293 K for yttrium and heavy lanthanides is in the order of 10-4 -10-3 mol dm-3 . The magnetic moments of the complexes were determined over the range 77–298 K. They obey the Curie-Weiss law. The values
of μeff calculated for all compounds are close to those obtained for Ln3+ by Hund and van Vleck. The results show that there is no influence of the ligand field on 4f electrons of lanthanide ions
in these polycrystalline compounds and 4f electrons do not take part in the formation of M-O bonding.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
9.
Fourteen new complexes with the general formula of Ln(Hmna)3·nH2O (n=2 for Ln=La-Ho and n=1 for Er-Lu, H2mna=2-mercaptonicotinic acid) were synthesized and characterized by elemental analyses, IR spectra and thermogravimetric analyses.
In addition, molar specific heat capacities were determined by a microcalorimeter at 298.15 K. The IR spectra of the prepared
complexes revealed that carboxyl groups of the ligands coordinated with Ln(III) ions in bidentate chelating mode. Hydrated
complexes lost water molecules during heating in one step and then the anhydrous complexes decomposed directly to oxides Ln2O3, CeO2, Pr6O11 and Tb4O7. The values of molar specific heat capacities for fourteen solid complexes were plotted against the atomic numbers of lanthanide,
which presented as ‘tripartite effect’. It suggested a certain amount of covalent character existed in the bond of Ln3+ and ligands, according with nephelauxetic effect of 4f electrons of rare earth ions. 相似文献
10.
The complexes of heavy lanthanides and yttrium with 2,3-dimethoxybenzoic acid of the formula: Ln(C9h9O4)3·nH2O, where Ln=Tb(III), Dy(III), Ho(III), Er(III), Tm(III), Yb(III), Lu(III), Y(III), and n=2 for Tb(III), Dy(III), Ho(III), Y(III), n=1 for Er(III), Tm(III), n=0 for Yb(III) and Lu(III) have been synthesized and characterized by elemental analysis, ir spectroscopy, thermogravimetric
studies and x-ray diffraction measurements. The complexes have colours typical for Lnł3+ ions (Tb(III), Dy(III), Tm(III), Yb(III), Lu(III), Y(III) - white; Ho(III) - cream and Er(III) - salmon). the carboxylate
groups in these complexes are a symmetrical, bidentate, chelating ligand or tridentate chelating-bridging. they are isostructural
crystalline compounds characterized by low symmetry. On heating in air to 1273 k the 2,3-dimethoxybenzoates of heavy lanthanides
and yttrium decompose in various ways. The complexes of Tb(III), Dy(III), Ho(III), Er(III), Tm(III) and Y(III) at first dehydrate
to form anhydrous salts which next are decomposed to the oxides of the respective metals. 2,3-dimethoxybenzoates of Yb(III)
and Lu(III) are directly decomposed to oxides. When heated in nitrogen the hydrates also dehydrate in one step to form the
anhydrous complexes that next form the mixture of carbon and oxides of respective metals or their carbonates. The solubility
of the yttrium and heavy lanthanide 2,3-dimethoxybenzoates in water at 293 k is of the order of 10-2 mol dm-3.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
11.
Wanda Brzyska Zofia Rzączyńska Alina Kula 《Monatshefte für Chemie / Chemical Monthly》1989,120(3):211-217
Summary
p-Aminosalicylates of Y, La and lanthanides prepared in the reaction of the ammoniump-aminosalicylate and lanthanide chlorides in solutions have the general formulaLn(C7H6O3N)3·nH2O, wheren=3 for La, Ce;n=2 for Pr, Nd, Sm, Eu;n=0 for Y, Gd—Lu. Their solubilities in water are of the order of 10–3 mol dm–3. Heating above 350–450 K leads to dehydration and decomposition at the same time. The IR and X-ray spectra for the obtained complexes were recorded. It was found that only complexes of La—Nd are crystalline compounds. The way of metal-ligand coordination is discussed.
Darstellung und Charakterisierung der Komplexe von Seltenen Erdmetallen mitp-Aminosalicylsäure
Zusammenfassung Zur Darstellung der Verbindungen des TypsLn(C7H6O3N)3·nH2O (mitn=3 für La, Ce;n=2 für Pr, Nd, Sm, Eu;n=0 für Y, Gd—Lu) wurde die berechnete Menge von Ammonium-p-aminosalicylat undLnCl3-Lösungen beipH5.8 gemischt und zur Kristallisation gebracht. Ihre Wasserlöslichkeit bei 298 K ist in der Größenordnung 10–3 mol dm–3. Beim Erhitzen erfolgt bei 350–450 K Entwässerung und Zersetzung zugleich. Die Infrarot- und Röntgenspektren der erhaltenen Komplexe wurden gemessen und dabei festgestellt, daß nur die La—Nd-Komplexe kristalline Verbindungen sind. Die Art der Koordination der Seltenerdmetalle mit den Liganden wird diskutiert.相似文献
12.
3-Methoxy-4-methylbenzoates of Y(III) and lanthanide(III) (La-Lu) were prepared as crystalline compounds with molar ratio of metal to organic ligand of 1.0:3.0 and general formula Ln(C9H9O3)3·nH2O, where n=2 for Y, La-Er and n=0 for Tm-Lu. IR spectra of the prepared complexes suggest that carboxylate groups are bidentate chelating. During heating dihydrated complexes lose crystallization water molecules in one (Y, La, Pr-Er) or two steps (Ce) and then all the anhydrous complexes decompose directly to oxides Ln2O3, CeO2, Pr6O11 and Tb4O7.Vadim Mamleev is grateful to Region Nord-pas-de-Calais (France) for financial support and to laboratory PERF of ENSCL for its kind invitation to continue the joint work on thermal analysis. 相似文献
13.
Spectral,
magnetic and thermal investigations of some d-electron
element 3-methoxy-4-methylbenzoates
Conditions
for the preparation of Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) 3-methoxy-4-methylbenzoates
were investigated and their quantitative composition and magnetic moments
were determined. The IR spectra and powder diffraction patterns of the complexes
prepared of general formula M(C9H9O3)2·nH2O (n=2
for Mn, Co n=1 for Ni, Cu, n=0
for Zn, Cd) were prepared and their thermal decomposition in air was studied.
Their solubility in water at 293 K is of the order 10–2
(Mn)–10–4 (Cu) mol dm–3.
IR spectra of the prepared 3-methoxy-4-methylbenzoates suggest that carboxylate
groups are bidentate bridging. The magnetic moments for the paramagnetic complexes
of Mn(II), Co(II), Ni(II) and Cu(II) attain values 5.50, 4.45, 3.16 and 1.79
B. M., respectively. During heating the hydrated complexes lose crystallization
water molecules in one step and then the anhydrous complexes decompose directly
to oxides MO and Mn3O4. Only Co(II) complex decomposes to Co3O4
with intermediate formation CoO. 相似文献
14.
Conditions for the formation of rare earth element (Y, La–Lu) 3-methylglutarates were studied and their quantitative composition
and solubilities in water at 293 K were determined (10–2 mol dm–3). The IR spectra of the prepared complexes with general formula Ln2(C6H8O4)3
nH2O (n=3–8) were recorded and their thermal decomposition in the air were investigated. During heating the hydrated 3-methylglutarates
are dehydrated in one step and next anhydrous complexes decompose to oxides Ln2O3 with intermediate formation Ln2O2CO3 (Y, La, Nd–Gd) or directly to the oxides, Ln2O3, CeO2, Pr6O11 and Tb4O7 (Ce, Pr, Tb–Lu).
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
15.
R. Łyszczek 《Journal of Thermal Analysis and Calorimetry》2007,90(2):533-539
The new 1,2,4-benzenetricarboxylates of lanthanide(III) of the formula Ln(btc)·nH2O, where btc is 1,2,4-benzenetricarboxylate; Ln is La-Lu, and n=2 for Ce; n=3 for La, Yb, Lu; and n=4 for Pr-Tm were prepared and characterized by elemental analysis, infrared spectra and X-ray diffraction patterns. Polycrystalline
complexes are isotructural in the two groups: La-Tm and Yb, Lu. IR spectra of the complexes show that all carboxylate groups
from 1,2,4-benzentricarboxylate ligands are engaged in coordination of lanthanide atoms.
The thermal analysis of the investigated complexes in air atmosphere was carried out by means of simultaneous TG-DTA technique.
The complexes are stable up to about 30°C but further heating leads to stepwise dehydration. Next, anhydrous complexes decompose
to corresponding oxides. The combined TG-FTIR technique was employed to study of decomposition pathway of the investigated
complexes. 相似文献
16.
M. S. Khan D. J. Schwartz N. A. Pasha A. K. Kakkar B. Lin P. R. Raithby J. Lewis 《无机化学与普通化学杂志》1992,616(10):121-124
Reaction of Pt(PnBu3)2Cl2 (1) or Pt(AsnBu32Cl2 (2) with stoichiometric amounts of 1,3,5-triethynylbenzene, [1,3,5-(H? C?C? )3C6H3] (3)yields monomeric, [1,3,5-Cl(PnBu3)2(Pt? C? C? )3C6H3] (4), [1,3,5-(C1)(AsnBu3)2Pt? C? C? 3C6H3] (5) or polymeric, {1,3,5-[(PnBu3)2Pt? C?C? ]3C6H3? )n (6), {1,3,5-[(AsnBu3)2Pt? C? C? ]3C6H3? }n (7) complexes. Treatment of (1) with (3) and 2,5-diethynyl-p-xylene,H? C? C? C6H2(CH3)2? C? C? H (8) in varying molar ratios yields a series of high molecular weight cross linked platinum metal containing polyyne copolymers. 相似文献
17.
Wiesława Ferenc B. Cristóvão J. Sarzyński Maria Wojciechowska 《Journal of Thermal Analysis and Calorimetry》2007,88(3):877-883
4-Chloro-2-methoxybenzoates of light lanthanides(III) were obtained as mono-, di-or trihydrates with metal to ligand ratio
of 1:3 and general formula Ln(C8H6ClO3)3·nH2O, where n=1 for Ln=Ce, Pr, n=2 for Ln=Nd, Sm, Eu, Gd and n=3 for Ln=La. The complexes were characterized by elemental analysis, IR spectra, thermogravimetric studies, X-ray diffraction and
magnetic measurements. The carboxylate group appears to be a symmetrical bidentate, chelating ligand. All complexes seem polycrystalline
compounds. Their thermal stabilities were determined in air. When heated they dehydrate to form anhydrous salts which next
are decomposed to the oxides of the respective metals. The solubilities of light lanthanide(III) 4-chloro-2-methoxybenzoates
in water at 293 K are of the order of 10−5 mol dm−3. The magnetic moments were determined over the range of 77–300 K. They obey the Curie-Weiss law. The values of μeff calculated for all compounds are close to those obtained for Ln3+ by Hund and Van Vleck. The results indicate that there is no influence of the ligand field of 4f electrons on lanthanide ions and the metal ligand bonding is mainly electrostatic in nature. 相似文献
18.
Salunke Gawali S. Dalvi R. Ah Khursheed Rane S. 《Journal of Thermal Analysis and Calorimetry》2004,76(3):801-812
Syntheses of phthiocol complexes with Cu(II) in inert media resulted in anhydrous monomer Cu-4: [Cu(NQ)2] and dimer Cu-5: [Cu(NQ)(NSQ)]2, however synthesis in air generates polymeric hydrated Cu-6: [Cu(NQ)2(H2O)2]n. Media and colligation give rise to charge transfers in coordination compounds and lead to different redox ligations of 3-methyl-2-hydroxy-1,4-naphthoquinone.
These redox forms are determined from quantitization of activation energies (E
a) of different pyrolytic steps in TG using the rising temperature expression of Coats and Redfern. 'Tyrosinase'-type mechanism
is discussed for the redox-type ligation. Characteristic six-line EPR signals of dimeric Cu-5 lead to zero field splitting
parameters D=0.01608 cm-1and E=0.01576 cm-1. Cu-6 shows molecular association through hydrogen bonding. Variable temperature magnetic measurement data of Cu-6 from 6
to 300 K is fitted to the polymeric expression of Bonner and Fisher model. The best fit was obtained with antiferrromagnetic
exchange coupling constantJ=-2 cm-1, g=2.2 having R=4.2·10-4.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
19.
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
20.
Z. Rzączyńska M. Woźniak W. Wołodkiewicz A. Ostasz S. Pikus 《Journal of Thermal Analysis and Calorimetry》2007,88(3):871-876
The complexes of yttrium(III) and lanthanides(III) with 5-amino-1,3-benzenedicarboxylic acid form two isostructural series
of compounds and have the general formula Ln2(C8H5O4N)3·nH2O, where n = 13 for Y, La-Er and n=9 for Tm, Yb, Lu. They are insoluble in water and stable at room temperature. On heating in air or inert gas atmosphere they
lose all water molecules in several steps. The anhydrous compounds are stable to about 400°C and next decompose to oxides. 相似文献