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1.
A bioactive Schiff base HL i.e. 2‐hydroxy‐benzoic acid(3,4‐dihydro‐2H ‐naphthalen‐1‐ylidene)‐hydrazide was synthesized by reacting equimolar amount of salicylic acid hydrazide and 1‐tetralone. Co(II), Ni(II) and Zn(II) complexes of ligand HL was synthesized in 1:1 and 1:2 molar ratio of metal to ligand. The structure of the synthesized ligand and metal complexes was established by elemental analysis, molar conductance, magnetic susceptibility measurements, electronic, IR and EPR spectral techniques. For determining the thermal stability the TGA has been done. In DFT studies the geometries of Schiff bases and metal complexes were fully optimized with respect to the energy using the 6–31 + g(d,p) basis set. Spectral data reveal that ligand behave uninegative tridentate in ML complexes and uninegative bidentate in ML2 complexes. On the basis of characterization octahedral geometry has been assigned for Co(II) and Ni(II) complexes, while tetrahedral for Zn(II) complexes. Antibacterial activity of the synthesized compounds were evaluated against Staphylococcus aureus , Bacillus subtilis, Escherichia coli , Xanthomonas campestris and Pseudomonas aeruginosa and the results revealed that metal complexes show enhanced activity in comparison to free ligand.  相似文献   

2.
Assemblies of pyrazine‐2,3‐dicarboxylic acid and CdII in the presence of bis(1,2,4‐triazol‐1‐yl)butane or bis(1,2,4‐triazol‐1‐yl)ethane under ambient conditions yielded two new coordination polymers, namely poly[[tetraaqua[μ2‐1,4‐bis(1,2,4‐triazol‐1‐yl)butane‐κ2N4:N4′]bis(μ2‐pyrazine‐2,3‐dicarboxylato‐κ3N1,O2:O3)dicadmium(II)] dihydrate], {[Cd2(C6H2N2O4)2(C8H12N6)(H2O)4]·2H2O}n, (I), and poly[[diaqua[μ2‐1,2‐bis(1,2,4‐triazol‐1‐yl)ethane‐κ2N4:N4′]bis(μ3‐pyrazine‐2,3‐dicarboxylato‐κ4N1,O2:O3:O3′)dicadmium(II)] dihydrate], {[Cd2(C6H2N2O4)2(C6H8N6)(H2O)2]·2H2O}n, (II). Complex (I) displays an interesting two‐dimensional wave‐like structure and forms a distinct extended three‐dimensional supramolecular structure with the help of O—H...N and O—H...O hydrogen bonds. Complex (II) has a three‐dimensional framework structure in which hydrogen bonds of the O—H...N and O—H...O types are found.  相似文献   

3.
Four new complexes of [Cu(bpm)(ox)(H2O)] ( 1 ), [Cu(tpd)(dca)(H2O)] ( 2 ), [Cu(bppz)(N3)2] ( 3 ), and [Cu(bpm)21,3‐N3)(N3)] ( 4 ) (bpm = 2,2′‐bipyrimidine, bppz = 2,3‐bis(2‐pyridyl)pyrazine, tpd = 4‐terpyridone, dca = dicyanamide, ox = oxalate) have been prepared and characterized by X‐ray single‐crystal analysis and variable‐temperature magnetic measurements. Compounds 1–4 are essentially mononuclear Cu(II) complexes. However, in complex 1 , Cu(II) it was found that intermolecular hydrogen bonding through between H2O and ox formed 1‐D chain structure. In complex 2 it was found that the hydrogen bonding between H2O and tpd of the next molecule led to for a binuclear Cu(II) complex. In complex 3 , two nitrogen atoms, one of the pyridyl group of bppz and one of N3? ligands, are weakly coordinated to neighbor Cu(II) ion thus leading to formation of a 1‐D chain structure. In complex 4 , one nitrogen atom of terminated N3? is weakly coordinated to the neighbor Cu(II) site to form a 1‐D polymeric structure. The magnetic susceptibility measurements indicate that complex 1 and 4 exhibit a weak antiferromagnetic interaction whereas a ferromagnetic coupling has been established for complexes 2 and 3 .  相似文献   

4.
In the present paper novel column solid phase extraction procedure was developed for the determination of Cd(II) and Pb(II) in cows', goats', ewes', buffalos' and humans' milk samples using newly synthesized reagent 2,2′‐DPED3P (2,2′‐{[1,2‐diphenylethane‐1,2‐diylidene]dinitrilo}diphenol) for preconcentration and separation prior to differential pulse polarography using amberlite XAD‐2 in the ranges of pH 4.0–5.0. The sorbed elements were subsequently eluted with 10 mL of 2 M HCl elutes were analysed by differential pulse polarography (DPP). The interference of foreign ions has also been studied. Effects of various instrumental parameters are investigated and received conditions are optimized. The total metal concentration of the milk samples in the study area were in the following ranges 0.030–0.090 μg L?1 of Cd(II), 0.009–0.026 μg L?1 of Pb(II) respectively. The limits of detections were found to be 0.020 and 0.024 μg L?1 for Cd(II) and Pb(II) respectively by applying a preconcentration factor ~40. The proposed enrichment method was applied successfully for the determination of metal ions in cows', goats', ewes', buffalos' and humans' milk samples.  相似文献   

5.
Seven new μ‐oxamido copper(II)‐lanthanide(III) heterobimetalic complexes described by the formula Cu(obbz) Ln‐(Ph‐phen)2NO3(Ln = La, Nd, Eu, Gd, Tb, Ho, Er), where obbz denotes the oxamidobis(benzoato) and Ph‐phen represents 5‐phenyl‐1, 10‐phenanthroline, have been synthesized and characterized by the elemental analyses, spectroscopic (IR, UV, ESR) studies, magnetic moments (at room temperature) and molar conductivity measurement. The temperature dependence of the magnetic susceptibility of Cu(obbz)Gd(Ph‐phen)2NO3 complex has been measured over the range 4.2–300 K. The least‐squares fit of the experimental susceptibilities based on the spin Hamiltonian operator, ? = ?2 J?1·?2, yielded J= +1.28 cm?1, a weak ferromagnetic coupling, A plausible mechanism for a ferromagnetic coupling between Gd(III)‐Cu(II) is discussed in terms of spin‐polarization.  相似文献   

6.
Monomeric and Polymeric Dimethylaminothiosquarato Complexes: The Crystal Structures of Nickel(II), Cobalt(II), Silver(I), Platinum(II), Gold(I), Mercury(II) and Lead(II) Dimethylaminothiosquarates The ligand 2‐dimethylamino‐3, 4‐dioxo‐cyclobut‐1‐en‐thiolate, Me2N‐C4O2S (L) forms neutral and anionic complexes with nickel(II), cobalt(II)‐, silver(I)‐, platinum(II)‐, gold(I)‐, mercury(II)‐ and lead(II). According to the crystal structures of seven complexes the ligand is O, S‐chelating in [Ni(L)2(H2O)2]·2 H2O, [Co(L)2(CH3OH)2] and (with limitations) in [Pb(L)2·DMF]. In the remaining compounds the ligand behaves essentially as a thiolate ligand. The platinum, gold and mercury complexes [TMA]2[Pt(L)4], [TMA] [Au(L)2] and [Hg(L)2] are monomeric. In [TMA][Ag2(L)3]·5.5 H2O a chain‐like structure was found. In the asymmetric unit of this structure eight silver ions, with mutual distances in the range 2.8949(4) to 3.1660(3)Å, are coordinated by twelve thiosquarato ligands. [Pb(L)2·DMF] has also a polymeric structure. It contains a core of edge‐bridged, irregular PbS4 polyhedra. TMA[Au(H2NC4O2S)2] has also been prepared and its structure elucidated.  相似文献   

7.
The stoichiometric reaction of copper(II) hydroxycarbonate, iminodiacetic acid (H2IDA = HN(CH2CO2H)2) and α‐picolinamide (pya) in water yields crystalline samples of (α‐picolinamide)(iminodiacetato)copper(II) dihydrate, [Cu(IDA)(pya)] · 2 H2O ( 1 ). The compound was characterised by thermal (TG analysis with FT‐IR study of the evolved gasses), spectral (IR, electronic and ESR spectra), magnetic and single crystal X‐ray diffraction methods. It crystallises in the triclinic system, space group P1, a = 8.8737(4), b = 10.23203(5), c = 15.7167(11) Å, α = 77.61(1)°, β = 103.89(1)°, γ = 80.32(1)°, Z = 4, final R1 = 0.056. The asymmetric unit contains two crystallographic independent molecules but chemically very similar ones. The CuII atom exhibits a square base pyramidal coordination (type 4 + 1). pya acts as N,O‐bidentate ligand supplying two among the four closest donor atoms of the metal [averaged bond distances (Å): Cu–N = 1.982(2), Cu–O(amide) = 1.972(2)]. IDA plays a N,O,O′‐terdentate chelating role [averaged bond distances (Å): Cu–N = 2.004(3), Cu–O = 1.941(2) and Cu–O = 2.242(2)]. The coordinating behaviour of pya in 1 is discussed on the basis of its N,O‐bidentate chelating role and the preference of the ‘Cu‐iminodiacetato' moiety [Cu(IDA)] to link the N‐heterocyclic donor of pya in trans versus the Cu–N(IDA) bond. Consistently the ligand pya is able to impose a fac‐chelating configuration to IDA one around the copper(II) as previously has been reported to mixed‐ligand complexes having a 1/1/2 CuII/IDA/N(heterocyclic) donor ratio or a closely related 1/1/1/1 CuII/IDA/N(heterocyclic)/N(aliphatic) one.  相似文献   

8.
顾文秀  夏文水 《中国化学》2006,24(10):1458-1461
A novel synthesis of the functional carbohydrate 2-amino-2-deoxy-D-gluconic acid was introduced and itscomplex formation with Cu(Ⅱ)was investigated to obtain the stability constant for its further applications to thefood and pharmaceutical industries.The equilibrium was investigated by spectrophotometric measurements andprocessed by dual-series linear regression method.Results:the yield of 2-amino-2-deoxy-D-gluconic acid is 70%.The complexation molar ratio is 1:2,the molar apsorptivity of the complex is 39.906 L·mol~(-1)·cm~(-1) at 630 nm,and the stability constant β_n is 6.24×10~5.  相似文献   

9.
Four new copper (II)‐manganese (II) heterobinuclear complexes bridged byN, N'‐bis[2‐(dimethylamino)ethyl)]oxamido dianion (dmoxæ) and end‐capped with 1, 10‐phenanthroline (phen), 5‐methyl‐1, 10‐phenanthroline (Mephen), diaminoethane (en) or 1,3‐di‐aminopropane (pn). respectively, namely, [Cu(dmoxae)MnL2] (CIO4)2 (L=phen, Mephen, en, pn), have been synthesized and characterized by elemental analyses, IR, electronic spectral studies, and molar conductivity measurements. The electronic reflectance spectrum indicates the presence of spin exchange‐coupling interaction between bridged copper(II) and manganese (II) ions. The cryomagnetic measurements (4.2‐300 K) of [Cu(dmoxae)Mn(phen)2](CIO4)2 (1) and [Cu(dmoxae)Mn(Mephen)2](CIO4)2(2) complexes demonstrated an antiferromagnetic interaction between the adjacent manganese(II) and copper (II) ions through the oxamido‐bridge within each molecule. On the basis of spin Hamiltonian, H= ‐ 2JS1. S2. the magnetic analysis was carried out for the two complexes and the spin‐coupling constant (J) was evaluated as ?35.9 cm?1 for 1 and ‐ 32.6 cm?1 for 2. The influence of methyl substitutions in the amine groups of the bridging ligand on magnetic interactions between the metal ions of this kind of complexes is also discussed.  相似文献   

10.
Functionalized acid amides are widely used in biology, medicine, environmental chemistry and many other areas. Among them, pyridine‐substituted amides, in particular N‐(pyridin‐2‐yl)acetamide and its derivatives, play an important role due to their excellent chelating properties. The donor properties of these ligands can be effectively modified by introducing electron‐donating substituents (e.g. alkyl groups) into the heterocycle. On the other hand, substituents in the α‐position of the pyridine ring can create steric hindrance, which significantly influences the coordination number and geometry. To achieve a better understanding of these effects, copper(II) complexes with sterically demanding N‐(6‐methylpyridin‐2‐yl)acetamide ligands (L ) and monoanions of different size, shape and coordination ability have been chosen as model compounds. The crystal structures of three new compounds, bromidobis[N‐(6‐methylpyridin‐2‐yl‐κN )acetamide‐κO ]copper(II) bromide, [CuBr(C8H10N2O)]Br, (I), aquabis[N‐(6‐methylpyridin‐2‐yl‐κN )acetamide‐κO ]copper(II) dinitrate, [Cu(C8H10N2O)(H2O)](NO3)2, (II), and aquabis[N‐(6‐methylpyridin‐2‐yl‐κN )acetamide‐κO ]copper(II) bis(perchlorate), [Cu(C8H10N2O)(H2O)](ClO4)2, (III), have been determined by single‐crystal X‐ray diffraction analysis. It has been shown that the presence of the 6‐methyl group results in either a distorted square‐pyramidal or a distorted trigonal–bipyramidal coordination geometry around the CuII centres instead of the typical octahedral geometry observed when the methyl substituent is absent or occupies any other position on the pyridine ring. Moreover, due to the steric hindrance provided by the L ligands, only the bromide ligand, the smallest of the series, enters into the first coordination sphere of the CuII ion in (I). In (II) and (III), the vacant coordination site of the CuII ion is occupied by a water molecule, while the nitrate and perchlorate anions are not involved in coordination to the metal centre. The structures of (I)–(III) are characterized by the presence of one‐dimensional infinite chains formed by hydrogen bonds of the types N—H…Br [in (I)], N—H…O and O—H…O [in (II) and (III)] between the amide groups of the L ligands, the coordinated water molecules and the uncoordinated anions. The hydrogen‐bonded chains are further interconnected through π–π stacking interactions between the pyridine rings of the L ligands, with approximate interplanar separations of 3.5–3.6 Å.  相似文献   

11.
A new and convenient method for the preparation of 2‐aryl‐2,3‐dihydro‐1,8‐naphthyridin‐4(1H)‐ones 4 has been developed. Thus, N‐{3‐[(2E)‐3‐arylprop‐2‐enoyl]pyridin‐2‐yl}‐2,2‐dimethylpropanamides 3 are synthesized from commercially available pyridin‐2‐amine using an easily performed three‐step sequence and are subjected to cyclization with deprotection under acidic conditions in H2O to give the desired products. Similarly, 2‐aryl‐2,3‐dihydro‐1,7‐naphthyridin‐4(1H)‐ones 8 and 2‐aryl‐2,3‐dihydro‐1,6‐naphthyridin‐4(1H)‐ones 12 can be prepared from pyridin‐3‐amine and pyridin‐4‐amine, respectively.  相似文献   

12.
A one step synthesis protocol for the conversion of heteroylthiosemicarbazides and 2,3‐dichloro‐1,4‐naphthoquinone to naphtho[2,3‐d]thiazoles, naphtho[2,3‐e][1,3,4]thiadiazines as well as bis(naphtho[2,3‐d]thiazolyl)copper(II) derivatives is described. The products were conclusively confirmed by single crystal X‐ray analyses. A mechanism for the formation of the products is presented.  相似文献   

13.
Heteroleptic Ru(II) complexes were designed based on 4,4′‐bis((E)‐styryl)‐2,2′‐bipyridine (bsbpy) as an ancillary ligand for dye‐sensitized solar cells (DSSCs), and those Ru(II) sensitizers, [Ru(L)(bsbpy)(NCS)2][TBA] (TBA; tetrabutylammonium), were synthesized according to a typical one‐pot reaction of [RuCl2(p‐cymene)]2 with the corresponding anchoring ligands (where L = 4,4′‐dicarboxy‐2,2′‐bipyridine (dcbpy), 4,4′‐bis((E)‐carboxyvinyl)‐2,2′‐bipyridine (dcvbpy), 4,7‐dicarboxy‐1,10‐phenanthroline (dcphen), or 4,7‐bis((E)‐carboxyvinyl)‐1,10‐phenanthroline (dcvphen)). The new Ru(II) dyes, [Ru(L)(bsbpy)(NCS)2][TBA] that incorporated vinyl spacer(s) into ancillary and/or anchoring ligand displayed red‐shifted bands over the overall UV/VIS region relative to the absorption spectra of N719 . A combination of bsbpy ancillary and dcphen anchoring ligand showed the best result for the overall power conversion efficiency (η); i.e., a DSSC fabricated with [Ru(dcphen)(bsbpy)(NCS)2][TBA] exhibited a power conversion efficiency (η) of 2.98% (compare to N719 , 4.82%).  相似文献   

14.
An α‐diimine Pd(II) complex containing chiral sec‐phenethyl groups, {bis[N,N′‐(4‐methyl‐2‐sec‐phenethylphenyl)imino]‐2,3‐butadiene}dichloropalladium (rac‐ C1 ), was synthesized and characterized. rac‐ C1 was applied as an efficient catalyst for the Suzuki–Miyaura cross‐coupling reaction between various aniline halides and arylboronic acid in PEG‐400–H2O at room temperature. Among a series of aniline halides, rac‐ C1 did not catalyze the cross‐coupling of aniline chlorides and fluorides but efficiently catalyzed the cross‐coupling of aniline bromides and iodides with phenylboronic acid. The catalytic activity reduced slightly with increasing steric hindrance of the aniline bromides. The complexes {bis[N,N′‐(4‐fluoro‐2,6‐diphenylphenyl)imino]‐2,3‐butadiene}dichloropalladium and {bis[N,N′‐(4‐fluoro‐2,6‐diphenylphenyl)imino]acenaphthene}dichloropalladium were also found to be efficient catalysts for the reaction. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

15.
A new and facile method for the general preparation of 3‐alkoxy‐2,3‐dihydro‐1H‐isoindol‐1‐ones has been developed. Thus, the reaction of 2‐(azidomethyl)benzoates with NaH affords, after workup with H2O, 3‐alkoxy‐2,3‐dihydro‐1H‐isoindol‐1‐ones 2 . 2‐Substituted 3‐alkoxy‐2,3‐dihydro‐1H‐isoindol‐1‐ones 4 can be obtained by adding alkyl halides prior to workup with H2O.  相似文献   

16.
Eight new two‐ligand complexes of copper(II) with 1,10‐phenanthroline and one of four different α‐hydroxy‐carboxylic acids (glycolic, lactic, mandelic and benzylic) were prepared. The complexes of general formula [Cu(HL)2(phen)] · nH2O (HL = monodeprotonated acid) ( 1 – 4 ) were characterized by elemental analysis, IR, electronic and EPR spectroscopy, magnetic measurements and thermo‐gravimetric analysis. The complexes of general formulae [Cu(HL)(phen)2](HL) · H2L · nSolv [ 1 a (HL = HGLYO, n = 1, Solv = MeCN) and 3 a (HL = HMANO, n = 0)] and [Cu(L)(phen)(OH2)] · nH2O [ 2 a (L = LACO2–, n = 4) and 4 a (L = BENO2–, n = 2)] were characterized by X‐ray diffractometry. In all these latter a pentacoordinated copper atom has a basically square pyramidal coordination polyhedron, the distortion of which towards a trigonal bipyramidal configuration has been evaluated in terms of the parameter τ. In 1 a and 3 a there are three forms of α‐hydroxycarboxylic acid: a monodentate monoanion, a monoanionic counterion, and a neutral molecule lying in the outer coordination sphere; in 2 a and 4 a the α‐hydroxycarboxylic acid is a bidentate dianion coordinating through carboxyl and hydroxyl oxygens.  相似文献   

17.
A novel Cu (II) Schiff‐base complex immobilized on core‐shell magnetic Fe3O4 nanoparticles (Fe3O4@SPNC) was successfully designed and synthesized. The structural features of these nanoparticles were studied and confirmed by using various techniques including FT‐IR spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy‐dispersive X‐ray spectroscopy (EDS), vibrating sample magnetometer (VSM), X‐Ray diffraction (XRD), wavelength dispersive X‐ray spectroscopy (WDX), and inductively coupled plasma (ICP). These newly synthesized nanoparticles have been used as efficient heterogeneous catalytic system for one‐pot multicomponent synthesis of new pyrano[2,3‐b]pyridine‐3‐carboxamide derivatives. Notably, the catalyst could be easily separated from the reaction mixture by using an external magnet and reused for several successive reaction runs with no significant loss of activity or copper leaching. The present protocol benefits from a hitherto unreported MNPs‐immobilized Cu (II) Schiff‐base complex as an efficient nanocatalyst for the synthesis of newly reported derivatives of pyrano[2,3‐b]pyridine‐3‐carboxamide from one‐pot multicomponent reactions.  相似文献   

18.
The synthesis of potassium (η2‐4‐allyl‐2‐methoxyphenol)trichloridoplatinate(II), K[PtCl3(C10H12O2)], ( 1 ), starting from Zeise's salt and Ocimum sanctum L. oil has been optimized. Starting from ( 1 ), three new platinum(II) complexes, namely (η2‐4‐allyl‐2‐methoxyphenol)chlorido(2‐methylquinolin‐8‐olato‐κ2N ,O )platinum(II), ( 2 ), (η2‐4‐allyl‐2‐methoxyphenol)chlorido(5‐nitroquinolin‐8‐olato‐κ2N ,O )platinum(II), ( 3 ), and (η2‐4‐allyl‐2‐methoxyphenol)chlorido(5,7‐dichloroquinolin‐8‐olato‐κ2N ,O )platinum(II), [Pt(C9H4Cl2NO)Cl(C10H12O2)], ( 4 ), containing eugenol and a quinolin‐8‐ol derivative (R‐OQ), have been synthesized and characterized by elemental analyses, MS, IR, 1H NMR and NOESY spectra. For ( 1 ) and ( 4 ), single‐crystal X‐ray diffraction studies were also carried out. Complexes ( 2 )–( 4 ) show good inhibiting abilities on three human cancer cell lines, i.e. KB, Hep‐G2 and LU, with IC50 values of 1.42–17.8 µM . Complex ( 3 ) gives an impressively high activity against KB, Hep‐G2, LU and MCF‐7, with IC50 values of 1.42–4.91 µM , which are much lower than those of cisplatin and some other platinum(II) complexes.  相似文献   

19.
Three new μ‐oxamido‐bridged heterodinuclear copper (II)‐chromium (III) complexes formulated [Cu(Me2oxpn)Cr‐(L)2](NO3)3, where Me2oxpn denotes N,N'‐bis(3‐amino‐2, 2‐dimethylpropyl)oxamido dianion and L represents 5‐methyl‐1,10‐phenanthroline (Mephen), 4,7‐diphenyl‐1,10‐phenanthroline (Ph2phen) or 2,2′‐bipyridine (bpy), have been synthesized and characterized by elemental analyses, IR and electronic spectral studies, magnetic moments of room‐temperature and molar conductivity measurements. It is proposed that these complexes have oxamido‐bridged structures consisting of planar copper (II) and octahedral chromium (III) ions. The variable temperature magnetic susceptibilities (4.2–300 K) of complexes [Cu(Me2oxpn)Cr(Ph2phen)2](NO3)3 (1) and [Cu(Me2oxpn)Cr(Mephen)2] (NO3)3 (2) were further measured and studied, demonstrating the ferromagnetic interaction between the adjacent chromium (III) and copper (II) ions through the oxamido‐bridge in both complexes 1 and 2. Based on the spin Hamiltonian, ? = ‐ 2J?1 · ?2, the exchange integrals J were evaluated as + 21.5 an?1 for 1 and + 22.8 cm?1 for 2.  相似文献   

20.
A study on the adsorption characteristics of Pb(II) and Cr(III) cations onto C‐4‐methoxyphenylcalix‐[4]resorcinarene (CMPCR) in batch and fixed bed column systems has been conducted. CMPCR was produced by one step synthesis from resorcinol, 4‐methoxybenzaldehyde, and HCl. The synthesis was carried out at 78 °C for 24 hours and afforded the adsorbent in 85.7% as a 3:2 mixture of C:C isomer. Most parameters in batch and fixed bed column systems confirm that CMPCR is a good adsorbent for Pb(II) and Cr(III), though Pb(II) adsorption was more favorable than that of Cr(III). The adsorption kinetic of Pb(II) and Cr(III) adsorptions in batch and fixed bed column systems followed a pseudo 2n order kinetics model. The rate constant of Pb(II) was higher than that of Cr(III) in the batch system, but this result was contrary to the result obtained in a fixed bed column system. Desorption studies to recover the adsorbed Pb(II) and Cr(III) were performed sequentially with distilled water and HCl, and the results showed that the adsorption was dominated by chemisorption.  相似文献   

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