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1.
The employment of a new rigid N‐tridentate ligand, bis(1‐chloroimidazo[1,5‐a]pyridin‐3‐yl)pyridine (bcpp), in the construction of cobalt(II) single‐ion magnets is reported. Two cobalt(II) complexes, [Co(bcpp)Cl2] ( 1 ) and [Co(bcpp)Br2] ( 2 ), have been prepared and characterized. Single‐crystal XRD analyses reveal that complexes 1 and 2 are isostructural. They are pentacoordinated mononuclear cobalt(II) compounds with expected trigonal bipyramidal geometry. Both analysis of the magnetic data and ab initio calculations reveal easy‐plane magnetic anisotropy (D>0) for 1 and 2 . Detailed alternating current magnetic susceptibility measurements reveal the occurrence of slow magnetic relaxation behavior for the cobalt(II) centers of 1 and 2 ; thus indicating that both complexes are field‐induced single‐ion magnets.  相似文献   

2.
For a long time, the cobalt(II) complex ([Co(napy)4](ClO4)2) (napy=1, 8‐naphthyridine) has been considered as an eight‐coordinate complex without any structural proof. After careful considerations, two complexes [Co(napy)2Cl2] ( 1 ) and [Co(napy)4](ClO4)2 ( 2 ) based on the bidentate ligand napy were synthesized and structurally characterized. X‐ray single‐crystal structural determination showed that the cobalt(II) center in [Co(napy)2Cl2] ( 1 ) is four‐coordinate with a tetrahedral geometry (Td), while [Co(napy)4](ClO4)2 ( 2 ) is seven‐coordinate rather than eight‐coordinate with a capped trigonal prism geometry (C2v). Direct‐current (dc) magnetic data revealed that complexes 1 and 2 possess positive zero‐field splitting (ZFS) parameters of 11.08 and 25.30 cm?1, respectively, with easy‐plane magnetic anisotropy. Alternating current(ac) susceptibility measurements revealed that both complexes showed slow magnetic relaxation behaviour. Theoretical calculations demonstrated that the presence of easy‐plane magnetic anisotropy (D>0) for complexes 1 and 2 is in agreement with the experimental data. Furthermore, these results pave the way to obtain four‐coordinate and seven‐coordinate cobalt(II) single‐ion magnets (SIMs) by using a bidentate ligand.  相似文献   

3.
Detailed ab initio calculations were performed on two structurally different cerium(III) single‐molecule magnets (SMMs) to probe the origin of magnetic anisotropy and to understand the mechanism of magnetic relaxations. The complexes [CeIII{ZnII(L)}2(MeOH)]BPh4 ( 1 ) and [Li(dme)3][CeIII(cot′′)2] ( 1 ; L=N,N,O,O‐tetradentate Schiff base ligand; 2 ; DME=dimethoxyethane, COT′′=1,4‐bis(trimethylsilyl)cyclooctatetraenyldianion), which are reported to be zero‐field and field‐induced SMMs with effective barrier heights of 21.2 and 30 K respectively, were chosen as examples. CASSCF+RASSI/SINGLE_ANISO calculations unequivocally suggest that mJ|±5/2〉 and |±1/2〉 are the ground states for complexes 1 and 2 , respectively. The origin of these differences is rooted back to the nature of the ligand field and the symmetry around the cerium(III) ions. Ab initio magnetisation blockade barriers constructed for complexes 1 and 2 expose a contrasting energy‐level pattern with significant quantum tunnelling of magnetisation between the ground state Kramers doublet in complex 2 . Calculations performed on several model complexes stress the need for a suitable ligand environment and high symmetry around the cerium(III) ions to obtain a large effective barrier.  相似文献   

4.
Four dinuclear LnIII? CuII complexes with Ln=Tb ( 1 ), Dy ( 2 ), Ho ( 3 ), and Er ( 4 ) were synthesized to investigate the relationship between their respective magnetic anisotropies and ligand‐field geometries. These complexes were crystallographically isostructural, and a uni‐axial ligand field was achieved by using three phenoxo oxygen groups. Complexes 1 and 2 displayed typical single‐molecule magnet (SMM) behaviors, of which the out‐of‐phase susceptibilities were observed in the temperature range of 1.8–5.0 K ( 1 ) and 1.8–20.0 K ( 2 ). The Cole–Cole plots exhibited a semicircular shape with α parameters in the range of 0.08–0.18 (2.6–4.0 K) and 0.07–0.24 (3.5–7.0 K). The energy barriers Δ/kB were estimated from the Arrhenius plots to be 32.9(4) K for 1 and 26.0(5) K for 2 . Complex 3 displayed a slow magnetic relaxation below 3.0 K, whereas complex 4 did not show any frequency‐dependent behavior for both in‐phase and out‐of‐phase susceptibilities, which indicates that easy‐axis anisotropy was absent. The temperature dependence of the dc susceptibilities for the field‐aligned samples of 1 – 3 revealed that the χMT value continuously increased as the temperature was lowered, which indicates the presence of low‐lying Stark sublevels with the highest |Jz| values. In contrast, complex 4 displayed a smaller and temperature‐independent χMT value, which also indicates that easy‐axis anisotropy was absent. Simultaneous analyses were carried out for 1 – 3 to determine the magnetic anisotropy parameters on the basis of the Hamiltonian that considers B20, B40, and B60.  相似文献   

5.
Tuning the magnetic anisotropy of metal ions remains highly interesting in the design of improved single‐molecule magnets (SMMs). We herein report synthetic, structural, magnetic, and computational studies of four mononuclear CoII complexes, namely [Co(hfac)2(MeCN)2] ( 1 ), [Co(hfac)2(Spy)2] ( 2 ), [Co(hfac)2(MBIm)2] ( 3 ), and [Co(hfac)2(DMF)2] ( 4 ) (MeCN=acetonitrile, hfac=hexafluoroacetylacetone, Spy=4‐styrylpyridine, MbIm=5,6‐dimethylbenzimidazole, DMF=N,N‐dimethylformamide), with distorted octahedral geometry constructed from hexafluoroacetylacetone (hfac) and various axial ligands. By a building block approach, complexes 2 – 4 were synthesized by recrystallization of the starting material of 1 from various ligands containing solution. Magnetic and theoretical studies reveal that 1 – 4 possess large positive D values and relative small E parameters, indicating easy‐plane magnetic anisotropy with significant rhombic anisotropy in 1 – 4 . Dynamic alternative current (ac) magnetic susceptibility measurements indicate that these complexes exhibit slow magnetic relaxation under external fields, suggesting field‐induced single‐ion magnets (SIMs) of 1 – 4 . These results provide a promising platform to achieve fine tuning of magnetic anisotropy through varying the axial ligands based on Co(II) bis(hexafluoroacetylacetonate) complexes.  相似文献   

6.
Three coordination polymers, namely [Co(BDC)( L )] · H2O ( 1 ), [Co(NPH)( L )] · H2O ( 2 ), and [Ni(NPH)( L )(H2O)3] · H2O ( 3 ) [H2BDC = 1, 3‐benzenedicarboxylic acid, H2NPH = 3‐nitrophthalic acid, L = N,N′‐bis(3‐pyridyl)‐terephthalamide] were hydrothermally synthesized by self‐assembly of cobalt/nickel chloride with a semi‐rigid bis‐pyridyl‐bis‐amide ligand and two aromatic dicarboxylic acids. Single crystal X‐ray diffraction analyses revealed that complexes 1 and 2 are two‐dimensional (2D) coordination polymers containing a one‐dimensional (1D) ribbon‐like Co‐dicarboxylate chain and a 1D zigzag Co‐ L chain. Although the coordination numbers of CoII ions and the coordination modes of two dicarboxylates are different in complexes 1 and 2 , they have a similar 3, 5‐connected {42.67.8}{42.6} topology. In complex 3 , the adjacent NiII ions are linked by L ligands to form a 1D polymeric chain, whereas the 1D chains does not extend into a higher‐dimensional structure due to the ligand NPH with monodentate coordination mode. The adjacent layers of complexes 1 and 2 and the adjacent chains of 3 are further linked by hydrogen bonding interactions to form 3D supramolecular networks. Moreover, the thermal stabilities, fluorescent properties, and photocatalytic activities of complexes 1 – 3 were studied.  相似文献   

7.
A novel Schiff base ligand (H2L) was prepared through condensation of 2,6‐diaminopyridine and o‐benzoylbenzoic acid in a 1:2 ratio. This Schiff base ligand was characterized using elemental and spectroscopic analyses. A new series of Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) metal complexes of H2L were prepared and characterized using elemental analysis, spectroscopy (1H NMR, mass, UV–visible, Fourier transform infrared, electron spin resonance), magnetic susceptibility, molar conductivity, X‐ray powder diffraction and thermal analysis. The complexes are found to have trigonal bipyramidal geometry except Cr(III), Mn(II) and Fe(III) complexes which have octahedral geometry based on magnetic moment and solid reflectance measurements. The infrared spectral studies reveal that H2L behaves as a neutral bidentate ligand and coordinates to the metal ions via the two azomethine nitrogens. 1H NMR spectra confirm the non‐involvement of the carboxylic COOH proton in complex formation. The presence of water molecules in all reported complexes is supported by thermogravimetric studies. Kinetic and thermodynamic parameters were determined using Coats–Redfern and Horowitz–Metzger equations. The synthesized ligand and its complexes were screened for antimicrobial activities against two Gram‐positive bacteria (Bacillus subtilis and Staphylococcus aureus), two Gram‐negative bacteria (Escherichia coli and Neisseria gonorrhoeae) and one fungus (Candida albicans). Anticancer activities of the ligand and its metal complexes against human breast cancer cell line (MCF7) were investigated. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

8.
The magnetic properties of two octahedral iron(II) complexes with Schiff base like equatorial N2O2 coordinating ligands and methanol (MeOH) as axial ligand are reported. Both compounds [FeL1(MeOH)2] ( 1 ) and [FeL2(MeOH)2] ( 2 ) (with L1 = [3,3′]‐[1,2‐phenylenebis(iminomethylidyne)‐bis(2,4‐pentanedionato)(2‐)‐N,N′,O2,O2′] and L2 = [E,E]‐[{diethyl 2,2′‐1,2‐phenylenebis(iminomethylidyne)bis(3‐oxo‐3‐phenylpropanato)} (2‐)‐N,N′,O3,O3′]) show a weak spontaneous magnetization below TC = 10 K. Results from X‐ray structure analysis of 1 indicate, that this is due to 2D network of hydrogen bonds as previously discussed for a similar complex.  相似文献   

9.
    
Cu (II), Ni (II) and Co (II) complexes of the type ML2,2B where L = 2′-hydroxy-5′-X-chalconeoxime (X = H, CH3, Cl) and B = water or pyridine have been obtained from chalconeoximes and by reacting the preformed metal (II) chalcone complexes with hydroxylamine. They have been characterised on the basis of elemental and thermal analyses, conductivity and magnetic measurements and ligand field and m spectra. All the complexes are high-spin octahedral species in contrast to the low-spin square planar Ni (II) and Co (II) salicylaldoxime complexes. IR spectral studies indicate that conjugation is relatively damped in chalconeoxime. The lower ligand field strangth of the oxime is attributed to the weak M-N bonding and less extensive dπ π*3 back-bonding. Replacement of water by pyridine weakens metal-oximino bond in the complexes.  相似文献   

10.
Coordination compounds of Mn (II), Fe (III), Co (II), Ni (II), Cu (II) and Cd (II) ions were synthesized from reaction with Schiff base ligand 4,6‐bis((E)‐(2‐(pyridin‐2‐yl)ethylidene)amino)pyrimidine‐2‐thiol (HL) derived from the condensation of 4,6‐diaminopyrimidine‐2‐thiol and 2‐(pyridin‐2‐yl)acetaldehyde. Microanalytical data, magnetic susceptibility, infrared and 1H NMR spectroscopies, mass spectrometry, molar conductance, powder X‐ray diffraction and thermal decomposition measurements were used to determine the structure of the prepared complexes. It was found that the coordination between metal ions and bis‐Schiff base ligand was in a molar ratio of 1:1, with formula [M (HL)(H2O)2] Xn (M = Mn (II), Co (II), Ni (II), Cu (II) and Cd (II), n = 2; Fe (III), n = 3). Diffuse reflectance spectra and magnetic susceptibility measurements suggested an octahedral geometry for the complexes. The coordination between bis‐Schiff base ligand and metal ions was through NNNN donor sites in a tetradentate manner. After preparation of the complexes, biological studies were conducted using Gram‐positive (B. subtilis and S. aureus) and Gram‐negative (E. coli and P. aeruginosa) organisms. Metal complexes and ligand displayed acceptable microbial activity against both types of bacteria.  相似文献   

11.
Mixed ligand complexes of Co(II) with nitrogen and sulfur donors, Co(OPD)(S–S) · 2H2O and Co(OPD)(S–S)L2 [OPD = o-phenylenediamine; S–S = 1,1-dicyanoethylene-2,2-dithiolate (i-MNT2?) or 1-cyano-1-carboethoxyethylene-2,2-dithiolate (CED2?); L = pyridine (py), α-picoline (α-pic), β-picoline (β-pic), or γ-picoline (γ-pic)], have been isolated and characterized by analytical data, molar conductance, magnetic susceptibility, electronic, and infrared spectral studies. The molar conductance data reveal non-electrolytes in DMF. Magnetic moment values suggest low-spin and high-spin complexes. The electronic spectral studies suggest distorted octahedral stereochemistry around Co(II) in these complexes. Infrared spectral studies suggest bidentate chelating behavior of i-MNT2?, CED2?, or OPD while other ligands are unidentate in their complexes.  相似文献   

12.
We report a series of 3d–4f complexes {Ln2Cu3(H3L)2Xn} (X=OAc?, Ln=Gd, Tb or X=NO3?, Ln=Gd, Tb, Dy, Ho, Er) using the 2,2′‐(propane‐1,3‐diyldiimino)bis[2‐(hydroxylmethyl)propane‐1,3‐diol] (H6L) pro‐ligand. All complexes, except that in which Ln=Gd, show slow magnetic relaxation in zero applied dc field. A remarkable improvement of the energy barrier to reorientation of the magnetisation in the {Tb2Cu3(H3L)2Xn} complexes is seen by changing the auxiliary ligands (X=OAc? for NO3?). This leads to the largest reported relaxation barrier in zero applied dc field for a Tb/Cu‐based single‐molecule magnet. Ab initio CASSCF calculations performed on mononuclear TbIII models are employed to understand the increase in energy barrier and the calculations suggest that the difference stems from a change in the TbIII coordination environment (C4v versus Cs).  相似文献   

13.
A novel Schiff base ligand (H‐DPPMHQ) derived from 2‐hydrazineylquinoline and 1,3‐diphenyl‐1H‐pyrazole‐5‐carbaldehyde and its dimeric complexes with compositions [Cr(DPPMHQ)Cl]2?2Cl and [M(DPPMHQ)Cl]2 (where M = Cu(II), Co(II), Ni(II) and Zn(II)) have been synthesized and characterized using physicochemical methods like elemental analysis, magnetic susceptibility and molar conductivity measurements, multispectral techniques and electrochemical studies. The molar conductance data reveal that all metal chelates are non‐electrolytes, except the Cr(III) complex which shows a ΛM value of 146.82 Ω?1 cm2 mol?1, indicating that it is a 1:2 electrolyte. Infrared spectral results show that the metal is organized through four nitrogen atoms (azomethine and deprotonated imine groups, pyrazole and quinoline rings) besides chlorine atoms. The NH proton is also displaced during complexation, as indicated by 1H NMR spectral data. Based on the electron spin resonance and ligand field parameter data, the bonding parameters of these complexes have been calculated. Using Coats–Redfern and Horowitz–Metzger equations, thermodynamic parameters were determined. The spectral data indicate that the dimeric complexes have octahedral geometry around the central metal ions. The cytotoxic activities of all compounds were evaluated towards human breast cancer (MCF‐7) and lung cancer (A549) cell lines.  相似文献   

14.
The facile and tunable preparation of unique dinuclear [(L?)Pd?X?Pd(L?)] complexes (X=Cl or N3), bearing a ligand radical on each Pd, is disclosed, as well as their magnetochemistry in solution and solid state is reported. Chloride abstraction from [PdCl( NNOISQ )] ( NNOISQ =iminosemiquinonato) with TlPF6 results in an unusual monochlorido‐bridged dinuclear open‐shell diradical species, [{Pd( NNO ISQ)}2(μ‐Cl)]+, with an unusually small Pd‐Cl‐Pd angle (ca. 93°, determined by X‐ray). This suggests an intramolecular d8–d8 interaction, which is supported by DFT calculations. SQUID measurements indicate moderate antiferromagnetic spin exchange between the two ligand radicals and an overall singlet ground state in the solid state. VT EPR spectroscopy shows a transient signal corresponding to a triplet state between 20 and 60 K. Complex 2 reacts with PPh3 to generate [Pd(NNOISQ)(PPh3)]+ and one equivalent of [PdCl( NNOISQ )]. Reacting an 1:1 mixture of [PdCl( NNOISQ )] and [Pd(N3)( NNOI SQ)] furnishes the 1,1‐azido‐bridged dinuclear diradical [{Pd( NNO ISQ)}21‐N;μ‐N3]+, with a Pd‐N‐Pd angle close to 127° (X‐ray). Magnetic and EPR measurements indicate two independent S=1/2 spin carriers and no magnetic interaction in the solid state. The two diradical species both show no spin exchange in solution, likely because of unhindered rotation around the Pd?X?Pd core. This work demonstrates that a single bridging atom can induce subtle and tunable changes in structural and magnetic properties of novel dinuclear Pd complexes featuring two ligand‐based radicals.  相似文献   

15.
Two symmetric tetrapodal ligands L1–2 and one asymmetric tetrapodal ligand L3 based on 4,5‐diazafluoren have been synthesized and characterized. Ligands L1–2 formed by the condensation of pentaerythrityl tetratosylate with 4,5‐diazafluoren‐9‐oxime and 9‐(4‐hydroxy)phenylimino‐4,5‐diazafluorene, respectively. L3 was prepared by two steps, 9‐(4‐hydroxy)phenylimino‐4,5‐diazafluorene reacted with pentaerythrityl tetratosylate affording 1,1′,1"‐tris[(4,5‐diazafluoren‐9‐ylimino)phenoxymethyl]‐1"′‐(p‐tosyloxymethyl)‐methane, which reacted with 4,5‐diazafluoren‐9‐oxime affording the asymmetric ligand L3. Three tetranuclear RuII complexes [(bpy)8L1–3Ru4](PF6)8 (bpy = bipyridine) were obtained by the reaction of Ru(bpy)2Cl2 · 2H2O with ligands L1–3. Spectroscopic studies of these complexes exhibit metal‐to‐ligand charge transfer absorptions at 440–445 nm and emissions at 575–579 nm. The electrochemical behaviors of these complexes are consistent with one RuII‐based oxidation couple and three ligand‐centered reduction couples.  相似文献   

16.
Two nickel(II) complexes were synthesized and structurally as well as magnetically characterized by using two positional isomeric nitronyl nitroxide radical ligands and H3cda as co‐ligand: [Ni(NIToPy)(cda)]H2O · CH3OH ( 1 ) and [Ni(IM4Py)2(cda)H2O] ( 2 ) [NIToPy = 2‐(3′‐pyridinyl)‐4,4,5,5‐tetramethyl‐4,5‐dihydro‐1H‐imidazolyl‐1‐oxyl‐3‐oxide; IM4Py = 2‐(4′‐pyridinyl)‐4,4,5,5‐tetramethylimidazoline‐l‐oxyl; H3cda = 4‐hydroxypyridine‐2,6‐dicarboxylic acid]. Single‐crystal structures analyses show that both complexes have similar mononuclear structures, in which the central NiII ions are hexacoordinated with a distorted octahedral arrangement. The magnetic properties of 1 and 2 were studied, and antiferromagnetic interactions between NiII ion and radicals are observed.  相似文献   

17.
A series of mononuclear complexes of the type, [MLCl2] [M = CoII, NiII, CuII, and ZnII] with a pyrimidene‐type ligand, which was synthesized by the reaction of 2‐furaldehyde and 1, 8‐diaminonaphthalene, was obtained. The ligand and its complexes were characterized by elemental analysis, IR, NMR, EPR, and UV/Vis spectroscopy, ESI‐mass spectrometry, magnetic susceptibility, molar conductivity, and thermogravimetric analyses. On the basis of UV/Vis spectroscopic and magnetic susceptibility data, an octahedral arrangement was assigned around all metal ions. The low molar conductivity data for all the complexes show their non‐electrolytic nature. The thermal behavior of the complexes was studied by TGA analyses. The electrochemical study carried out on the CuII complex exhibits a quasi reversible redox process. The ligand and its complexes showed potential antioxidant and antimicrobial activities.  相似文献   

18.
The cover picture shows how differing coordination algorithms control the molecular architecture of complexes of the pyridazine‐containing, two‐armed, acyclic Schiff base ligand L2 (left, prepared from one equivalent of 3,6‐diformylpyridazine and two equivalents of d‐anisidine). Two very different complexes of L2 self‐assemble from tetrahedral copper(I ) versus octahedral zinc(II ), nickel(II ), and cobalt(II ) controlled 1 : 1 reactions with L2. In both cases the metal ions are bridged by the pyridazine moieties in L2, but in the case of the tetrahedral copper(II ) the result is a tetrametallic [2×2] grid complex ([CuI4(L2)4]4+: top right), whilst in the case of the octahedral metal(II ) ions dimetallic side‐by‐side complexes, [MII2(L2)2(X)4]y+ (M = Mn, Co, Ni, Zn; X = solvent or anion), are formed (bottom right). The cover image was kindly generated by M. Crawford (University of Otago) with Strata Studio Pro (Strata). More details are given by S. Brooker and co‐workers on p. 3772 ff.  相似文献   

19.
Syntheses and structures of five imido‐bridged dinuclear titanium complexes and two (bis)ligand‐coordinated mononuclear titanium complexes are reported. Addition of 1 or 2 equiv. of Schiff base ligand (((1H‐pyrrol‐2‐yl)methylene)amino)‐2,3‐dihydro‐1H‐inden‐2‐ol (H2L) to Ti(NMe2)4 resulted in transamination with 4 equiv. of dimethylamides generating a (bis)ligand‐coordinated complex Ti(L)2 ( 1 ). Treatment of Ti(NMe2)4 with 1 equiv. of tBuNH2 followed by addition of 1 equiv. of H2L afforded an imido‐bridged complex [Ti(L)(NtBu)]2 ( 2 ). 1:1:1:1 reaction of Ti(NMe2)4/RNH2/H2L/py(or phen) produced imido‐bridgedcomplexes [Ti(L)(NPh)(py)]2 ( 3 ), [Ti(L)(4‐F‐PhN)(py)]2·Tol ( 4 ·Tol), [Ti(L)(4‐Cl‐PhN)(py)]2·Tol·THF ( 5 ·Tol·THF), [Ti(L)(4‐Br‐PhN)(py)]2·Tol ( 6 ·Tol) and a (bis)ligand‐coordinated complex Ti(L)2·phen ( 7 ) (py = pyridine, phen = 1,10‐phenanthroline). Attempts to prepare the monomeric titianium imido complexes were unsuccessful. DFT studies show that the assumed compound which contains Ti = N species is less stable than imido‐bridged Ti‐N(R)‐Ti complexes, providing the better understanding of the experimental results.  相似文献   

20.
Two new binuclear cobalt(II) complexes, [Co2 L1 (μ2‐DPP)]2+ ( 1 ) (H L1 = N, N, N′, N′‐ tetrakis (2‐benzimidazolylmethyl)‐2‐hydroxyl ‐1,3‐diaminopropane; DPP = diphenylphosphinate) and [Co2 L2 (μ2‐BNPP)2]+ ( 2 ) (H L2 = 2,6‐bis‐[N,N‐di(2‐ pyridylmethyl)aminomethyl]‐4‐methylphenol, BNPP = bis(4‐nitrophenyl)phosphate) have been synthesized and their crystal structures and magnetic properties are shown. In 1 , each CoII atom has a distorted trigonal bipyramidal coordination sphere with a N3O2 donor set and the central two CoII atoms are bridged by one alkoxo‐O atom and one μ2‐DPP ion with the Co1‐Co2 separation of 3.542Å. In 2 , each CoII atom has a pseudo octahedral environment with a N3O3 donor set and the central two CoII atoms are bridged by a phenolic oxygen atom of L2 and two μ2‐BNPP ions with the Co1‐Co2 separation of 3.667Å. Susceptibility data of 1 and 2 indicate intramolecular antiferromagnetic coupling of the high‐spin CoII atoms.  相似文献   

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