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1.
M. O. Talismanova A. A. Sidorov G. G. Aleksandrov V. N. Charushin S. K. Kotovskaya V. P. Ananikov I. L. Eremenko I. I. Moiseeva 《Russian Chemical Bulletin》2008,57(1):47-55
The reactions of palladium(II) salts with 2-mercaptobenzimidazole (HL) and its 5,6-difluorinated derivative (HLF) were investigated. In the presence of hydrochloric acid, PdCl2 and K2PdCl4 react with HL and HLF in the ethanol—water and acetonitrile—water systems to form the mono-nuclear dicationic complexes [Pd(HL)4]Cl2 (1) and [Pd(LF)4]Cl2 (2). In the absence of HCl, the reactions afford the tetranuclear complex Pd4[(L)2(μ3-S,N-(L))2(μS,N-(L))4] (3). The reaction of triethylamine with an ethanolic solution of 3 leads to degradation of 3 and the formation of the lantern-type dinuclear complex Pd2[(μ2-(L)4] (4), in which the palladium atoms are in the nonequivalent coordination environment, PdN4 and PdS4. The reaction of K2PdCl4 with HL or HLF in the THF—water or acetonitrile—water systems (for the reaction with HLF) in the presence of Et3N produces the lantern-type dinuclear complexes Pd2[(μS,N′-(L3))4] and Pd2[(μ-S,N′-(LF))4] (5), in which the metal atoms are in the equivalent coordination environment (cis-PdN2S2).
Dedicated to Academician G. A. Tolstikov on the occasion of his 75th birthday.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 45–52, January, 2008. 相似文献
2.
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
3.
Abstract
A series of 1-D lanthanide coordination polymers [Ln(μ3-OH)(pybz)(pa)] n (Ln = Er (1), Tb (2), Gd (3), Hpybz = 4-pyridin-4-yl-benzoic acid, Hpa = 2-picolinic acid) based on [Ln4(μ3-OH)4] cluster units have been hydrothermally synthesized and characterized by single crystal X-ray diffraction, IR, elemental analysis, and thermogravimetric analysis. X-ray crystal structure analyses reveal that 1–3 are isomorphous with tetragonal space group P [`4] \overline{4} 21c and comprise tetranuclear Ln–O clusters, in which four Ln3+ centers are joined together by four μ3-bridging hydroxyl groups to form cubane-like [Ln4(μ3-OH)4]8+ cores that are further linked by four μ3-pa− ligands to produce 1-D chains along the c-axis. 相似文献4.
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
5.
R. L. Fernandes P. M. Takahashi R. C. G. Frem A. V. G. Netto A. E. Mauro J. R. Matos 《Journal of Thermal Analysis and Calorimetry》2009,97(1):123-126
The synthesis and thermal behavior of the new [Pd(fum)(bipy)]
n
·2nH2O (1), [Pd(fum)(bpe)]
n
·nH2O (2) and [Pd(fum)(pz)]
n
·3nH2O (3) {bipy = 4,4′-bipyridine, bpe = 1,2-bis(4-pyridyl)ethene and pz = pyrazine} fumarate complexes are described in this work
as well their characterization by IR and 13C CPMAS NMR spectroscopies. TG curves showed that the compounds released organic ligands and lattice water molecules in the
temperature range of 46–491 °C. In all the cases, metallic palladium was identified as the final residue. 相似文献
6.
Abstract
A new lanthanide coordination polymer, {[Yb4(μ 3 -OH)4(bpdc)4(H2O)6]}2·17(H2O) (1), which contains the tetranuclear lanthanide cluster of cubane-like [Yb4(μ 3 -OH)4]8+, was obtained by hydrothermal reaction. As building blocks, [Yb4(μ 3 -OH)4]8+ clusters were further assembled into two-dimensional network structure through the linking of 2,2′-bipyridine-3,3′-dicarboxylate (bpdc) with different four coordination modes. It is unprecedented that the adjacent [Yb4(μ 3 -OH)4]8+ clusters are in the arraying form of ···AABB···(Yb1–Yb4 unit as A and Yb5–Yb8 unit as B). The thermal stability and magnetic property of compound 1 were investigated further. 相似文献7.
N. N. Golovnev A. A. Leshok G. V. Novikova 《Russian Journal of Inorganic Chemistry》2010,55(2):291-293
The effect of acidity and equilibrium chloride ion concentration on the interaction of PdCl4
2- with cystine (H2CySS) in hydrochloric acid solutions was studied. Pd(H4CySS)Cl3+ complex was found to form at [Cl–] = 1.0, 0.5, or 0.25 mol/Linthe [H+] range from 0.10 to 1.00 mol/L; the relevant equilibrium constant was determined. Monodentate coordination of cystine to
palladium(II) through the sulfur atom was proposed on the basis of analysis of conditional stability constants as functions
of [Cl–] and [H+]. 相似文献
8.
Treatment of the triosmium hydrido cluster, [Os3(μ-H)2(CO)10], with one equivalent of [IrCp*Cl2]2 (Cp* = pentamethylcyclopentadiene) in refluxing THF afforded four osmium–iridium clusters, including [Os3Ir2(μ-CO)(μ-H)2(CO)9(Cp*)2] (1), [Os3IrCp*(μ-H)3(μ-Cl)(CO)9] (2), [Os3IrCp*(μ-H)(μ-Cl)(μ-CO)(CO)9] (3) and [Os2IrCp*(μ-H)(μ-Cl)(CO)7] (4), in moderate yields. The reactivity of complex 3 with hydrogen, carbon monoxide, and thallium hexafluorophosphate was studied. Complex 4 was found to react with [Os3(μ-H)2(CO)10] to give 2 and 3. All of the new compounds were characterized by conventional spectroscopic methods and single-crystal X-ray analysis.
This work is dedicated to Professor Frank Albert Cotton for his pioneering contributions to the chemistry of metal clusters 相似文献
9.
Abstract
Three new cadmium coordination polymers, [CdBr2(tmdp)2(μ-tmdp)2] n ·n(H2O) (1), [Cd(SCN)2(μ-tmdp)2] n ·2n(PhS) (2) and [Cd(SCN)2(μ-tmdp)2] n ·n(Ph2S2)·n(CH3CN) (3) (tmdp = 4,4′-trimethylenedipyridine), have been synthesized under solvothermal conditions and structurally characterized by single-crystal X-ray diffraction analysis. The geometry around cadmium is a slightly distorted octahedron with four tmdp and two Br- or SCN- ligands. Complex 1 represents a one-dimensional structure, whereas complexes 2 and 3 are two-dimensional coordination polymers. The rhombic channels of the coordination network of 2 and 3 are occupied by 1D polymeric (PhS) n and diphenyl disulfide (Ph2S2) molecules, respectively. The photoluminescent properties of coordination polymers 1–3 were investigated in solid state at room temperature. The TGA experiments showed that these three complexes were quite thermally stable. 相似文献10.
Juribašić M Bellotto L Traldi P Tušek-Božić L 《Journal of the American Society for Mass Spectrometry》2011,22(10):1815-1825
The mass spectrometric behavior of palladium(II) halide complexes of three types of quinolinylaminophosphonates, diethyl and
dibutyl esters of [α-anilino-(quinolin-2-yl)methyl]phosphonic (L1, L2), [α-anilino-(quinolin-3-yl)methyl]phosphonic (L3, L4), and [α-(quinolin-3-ylamino)-N-benzyl]phosphonic acid (L5, L6), was investigated under positive ion electrospray ionization conditions. Each type of ligand forms complexes with different
metal–ligand interactions. Mononuclear dihalide adducts cis-[Pd(L1/L2)X2] (1–4) and trans-[Pd(L3/L4)2X2] (5–8) as well as dinuclear tetrahalide complexes [Pd2(L5/L6)3X4] (9–12) (X = Cl, Br) are formed by metal bonding either through the quinoline or both the quinoline and amino nitrogen atoms. The
sodiated molecule [M + Na]+ is observed in the mass spectra of all the complexes, and its abundance as well as the fragmentation pathway depend on the
type of the complex. In the cis complexes (1–4) the initial decomposition goes under two fragmentation routes: those in which the sodium molecular adduct sequentially loses
halides HX/NaX and those in which this loss is in the competition with the loss of dialkyl phosphite. The predominant pathways
for decomposition of trans dihalide (5–8) and tetrahalide (9–12) complexes include three competitive reactions; the loss of halides, dialkyl phosphites and the intact phosphonate ligand
molecule and its fragments formed by ester dissociation or complete loss of the phosphonate ester moiety. A series of acetonitrile
adducts and cluster ions derived from dimolecular clusters [2M + Na]+ were also detected. The most important fragmentation patterns are rationalized and supported by the MS
n
studies. 相似文献
11.
Xi-ke gao Jian-min dou Da-cheng li Feng-ying dong Da-qi wang 《Journal of inclusion phenomena and macrocyclic chemistry》2005,53(1-2):111-119
Five novel 2,3-naphtho crown ether group 10 metal bis(dithiolate) complexes, [Na(N15C5)2]2[Pd(mnt)2] (1), [Na(N15C5)]2[Pd(i-mnt)2] (2) and [K(N18C6)]2[M(i-mnt)2] (3
5) (where mnt = 1,2-dicyanoethylene-1,2-dithiolate, i-mnt = 1,1-dicyanoethylene-2,2-dithiolate and M = Ni, Pd, Pt for complexes
3–5, respectively), have been synthesized and characterized by elemental analysis, FT-IR, UV–Visible spectra and single crystal
X-ray diffraction. X-ray diffraction analyses reveal that complexes 1 and 2 have different structural features while complexes 3–5 are structurally isomorphous. Complex 1 consists of two [Na(N15C5)2]+ sandwich complex cations and one [Pd(mnt)2]2− anion, affording a zero-dimensional structure. For 2, the [Na(N15C5)]+ mono-capped complex cations act as the bridges linking the [Pd(i-mnt)2]2− anions into a 1D infinite chain through Na–N interactions and SȮFC and SȮFπ interactions are observed in the resulting chain.
Complexes 3–5 all consist of two [K(N18C6)]+ complex cations and one [M(i-mnt)2]2− (M = Ni, Pd or Pt) anion and the complex molecules are linked into␣1D␣chains by the bridging K–O(ether) interactions between
the adjacent [K(N18C6)]+ units. What’s novel is that the resulting chains are assembled into novel 2D networks through interchain π–π stacking interactions
between the neighboring naphthylene moieties of N18C6. The stack model of naphthylene group in complexes 3–5 is discussed. 相似文献
12.
Carolina V. Barra Fillipe V. Rocha Adelino V. G. Netto 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):489-494
This study describes the synthesis, IR, 1H, and 13C{1H} NMR spectroscopic as well the thermal characterization of the new palladium(II) pyrazolyl complexes [PdCl2(HmPz)2] 1, [PdBr2(HmPz)2] 2, [PdI2(HmPz)2] 3, [Pd(SCN)2(HmPz)2] 4 {HmPz = 4-methylpyrazole}. The residues of the thermal decomposition were identified as Pd0 by X-ray powder diffraction. From the initial decomposition temperatures, the thermal stability of the complexes can be ordered
in the sequence: 1 > 2 > 4 ≈ 3. The cytotoxic activities of the complexes and the ligand were investigated against two murine cancer cell lines: mammary
adenocarcinoma (LM3) and lung adenocarcinoma (LP07) and compared to cisplatin under the same experimental conditions. 相似文献
13.
Ji-Cai Zhang Xiao-Shuang Zhou Xiao-Ling Wang Xiao-Fang Li Zhong-Lu You 《Transition Metal Chemistry》2011,36(1):93-98
Three azido-bridged copper(II) complexes, [Cu2(L1)2(μ1,1,3-N3)2]
n
·2nH2O (1), [Cu4(L2)4(μ1,1-N3)2(μ1,1,3-N3)2]
n
(2), and [Cu2(L3)2(μ1,1-N3)2] (3), where L1, L2, and L3 are the deprotonated forms of 4-bromo-2-[(2-methylaminoethylimino)methyl]phenol (HL1), 4-bromo-2-[(2-ethylaminoethylimino)methyl]phenol (HL2), and 4-bromo-2-[(2-isopropylaminoethylimino)methyl]phenol (HL3), respectively, have been prepared and structurally characterized by single-crystal X-ray diffraction analysis and IR spectra.
The slight differences in the terminal groups of the Schiff bases lead to different bridging modes of the azido groups. 相似文献
14.
Pradip Kumar Ghosh Harasit Kumar Mandal Ambikesh Mahapatra 《Transition Metal Chemistry》2010,35(6):679-687
Interaction of adenine (A) with dichloro-[1-alkyl-2-(α-naphthylazo)imidazole] palladium(II) [Pd(α-NaiR)Cl2], 1 and dichloro-[1-alkyl-2-(β-naphthylazo)imidazole] palladium(II) [Pd(β-NaiR)Cl2], 2 {where R=Me (a), Et (b) or Bz (c)} in MeCN-water (50% v/v) medium to yield [{1-alkyl-2-(α-naphthylazo)imidazole}(adenine)]palladium(II) perchlorates (3a, 3b, 3c) and [{1-alkyl-2-(β-naphthylazo)imidazole}(adenine)]palladium(II) perchlorates (4a, 4b, 4c) was studied. The products were characterized by physico-chemical and spectroscopic methods. The reaction kinetics were second
order overall, being first order in both the Pd(II) complex and adenine. The effect of adding chloride was consistent with
rate-limiting dissociation of chloride from the complex. Thermodynamic parameters were determined from temperature variation
experiments. The second-order rate constant k
2
corroborates with the experimental Δ‡H° values, while the negative values of Δ‡S° indicate that the reaction proceeds through an associative inner sphere mechanism. 相似文献
15.
Aliakbar Dehno Khalaji Smail Triki Debasis Das 《Journal of Thermal Analysis and Calorimetry》2011,103(3):779-783
New 1D-chain copper(I) complex [Cu2(μ-(3,4,5-MeO-ba)2bn)(μ-I)2]
n
(1), where (3,4,5-MeO-ba)2bn = N,N′-bis(3,4-dimethoxybenzylidene)-butane-1,4-diamine, involving a new bidentate Schiff-base containing a flexible spacer (=N–C–C–C–C–N=)
has been synthesized and characterized by elemental analyses (CHN) and FT-IR spectroscopy. The crystal structure of 1 was determined from single-crystal X-ray diffraction analyses and shows the (3,4,5-MeO-ba)2en acts as a bridging ligand with the nitrogen atoms of the two imine functions and leading to the dinuclear [Cu2((μ-(3,4,5-MeO-ba)2en)] groups. Such dinuclear [Cu2((μ-(3,4,5-MeO-ba)2en)] groups are bridged by two iodine anions [(μ-I)2] to form a neutral 1D-chain copper(I) iodide coordination polymer. The coordination polyhedron about the copper(I) center
in 1 is best described as a distorted trigonal planar. Thermogravimetric analyses reveal the thermal stability and decomposition
pattern of 1. 相似文献
16.
S. E. Nefedov N. Yu. Kozitsyna N. S. Akhmadullina N. V. Cherkashina M. N. Vargaftik I. I. Moiseev 《Russian Journal of Inorganic Chemistry》2011,56(3):357-374
The reactions of palladium(II) acetate with neodymium(III) and cerium(III) acetates in acetic acid containing a specified
amount of water have been studied. The following homo- and heterometallic complexes have been synthesized and characterized
by X-ray diffraction: Nd2(μ-OOCMe)2(μ,η2-OOCMe)2(η2-OOCMe)2(HOOCMe)2(OH2)2 · 4HOOCMe, [Pd(μ-OOCMe)4Ce(OH2)2(μ,η2-OOCMe)]2 · 2HOOCMe · 6H2O, [Pd(μ-OOCMe)4Ce(OH2)2(μ,η2-OOCMe)]2 · 14H2O, [Pd(μ-OOCMe)4M(HOOCMe)2(OH2)2]+ [Pd(μ-OOCMe)4M(μ-OOCMe)4Pd]− · 2MeCOOH · 1.5H2O (M = Nd, Ce), and {[Pd(μ-OOCMe)4Ce(OOCMe)4]2 [Pd4(μ-OOCMe)4]2(μ4-O)8CePd4}(OH)3 · 27H2O. From kinetic and structural data and optical spectra of reaction solutions, the conclusion was drawn that hydrolytic processes
play a decisive role in complexation reactions. 相似文献
17.
S. I. Orysyk L. N. Rybachuk V. I. Pekhnyo V. V. Orysyk 《Russian Journal of Inorganic Chemistry》2011,56(11):1747-1751
New Pd(II) complexes with 1-allyl-3-(2-pyridyl)thiourea (APTU) of the formulas [Pd(C9H11N3S)Cl2] (I) and [Pd(C9H11N3S)2]Cl2 (II) were obtained and examined by UV-Vis, IR, and 1H NMR spectroscopy. The conditions for the complexation reactions were optimized.
The instability constants and molar absorption coefficients of these complexes were calculated. Comparison of the characteristic
bands in the UV-Vis and IR spectra of the complexes and free APTU revealed that the ligand in both complexes is coordinated
to the metal atom in the thione form in the bidentate chelating mode through the S atom of the thiourea group and the pyridine
N atom. In the UV-Vis spectra of the complexes, the charge transfer bands (π → π* Py) and n → π* (C=NPy), (C=S) experience hypsochromic shifts by 450–470 cm−1 caused by the coordination of APTU to the metal ion, which gives rise to ligand-metal charge-transfer bands (C=NPy → Pd, n → π* (C=S)) and (SPd). The protons in the 6-, 4-, and 3-positions of the pyridine ring and the thiourea NH proton in the
chelate ring are most sensitive to the complexation. 相似文献
18.
Zhi-Feng Ye Zhi-Gang Pan Wei-Jiang He Xian-Fa Shi Long-Gen Zhu 《Journal of inclusion phenomena and macrocyclic chemistry》2001,40(1-2):89-93
Three new thiacalix[4]arene derivatives, 5,11,17,23-tetra-tert-butyl-25,27-di(2-hydroxyethoxy)-26,28-dihydroxythiacalix-{}[4]arene (2), 5,11,17,23-tetra-tert-25, 26,27,28-tetrakis[(methylcarboxyl)methoxy]thiacalix[4]arene (3),5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrakis(2-hydroxy-1-propanoxy)thiacalix[4]arene (4), were synthesized for the first time. The coordination properties of thiacalix[4]arene(1) and its derivatives (2 and 4) were investigated by detecting the interactions betweenthese compounds and two palladium complexes, cis-[Pd(en)(H2O)2]2+ and cis-[Pd(dtco-3-OH)(H2O)2]2+, by means of electrospray ionization mass spectrometry (ESI-MS) technique. 相似文献
19.
V. V. Sharutin V. S. Senchurin O. K. Sharutina N. V. Somov A. V. Gushchin 《Russian Journal of Coordination Chemistry》2011,37(11):854-860
The complexes [Bu4N]2+[PtBr6]2− (I), [Ph4P]2+[PtBr6]2− (II), and [Ph3(n-Am)P]2+ (III) are synthesized by the reactions of tetrabutylammonium bromide, tetraphenylphosphonium bromide, and triphenyl(n-amyl)-tetraphenylphosphonium bromide, respectively, with potassium hexabromoplatinate (mole ratio 2: 1). After recrystallization
from dimethyl sulfoxide, complexes I, II, and III transform into [Bu4N]+[PtBr5(DMSO)]− (IV), [Ph4P]+[PtBr5(DMSO)]− (V), and [Ph3(n-Am)P]+[PtBr5(DMSO)]− (VI). According to the X-ray diffraction data, the cations of complexes IV–VI have a slightly distorted tetrahedral structure. The N-C and P-C bond lengths are 1.492(7)–1.533(6) and 1.782(10)–1.805(10)
?, respectively. The platinum atoms in the mononuclear anions are hexacoordinated. The dimethyl sulfoxide ligands are coordinated
with the Pt atom through the sulfur atom (Pt-S 2.3280(18)–2.3389(11) ?). The Pt-Br bond lengths are 2.4330(6)–2.4724(6) ?. 相似文献
20.
S. P. Khranenko I. A. Baidina N. V. Kuratieva S. A. Gromilov 《Journal of Structural Chemistry》2009,50(1):166-169
A new Pd nitrate complex KCs[Pd(NO3)4]·0.5H2O is synthetized. Its crystal structure contains isolated complex anions [Pd(NO3)4]2−, cations K+, Cs+, and crystallization water. Square-planar coordination around Pd is achieved by oxygen atoms of monodentate nitrate ligands.
The coordinated nitrate ligands are all oriented in the same way, in a “basket”-like arrangement. The coordination around
Pd is completed to 4+1 by forming Pd...Pd contacts of 3.564 ?.
Original Russian Text Copyright ? 2009 by S. P. Khranenko, I. A. Baidina, N. V. Kuratieva, and S. A. Gromilov
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 1, pp. 173–176, January–February, 2009. 相似文献