共查询到20条相似文献,搜索用时 93 毫秒
1.
Carolina V. Barra Fillipe V. Rocha Adelino V. G. Netto B. Shimura Regina C. G. Frem Antonio E. Mauro Iracilda Z. Carlos Sandra R. Ananias Marcela B. Quilles 《Journal of Thermal Analysis and Calorimetry》2011,106(2):483-488
The pyrazole ligand 3,5-dimethyl-4-iodopyrazole (HdmIPz) has been used to obtain a series of palladium(II) complexes (1–4) of the type [PdX2(HdmIPz)2] {X = Cl− (1); Br− (2); I− (3); SCN− (4)}. All compounds have been isolated, purified, and characterized by means of elemental analysis, IR spectroscopy, 1H and 13C{1H}-NMR experiments, differential thermal analysis (DTA), and thermogravimetry (TG). The TG/DTA curves showed that the compounds
released ligands in the temperature range 137–605 °C, yielding metallic palladium as final residue. The complexes and the
ligand together with cisplatin have been tested in vitro by MTT assay for their cytotoxicity against two murine cancer cell
lines: mammary adenocarcinoma (LM3) and lung adenocarcinoma (LP07). 相似文献
2.
Derivative of 8-hydroxyquinoline i.e. Clioquinol is well known for its antibiotic properties, drug design and coordinating
ability towards metal ion such as Copper(II). The structure of mixed ligand complexes has been investigated using spectral,
elemental and thermal analysis. In vitro anti microbial activity against four bacterial species were performed i.e. Escherichia coli, Pseudomonas aeruginosa, Serratia marcescens, Bacillus substilis and found that synthesized complexes (15–37 mm) were found to be significant potent compared to standard drugs (clioquinol
i.e. 10–26 mm), parental ligands and metal salts employed for complexation. The kinetic parameters such as order of reaction
(n = 0.96–1.49), and the energy of activation (E
a = 3.065–142.9 kJ mol−1), have been calculated using Freeman–Carroll method. The range found for the pre-exponential factor (A), the activation entropy (S* = −91.03 to−102.6 JK−1 mol−1), the activation enthalpy (H* = 0.380–135.15 kJ mol−1), and the free energy (G* = 33.52–222.4 kJ mol−1) of activation reveals that the complexes are more stable. Order of stability of complexes were found to be [Cu(A4)(CQ)OH] · 4H2O > [Cu(A3)(CQ)OH] · 5H2O > [Cu(A1)(CQ)OH] · H2O > [Cu(A2)(CQ)OH] · 3H2O 相似文献
3.
Fillipe V. Rocha Carolina V. Barra Silmar J. S. Franchi Adelino V. G. Netto Antonio E. Mauro Regina C. G. Frem 《Journal of Thermal Analysis and Calorimetry》2011,106(2):385-389
Four new mononuclear Pd(II) complexes of the type [PdX2(tdmPz)] {X = Cl− (1); Br− (2); I− (3); SCN− (4); tdmPz = 1-thiocarbamoyl-3,5-dimethylpyrazole} have been synthesized and characterized by elemental analysis, IR spectroscopy,
1H and 13C{1H}-NMR experiments. The thermal behavior of the complexes 1–4 has been investigated by means of thermogravimetry (TG) and differential thermal analysis (DTA). From the initial decomposition
temperatures, the thermal stability of the complexes can be ordered in the sequence: 3 < 4 ≡ 2 < 1. The final products of the thermal decompositions were characterized as metallic palladium by X-ray powder diffraction. 相似文献
4.
Rodrigo A. de Souza Antonio E. Mauro Adelino V. G. Netto Gislaine A. da Cunha Eduardo T. de Almeida 《Journal of Thermal Analysis and Calorimetry》2011,106(2):375-378
Palladium(II) coordination compounds of general formula trans-[PdX2(isn)2], X = Cl− (1), N3
− (2), SCN− (3), NCO− (4), isn = isonicotinamide; were synthesized and characterized in solid state by elemental analysis, infrared spectroscopy,
and simultaneous TG–DTA. TG experiments reveal that the compounds 1–4 undergo thermal decomposition in three or four stages, yielding Pd0 as final residue, according to calculus and identification by X-ray powder diffraction. 相似文献
5.
Wandee Rakrai Nongnit Morakot Somchai Keawwangchai Chatthai Kaewtong Banchob Wanno Vithaya Ruangpornvisuti 《Structural chemistry》2011,22(4):839-847
The structural geometries of three tripodal thiourea receptors, i.e. 1,3,5-triethyl-2,4,6-tris[(N′-methylthioureido)methyl]benzene (1), tris[N′-methyl-N-(2-aminoethyl)thiourea]methane (2), tris[N′-methyl-N-(2-aminoethyl)thiourea]amine (3), and their complexes with F−, Cl−, Br−, I−, NO3
−, CO3
2−, SO4
2−, HSO4
−, PO4
3−, HPO4
2− and H2PO4
− were obtained using the density functional theory calculations. Electronic and thermodynamic properties of anion binding
complexes of the receptors 1, 2 and 3 were investigated. Recognition abilities of all the receptors in terms of selectivity coefficients are reported. Intermolecular
interactions in all the studied complexes occurring via multi-point hydrogen bonding were found. The receptors 1, 2 and 3 were found to be excellent selectivity for phosphate ion and their binding free energy for the phosphate ion are −292.57,
−291.77 and −295.01 kcal/mol, respectively. 相似文献
6.
Francisco C. C. Arantes Antonio C. Moro Iolanda S. Klein Cristiana da Silva Adelino V. G. Netto Antonio E. Mauro Vânia M. Nogueira 《Journal of Thermal Analysis and Calorimetry》2011,106(2):379-383
The synthesis, spectroscopic characterization, and thermal analysis of the compounds [Pd(X)2(mtu)(PPh3)] (X = Cl− (1), SCN− (2); mtu = N-methylthiourea; PPh3 = triphenylphosphine) and [Pd(X)2(phtu)(PPh3)] (X = Cl− (3), SCN− (4); phtu = N-phenylthiourea) are described. The thermal decomposition of the compounds occurs in two, three, or four stages and the final
decomposition products were identified as Pd0 by X-ray powder diffraction. The thermal stability order of the complexes is 4 > 3>2 > 1. 相似文献
7.
Two two-dimensional coordination complexes, {[Cu4(BTM)6(OPA)4] · 4DMF · 3H2O}
n
(1) and {[Cu(BDTM)(OH)](ClO4) · 2H2O}
n
(2) (BTM = bis(1,2,4-triazol-1-yl)methane, BDTM = bis(3,5-dimethyl-1,2,4-triazol-1-yl)methane, OPA2− = ortho-phthalic dianion, DMF = N,N-dimethylformamide), were synthesized and structurally characterized. Each Cu(II) ion locates in a distorted square pyramidal
geometry in 1, in which OPA2− ligands bridge Cu2+ ions along a axis to form a magnetic transmission chain and BTM ligands act as flexible spacers to construct the two-dimensional layer
structure. In 2, each Cu2+ ion adopts tetra-coordination geometry to two hydroxyl groups and two triazolyl nitrogen atoms from two different BDTM ligands.
Two hydroxyl groups bridge two Cu2+ ions to form a rhombic diamond, and four BDTM ligands connect four diamonds to form a 36-membered macrocyclic structure with
large channels along a axis. Magnetic properties revealed that both OPA2− and OH− mediate anti-ferromagnetic interactions between Cu2+ ions with J = − 0.06(3) and −301.9(2) cm−1 for 1 and 2, respectively.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
8.
H. M. Ye N. Ren H. Li J. J. Zhang S. J. Sun L. Tian 《Journal of Thermal Analysis and Calorimetry》2010,101(1):205-211
The complex of [Nd(BA)3bipy]2 (BA = benzoic acid; bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR spectra, single
crystal X-ray diffraction, and TG/DTG techniques. The crystal is monoclinic with space group P2(1)/n. The two–eight coordinated Nd3+ ions are linked together by four bridged BA ligands and each Nd3+ ion is further bonded to one chelated bidentate BA ligand and one 2,2′-bipyridine molecule. The thermal decomposition process
of the title complex was discussed by TG/DTG and IR techniques. The non-isothermal kinetics was investigated by using double
equal-double step method. The kinetic equation for the first stage can be expressed as dα/dt = A exp(−E/RT)(1 − α). The thermodynamic parameters (ΔH
≠, ΔG
≠, and ΔS
≠) and kinetic parameters (activation energy E and pre-exponential factor A) were also calculated. 相似文献
9.
Shafqat Nadeem Muhammad Khawar Rauf Saeed Ahmad Masahiro Ebihara Syed Ahmed Tirmizi Sarfaraz Ahmed Bashir Amin Badshah 《Transition Metal Chemistry》2009,34(2):197-202
Palladium(II) complexes of thiones having the general formula [Pd(L)4]Cl2, where L = thiourea (Tu), methylthiourea (Metu), N,N′-dimethylthiourea (Dmtu), and tetramethylthiourea (Tmtu) were prepared by reacting K2[PdCl4] with the corresponding thiones. The complexes have been characterized by elemental analysis, IR and NMR spectroscopy, and
two of these, [Pd(Dmtu)4]Cl2 · 2H2O (1) and [Pd(Tmtu)4]Cl2 (2), by X-ray crystallography. An upfield shift in the >C=S resonance of thiones in 13C NMR and downfield shift in N–H resonance in 1H NMR are consistent in showing sulfur coordination with palladium(II). The crystal structures of the complexes show a square-planar
coordination environment around the Pd(II) ions with the average cis and trans S–Pd–S bond angles of 89.64° and 173.48°, respectively.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.
An erratum to this article can be found at 相似文献
10.
Ashok K. Vishwakarma Prasanna S. Ghalsasi 《Journal of Thermal Analysis and Calorimetry》2012,107(1):155-158
The thermal decomposition paths of anilinium, 4-chloro anilinium tetrachlorocopper(II) complexes are compared to their benzilinium
derivative. All these complexes crystallize in the layered structure, typical for a A2MX4 family, are studied in literature for their magnetic, semiconducting properties. TG analyses of (anilinium)2CuCl4 (A) and (4-chloro anilinium)2CuCl4 (B) loses one molecule of organic ammonium hydrochloride along with one molecule of amine, to form (H)CuCl3, which subsequently completely decomposes to Cu above 500 °C. On the other hand, (benzilinium)2CuCl4 (C) loses two molecules of hydrochloride along with chlorine molecule first then two molecules of benzyl amine with formation
of Cu above 300 °C. DSC studies on C have shown reversible endothermic phase transition at 130.95 °C (−1.98 J g−1) while heating and exothermic phase transition at 117.07 °C (0.93 J g−1) while cooling. Thus, the observed changes in the decomposition pathway can be correlated to the order–disorder phase transition
occurred in the compound C. 相似文献
11.
New liquid-crystalline heteropolynuclear complexes L2M (M=Cu2+ (2a), Pd2+ (2b)) were synthesized by the reactions of C5H5FeC5H4−C6H4NH−C2H2−(CO)−C6H4OC12H25 (1, LH) with copper(ii) and palladium(ii) acetates. Compound2b was found to possess monotropic nematic and smectic phases;2a exhibits the monotropic nematic phase and a phenomenon of “double melting”. The compositions and structures of compounds1 and2a,b were established by elemental analysis,1H and13C NMR, ESR, and IR spectroscopy.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 381–383, February, 1999. 相似文献
12.
以5-(4-羧基苯氧基)烟酸配体(H2cpna)和稀土金属离子Dy3+、Ho3+、Er3+和Tm3+为原料,采用水热法合成了4种稀土金属配合物[M(Hcpna)(cpna)(H2O)3]n,其中M=Dy(1)、Ho (2)、Er (3)、Tm (4)。单晶X射线衍射分析表明配合物1、2、3和4为同构配合物,均为一维链状结构。通过红外、元素分析以及粉末X射线衍射对所得配合物进行了表征,同时对配合物的荧光和磁学性质开展了研究。荧光测试结果表明,配合物1~4的荧光强度均低于配体H2cpna的荧光强度。在2~300 K温度范围内1 kOe直流电场下测试了配合物1~4的磁性,结果表明配合物1、2、3和4的χmT值分别为14.04、14.15、11.08和6.83 cm3·mol-1·K,与文献理论值相符合。 相似文献
13.
A new symmetrical vicinal dioxime, N,N′-bis-{4-[[(2-hydroxyphenyl)methylene]hydrazinecarbonyl]phenyl}diaminoglyoxime (LH4), was prepared by reacting anti-dichloroglyoxime with salicylaldehyde 4-aminobenzoylhydrazone. The reaction of ligand with Ni2+ salts gave mono-and homopentanuclear complexes, [Ni(LH3)2] and [Ni5(LH)2X2]. Furthermore, heteropentanuclear complexes of dioxime ligand, [Cu4Ni(LH)2X4], were prepared by the reaction of [Ni(LH3)2)] with Cu2+ salt and a monodentate ligand (X = SCN−, CN−, or N
3
−
). The structures of both the new symmetrical vicinal dioxime and its complexes were identified by elemental analyses, IR,
1H NMR, UV-VIS spectra, and magnetic susceptibility. The elemental analyses and spectral data indicate that the hydrazone side
of ligand acts as a O,N,O′ tridentate and the fourth position is occupied with monodentate anion such as SCN−, CN−, N
3
−
. 相似文献
14.
V. A. Lucca Neto A. E. Mauro A. V. G. Netto A. C. Moro V. M. Nogueira 《Journal of Thermal Analysis and Calorimetry》2009,97(1):57-60
The cyanate-bridged cyclopalladated compound [Pd(C2,N-dmba)(μ-NCO)]2 (dmba=N,N-dimethylbenzylamine) reacts in acetone with pyrazole (pz), 3,5-dimethylpyrazole (dmpz), imidazole (imz) and 2-methylimidazole
(mimz) to give [Pd2(C2,N-dmba)2(μ-NCO)(μ-pz)] (1), [Pd2(C2,N-dmba)2(μ-NCO)(μ-dmpz)] (2), [Pd(C2,N-dmba)(NCO)(imz)] (3) and [Pd(C2,N-dmba)(NCO)(mimz)] (4), respectively. The compounds were characterized by elemental analysis, IR spectroscopy and TG. The thermal decomposition
of the compounds occurs in three consecutive steps and the final decomposition products were identified as Pd(0) by X-ray
powder diffraction. The thermal stability order of the complexes is 2>3>1>4. 相似文献
15.
Li Xu Yang-Yin Xie Nan-Jing Zhong Zhen-Hua Liang Juan He Hong-Liang Huang Yun-Jun Liu 《Transition Metal Chemistry》2012,37(2):197-205
Two ruthenium(II) polypyridyl complexes, namely [Ru(phen)2(DMDPPZ)](ClO4)2
1 (phen = 1,10-phenanthroline, DMDPPZ = 3,6-dimethyldipyrido[3,2-a:2′,3′-c]phenazine) and [Ru(dmp)2(DMDPPZ)](ClO4)2
2 (dmp = 2,9-dimethyl-1,10-phenanthroline), have been synthesized and characterized. The DNA-binding properties of the complexes
were investigated by spectrophotometric methods, viscosity measurements, and photoactivated cleavage studies. The DNA-binding
constants for complexes 1 and 2 have been determined as 8.78 (±0.94) × 105 M−1 (s = 3.02) and 1.26 (±0.35) × 105 M−1 (s = 1.69), respectively. The results suggest that these complexes bind to calf thymus DNA through intercalation. When irradiated
at 365 nm, the complexes promote the photocleavage of pBR322 DNA, and complex 1 cleaves DNA more effectively than complex 2 under comparable experimental conditions. The cytotoxicities of complexes 1 and 2 have been evaluated by the MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-2H-tetrazolium bromide) method. Complex 2 shows higher anticancer potency than complex 1 against four tumor cell lines. The apoptosis-inducing activity was assessed by acridine orange/ethidium bromide staining
assay, and the antioxidant activities of these complexes against hydroxyl radical were also explored. 相似文献
16.
Thermal behaviour of nickel amine complexes containing SO4
2−, NO3
−, Cl− and Br− as counter ions and ammonia and ethylenediamine as ligands have been investigated using simultaneous TG/DTA coupled with
mass spectroscopy (TG/DTA–MS). Evolved gas analyses detected various transient intermediates during thermal decomposition.
The nickel ammonium sulphate complex produces NH, N, S, O and N2 species. The nickel ammonium nitrate complex generated fragments like N, N2, NO, O2, N2O, NH2 and NH. The halide complexes produce NH2, NH, N2 and H2 species during decomposition. The ligand ethylenediamine is fragmented as N2/C2H4, NH3 and H2. The residue hexaamminenickel(II) sulphate produces NiO with crystallite size 50 nm. Hexaammine and tris(ethylenediamine)nickel(II)
nitrate produce NiO in the range 25.5 nm and 23 nm, respectively. The halide complexes produce nano sized metallic nickel
(20 nm) as the residue. Among the complexes studied, the nitrate containing complexes undergo simultaneous oxidation and reduction. 相似文献
17.
Alessandra Stevanato Antonio E. Mauro Adelino V. G. Netto 《Journal of Thermal Analysis and Calorimetry》2009,97(1):149-152
Synthesis, spectroscopic characterization and thermal analysis of the [Pd(dmba)(Cl)(iso)] (1), [Pd(dmba)(NCO)(iso)] (2), [Pd(dmba)(N3)(iso)] (3) and [Pd(dmba)(Br)(iso)] (4) (dmba = N,N′-dimethylbenzylamine; iso = isonicotinamide) compounds are described in this work. The complexes were investigated by infrared
spectroscopy (IR), differential thermal analysis (DTA) and thermogravimetry (TG) and the residues of the thermal decomposition
were identified as Pdo by X-ray powder diffraction. The thermal stability order of the complexes varied as [Pd(dmba)(Cl)(iso)] (1) > [Pd(dmba)(Br)(iso)] (4) > [Pd(dmba)(NCO)(iso)] (2) > [Pd(dmba)(N3)(iso)] (3). 相似文献
18.
Wei Li Yun-Li Liu Jian Liu Huai-teng Zhang Shu-Zhong Zhan De-Rong Cao 《Transition Metal Chemistry》2011,36(3):255-260
The triazenide, 1-[(2-carboxyethyl)benzene]-3-[2-pyridine]triazene (HL), has been synthesized. In the presence of Et3N, the reaction of HL with Cu(OAc)2·H2O or CuCl2·2H2O gives the tetranuclear copper(II) complexes {Cu4(L)2(μ2-OH)2(OAc)4} 1 and {Cu4L4(μ4-O)Cl2} 2, respectively. The X-ray crystal structures of both complexes have been obtained. Magnetic studies indicate significant antiferromagnetic
coupling between the copper(II) centers for both complexes, with coupling constants (J) of −493.4 cm−1 for 1 and −165 cm−1 for 2. 相似文献
19.
Solvothermal synthesis and structures of three novel heterometallic microporous coordination polymers assembled from 2-hydroxy-nicotinic acid 总被引:1,自引:0,他引:1
Hua Hong Zou Shu Hua Zhang Yu Xiao Chao Feng Yin Guang Wang 《Structural chemistry》2011,22(1):135-140
Abstract
Three novel heterometallic microporous coordination polymers {M(Hnico)3M′} n (1, M = Co, M′ = K; 2, M = Ni, M′ = K; 3, M = Co, M′ = Na, Hnico is the anion of 2-hydroxy-nicotinic acid, where the proton is transferred from the phenolate hydroxy group to the nitrogen atom of imine pyridine ring) were synthesized by hydrothermal reaction between M(Ac)2·4H2O, M′OH and a multifunctional organic aromatic H2nico ligand and characterized by IR spectrum, elemental analysis, raman spectrum and the single crystal X-ray diffractions. In complexes 1–3, the M2+ ions linked three different Hnico ligand formed [M(Hnico)3]− subunit which further interlinked the six-coordination M′+ cation constructed 3D network. The network topology of 1–3 can be simplified a rare 3D (4,4)-connected (41263) net. 相似文献20.
Xing Chen Wen-Tao Yin Qian Huang Hong-Rong Zuo Jia-Rong Zhou Lin-Liang Yu Chun-Lin Ni Xue-Lei Hu 《Transition Metal Chemistry》2010,35(2):143-149
Two new salts, [BzTPP]2[Cu(mnt)2] (1) and [4NO2BzTPP]2[Cu(mnt)2] (2) (BzTPP+ = benzyltriphenylphosphonium and mnt2− = maleonitriledithiolate) have been prepared and characterized by elemental analyses, UV, IR, molar conductivity and single-crystal
X-ray diffraction. The single-crystal structure analysis shows that 1 crystallizes in the monoclinic space group P21/n, while 2 crystallizes in the triclinic space group P−1. The effects of weak intramolecular interactions such as C–H···O, C–H···S, C–H···N, C–H···Cu hydrogen bonds and p···π, π···π stacking interactions in the solids generate a 3D network structure. It is noted that the change in the molecular
topology of the counteraction when the 4-substituted group in the benzyl ring is changed from H to NO2 results in differences in the crystal system, space group, weak interactions and the stacking mode of the cations and anions
of 1 and 2. The magnetic susceptibilities of these salts measured in the temperature range 2.0 to 300 K show weak ferromagnetic coupling
features with θ = 2.05 × 10−2 K for 1 and 5.13 × 10−3 K for 2. 相似文献