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1.
Two Ni(II) complexes of the dianionic ligands, Mebpb2−, [H2Mebpb = N,N′-bis(pyridine-2-carboxamido)-4-methylbenzene] and Mebqb2−, [H2Mebqb = N,N′-bis(quinoline-2-carboxamido)-4-methylbenzene] have been synthesized and characterized by elemental analyses, IR, and UV-Vis spectroscopy. The crystal and molecular structures of [Ni(Mebpb)], (1), and [Ni(Mebqb)], (2), were determined by X-ray crystallography. Both complexes exhibit distorted square-planar NiN4 coordination figures with two short and two long Ni-N bonds (Ni-N ∼1.84 and ∼1.95 Å, respectively). The electrochemical behavior of these complexes with the goal of evaluating the structural effects on the redox properties has been studied. 相似文献
2.
Nickel(II) complexes of N,N′-dimethyl-N,N′-bis(pyridyl-2yl-methyl)ethylene-diamine (L1), N,N′-dimethyl-N,N′-bis(pyridyl-2-ylmethyl)-1,2-diaminopropane (L2) and N,N′-dimethyl-N,N′-bis(pyridyl-2-ylmethyl)-1,3-diaminopropane (L3) were prepared and their spectroscopic and redox properties studied. The distorted octahedral structure was determined for [NiL3ClCH3OH](ClO4) by using X-ray crystallography. The electronic spectral behavior of the complexes at different pHs was analyzed; it is shown that a new band grew at the expense of the other band intensity in acid media. The redox properties of ligands and their complexes show the peaks of Ni(II) → Ni(III) and Ni(II) → Ni(0) as these were detected at low concentration while Ni(II) → Ni(I) process was detectable clearly at high concentration. Furthermore, the interaction studies of 2-mercaptoethanesulfonic acid as a simulator of coenzyme M reductase (CoM) with NiN4 chromophores are discussed. 相似文献
3.
Bassem A. Al-Maythalony 《Inorganica chimica acta》2009,362(9):3109-1266
A series of gold(III) metalacycle of five-, six- and seven-membered ring was prepared by reacting Auric acid (HAuCl4 · 3H2O) with 1 equiv. unsubstituted ethylenediamine (en), propylene diamine (pn) and butylenediamine (bn) ligands and with some N-mono-substituted as well as N,N′-disubstituted ethylenediamine ligands. The general formula of these complexes is [Au(alkyldiamine)Cl2]Cl. These complexes are characterized by melting point and elemental analysis, while structural analysis was done by spectroscopic techniques such as UV-Vis, Far-IR, IR spectroscopy, 1H and 13C solution as well as 13C and 15 N solid-state NMR. The solid-state 15 N NMR shows that the chemical shift difference between free and bound ligand decreases as bn > pn > en, indicating stronger Au-N bond for bn complex compared to pn and en. UV-Vis shows relative stability of the Au(III) complexes of unsubstituted ethylenediamine with respect to N,N′-di-substituted ethylenediamine. Far-IR data show the six-membered metalacycle gold(III) alkanediamine complexes to be more stable. Spectroscopic data are evaluated by comparisons with calculated data of the built and optimized structure by gaussian03 at the RB3LYP level with LanL2DZ bases set. 相似文献
4.
《Inorganica chimica acta》2002,328(1):111-122
The electrochemical oxidation of anodic metal (nickel, copper, zinc and cadmium) in acetonitrile solutions containing N,N′-bis[(4-methylphenyl)sulfonyl]ethylenediamine H2L and an additional nitrogen coligand, such as 1,10-phenanthroline, yielded mixed complexes of general formula [ML(phen)2] (M=Ni, Cu, Zn and Cd). The compounds have been characterized by microanalysis, IR and UV-Vis (Ni, Cu complexes) spectroscopy, FAB mass spectrometry, 1H NMR spectroscopic studies (Zn, Cd complexes) and EPR spectroscopy (Cu and Ni complexes). All compounds have also been characterized by single crystal X-ray diffraction. The molecular structures of these compounds consist of individual monomeric molecules in which the metal atom is in an [MN6] distorted octahedral environment. 相似文献
5.
Two sets of ligands, set-1 and set-2, have been prepared by mixing 1,3-diaminopentane and carbonyl compounds (2-acetylpyridine or pyridine-2-carboxaldehyde) in 1:1 and 1:2 ratios, respectively, and employed for the synthesis of complexes with Ni(II) perchlorate, Ni(II) thiocyanate and Ni(II) chloride. Ni(II) perchlorate yields the complexes having general formula [NiL2](ClO4)2(L = L1 [N3-(1-pyridin-2-yl-ethylidene)-pentane-1,3-diamine] for complex 1 or L2[N3-pyridin-2-ylmethylene-pentane-1,3-diamine] for complex 2) in which the Schiff bases are monocondensed terdentate, whereas Ni(II) thiocyanate results in the formation of tetradentate Schiff base complexes, [NiL(SCN)2] (L = L3[N,N′-bis-(1-pyridin-2-yl-ethylidine)-pentane-1,3-diamine] for complex 3 or L4 [N,N′-bis(pyridin-2-ylmethyline)-pentane-1,3-diamine] for complex 4) irrespective of the sets of ligands used. Complexes 5 {[NiL3(N3)2]} and 6 {[NiL4(N3)2]} are prepared by adding sodium azide to the methanol solution of complexes 1 and 2. Addition of Ni(II) chloride to the set-1 or set-2 ligands produces [Ni(pn)2]Cl2, 7, as the major product, where pn = 1,3-diaminopentane. Formation of the complexes has been explained by the activation of the imine bond by the counter anion and thereby favouring the hydrolysis of the Schiff base. All the complexes have been characterized by elemental analyses and spectral data. Single crystal X-ray diffraction studies confirm the structures of three representative members, 1, 4 and 7; all of them have distorted octahedral geometry around Ni(II). The bis-complex of terdentate ligands, 1, is the mer isomer, and complexes 4 and 7 possess trans geometry. 相似文献
6.
Duha Jawad Awad 《Inorganica chimica acta》2011,365(1):127-132
Due to the better solubility of the 4,4′-substituted bipyridine ligand a series of 4,4′-bis(tert-butyl)-2,2′-bipyridinedichlorometal(II) complexes, [M(tbbpy)Cl2], with M = Cu, Ni, Zn, Pd, Pt was synthesised and characterised. The blue copper complex 4,4′-bis(tert-butyl)-2,2′-bipyridinedichlorocopper(II) was isolated in two different polymorphic forms, as prisms 1 with a solvent inclusion and solvent-free as needles 2. Both structures were determined by X-ray structure analysis. They crystallise in the monoclinic space group P21/c with four molecules in the unit cell, but with different unit cells and packing motifs. Whereas in the prisms 1, with the unit cell parameters a = 12.1613(12), b = 10.6363(7), c = 16.3074(15) Å, β = 94.446(8)°, the packing is dominated by intra- and intermolecular hydrogen bonds, in the needles 2, with a = 7.738(1), b = 18. 333(2), c = 13.291(3) Å, β = 97.512(15)°, only intramolecular hydrogen bonds appear and the complex molecules are arranged in columns which are stabilised by π-π-stacking interactions. In both complexes the copper has a tetrahedrally distorted coordination sphere. These copper complexes were also studied by EPR spectroscopy in solution, as frozen glass and diamagnetically diluted powder with the analogue [Pd(tbbpy)Cl2] as host lattice. 相似文献
7.
Wolfgang Bauer 《Inorganica chimica acta》2009,362(7):2341-2346
Five new octahedral iron(II) complexes [FeL2(4-dpa)]n(EtOH) (1), [FeL2(bipy)]n(DMF) (2), [FeL1(bpee)]n (3), [Fe2L3(1-meim)4](1-meim)4 (4) and [FeL1(DMAP)2] (5), with L1 and L2 being tetradentate coordinating Schiff base like ligands (L1 = (E,E)-[{diethyl-2,2′-[1,2-phenylenebis(iminomethylidyne)]bis[3-oxobutanato](2-)-N,N′,O3,O3′}, L2 = (3,3′)-[{1,2-phenylenebis(iminomethylidyne)]bis(2,4-pentane-dionato)(2-)-N,N′,O2,O2′}) and L3 being a octadentate dinucleating coordinating Schiff base like ligand ({tetraethyl-(E,E,E,E)-2,2′,2′′,2′′′-[1,2,4,5-phenylentetra(iminomethylidine)]tetra[3-oxobutanoato](2-)-N,N′,N′′,N′′′,O3,O3′,O3′′,O3′′′}); 4-dpa = di(4-picolyl)-amine, bipy = 4,4′-bipyridine, bpee = trans-1,2-bis(4-pyridyl)ethylene, 1-meim = 1-methylimidazole and DMAP = 4-dimethylaminopyridine, have been synthesized and characterised using X-ray structure analysis and T-dependent susceptibility measurements. Both methods indicate that all iron(II) centres are in the paramagnetic high-spin state over the whole temperature range investigated. The O-Fe-O angle, the so called bit of the equatorial ligand, is with an average of 111° in the region typical for high-spin iron(II) complexes of this ligand type. In the case of compound 1 an infinite two-dimensional hydrogen bond network can be found, for the compounds 2-4 no hydrogen bond interactions are observed between the complex molecules. A comparison of the curve progression obtained from the magnetic measurements of the mononuclear complex 5 and the polymeric complexes 1-3 leads to the conclusion that no magnetic interactions are mediated over the bridging axial ligands. For the dinuclear complex 4 weak antiferromagnetic interactions between the two iron centres are found. 相似文献
8.
The preparation and characterization of manganese(III) complexes containing the quadridenate ligand, N,N′-bis(aminobenzylidene)-1,2-ethanediamine (H2amben), and its previously unreported analogue, N,N′-bis(2-amino-5-nitro-benzylidene)-1,2-ethanediamine (H2nitroamben), are described. The new manganese(III) halide/pseudohalide complexes, Mn(amben)X · nH2O and Mn(nitroamben)X · nH2O (X = Cl, Br, I, NCS; n = 0.5 or 1), were isolated as red-brown, microcrystalline solids, which were characterized fully. 相似文献
9.
Bikshandarkoil R. Srinivasan Sunder N. Dhuri Wolfgang Bensch 《Inorganica chimica acta》2005,358(2):279-287
The title compounds 1,3-propanediammonium tetrathiomolybdate, (1,3-pnH2)[MoS4], 1 and, N,N,N′,N′-tetramethylethylenediammonium tetrathiomolybdate, (tmenH2)[MoS4], 2, were prepared by reacting the ammonium salt of [MoS4]2− with the corresponding organic diamine. In 1 and 2 the organic diamines 1,3-propanediamine (1,3-pn) and N,N,N′,N′-tetramethylethylenediamine (tmen) are present in their diprotonated form. The reaction of 1 or 2 with [Ni(en)3]Cl2 · 2H2O (en is ethylenediamine) results in the formation of the highly insoluble complex tris(ethylenediamine)Ni(II) tetrathiomolybdate, [Ni(en)3][MoS4], in quantitative yields. 1 and 2 have been characterized by chemical analysis, vibrational, UV-Vis and NMR spectroscopy, TG-DTA-MS and single crystal X-ray crystallography. Compound 1 is thermally more stable compared to 2. Both complexes decompose in a single step forming amorphous molybdenum sulfide. The structure of the title complexes can be described as consisting of tetrahedral [MoS4]2− dianions which accept a complex series of H-bonds from the organic dications. The strength and number of these hydrogen bonds affect the Mo-S bond lengths. 相似文献
10.
Carol F. Fortney Steven J. Geib Fu-tyan Lin Rex E. Shepherd 《Inorganica chimica acta》2005,358(10):2921-2932
Two ruthenium nitrosyl bis-pyridyl/biscarboxamido compounds, [Ru(NO)(bpp)Cl · 2H2O] [bpp = N,N′-bis(2-pyridinecarboxamide)-1,3-propane dianion] and [Ru(NO)(bpe)Cl · 2H2O] [bpe = N,N′-(bis-2-pyridinecarboxamide)-1,2-ethane dianion] have been characterized by 1H NMR, 13C{1H} NMR, and IR spectroscopies, electrospray ionizaton mass spectrometry, and X-ray crystallography. 相似文献
11.
Three mono oxovanadium(V) complexes of tridentate Schiff base ligands [VO(OMe)L1] (1), [VO(OMe)L2] (2) and [VO(OMe)L3] (3) obtained by monocondensation of 3-hydroxy-2-naphthohydrazide and aromatic o-hydroxyaldehydes have been synthesized (H2L1 = (E)-3-hydroxy-N′-(2-hydroxy-3-methoxybenzylidene)-2-naphthohydrazide, H2L2 = (E)-3-hydroxy-N′-(2-hydroxybenzylidene)-2-naphthohydrazide and H2L3 = (E)-N′-(5-bromo-2-hydroxybenzylidene)-3-hydroxy-2-naphthohydrazide). The complexes were characterized by spectroscopic methods in the solid state (IR) and in solution (UV-Vis, 1H NMR). Single crystal X-ray analyses were performed with 1 and 2. The catalytic potential of these complexes has been tested for the oxidation of cyclooctene using H2O2 as the terminal oxidant. The effects of various parameters including the molar ratio of oxidant to substrate, the temperature, and the solvent have been studied. The catalyst 2 showed the most powerful catalytic activity in oxidation of various terminal, cyclic and phenyl substituted olefins. Excellent conversions have been obtained for the oxidation of cyclic and bicyclic olefins. 相似文献
12.
Muriel A. Fabre 《Inorganica chimica acta》2005,358(7):2384-2394
Several new mononuclear and dinuclear ruthenium(II) complexes - incorporating 2,2′:6′,2″-terpyridine and acetylacetonate as ancillary ligands and phenylcyanamide derivative ligands - of the type [Ru(tpy)(acac)(L)] and [{Ru(tpy)(acac)}2(μ-L′)] (where tpy = 2,2′:6′,2″-terpyridine, acac = acetylacetonate, L = hmbpcyd = 4-(3-hydroxy-3-methylbutynyl)phenylcyanamide anion (2) and epcyd = 4-ethynylphenylcyanamide anion (3) and L′ = bcpda = bis(4-cyanamidophenyl)diacetylene dianion (4) and bcpea = 9,10-bis(4-cyanamidophenylethynyl)anthracene dianion (5)) were synthesized in a stepwise manner starting from [Ru(tpy)(acac)(Ipcyd)] (1), where Ipcyd = 4-iodophenylcyanamide anion. Tetraphenylarsonium salts of the phenylcyanamide derivative ligands were also prepared. The four complexes have been characterized by UV-Vis, IR, ES-MS, electrochemistry and 1H NMR. Mononuclear complexes 2 and 3 were further characterized by 13C NMR. The single crystal X-ray structure of 2 was determined, it crystallized with one molecule of water with empirical formula of C32H31N5O5Ru, in a monoclinic crystal system and space group of P21/n with a = 17.642(5) Å, b = 9.634(2) Å, c = 20.063(7) Å, β = 92.65(3)°, V = 3406(2) Å3 and Z = 4. The structure was refined to a final R factor of 0.040. The Ru(III/II) couple of 1-3 appeared around 0.34 V versus the saturated calomel electrode in dimethylformamide and at a slightly higher potential, around 0.36-0.37 V for 4 and 5. Spectroelectrochemical studies were also performed for 4 and 5, no intervalence transition was observed despite all attempts. 相似文献
13.
A new phenoxo-bridged binuclear manganese(III) Schiff base complex, [Mn(L)(N3)]2 (1) where L = N,N′-bis(salicylidene)-1,2-propanediamine has been synthesized and characterized by IR, elemental analysis, crystal structure analysis and variable temperature magnetic susceptibility measurements. The single crystal X-ray diffraction reveals that the structure is dimeric with each phenolate oxygen atom acting as a bridge between two symmetry equivalent Mn atoms. Low temperature magnetic study shows that the complex exhibits intra-dimer ferromagnetic exchange and single-molecule-magnet (SMM) behavior as well. 相似文献
14.
《Inorganica chimica acta》2004,357(9):2561-2569
Ni(II), Cu(II), Zn(II) and Cd(II) complexes of an N4-donor Schiff base, containing (CH2)2 as spacer, have been prepared. The X-ray crystal structures of monohelical Ni(ETs) · H2O and the homochirally crystallised Δ-Cu(ETs), as well as the meso-helicate Zn2(ETs)2 · MeCN [H2ETs: N,N′-bis(2-tosylaminobenzylidene)-1,2-diaminoethane] have been solved. In the latter, the ligand behaves as bis-bidentate, displaying a “C”-type arrangement, instead of the typical “S”-type fashion present in bis-helical dinuclear complexes. 相似文献
15.
The copper(II) complex of the acyclic EBTA ligand (H4EBTA = 1,2-bis(2-aminoethoxy)benzene-N,N,N′,N′-tetraacetic acid) has been prepared and characterized by X-ray analysis. The two copper ions of the dinuclear unit present the same distorted octahedral coordination polyhedra. The EBTA ligand is shared between two copper coordination centres, with the formation of centrosymmetric dimers, which are linked in a supramolecular tridimensional structure via additional interactions through the coordinated waters molecules with adjacent carboxylic oxygen atoms. The stability and protonation constants of EBTA with Cu(II) and Zn(II) ions indicate a higher stability of these complexes with respect to the corresponding complexes with the more flexible EGTA ligand (H4EGTA = ethyleneglycol-bis(2-aminoethylether)-N,N,N′,N′-tetraacetic acid). On the other hand, the lower stability of [Gd(EBTA)]− than [Gd(EGTA)]− results in a decreased overall selectivity (lower Ksel) of EBTA towards Gd(III) and suggests that this complex may undergoes transmetallation reactions under physiological conditions. 相似文献
16.
Fatma Yuksel Ay?e Gül Gürek ?lke Gürol Erwann Jeanneau 《Inorganica chimica acta》2008,361(8):2225-2235
N,N′-Bis[allylamino]glyoxime, N,N′-bis[anilino]glyoxime, and N,N′-bis[1,2,3,4-tetrahydro-5-naphthalenamino]glyoxime have been prepared from corresponding amines and (E,E)-dichloroglyoxime. These ligands gave orange-red compound with NiCl2 in less acidic medium (pH ∼ 5) that are bis(E,E-dioximato)nickel(II) complexes {[(E,E)-Ni(HL)2]} (1a-3a) and green compounds in acidic medium (pH ∼ 2) that are tris(E,E-dioximato)nickel(II) dichloride complexes {[(E,E)-Ni(LH2)3]Cl2} (1b-3b). The crystal structures of all complexes have been determined by X-ray diffraction on a single crystal. The study of absorption spectra of these two types of complexes shows that they may be converted to each other by addition of acids (1a-3a) or bases (1b-3b) and there is no way for the amphi form. 相似文献
17.
The synthesis and characterization of Pd(II) complexes with the general formula cis-[Pd(L-O,S)2] (HL = N,N-diethyl-N′-benzoylthiourea, N,N-diisobutyl-N′-benzoylthiourea or N,N-dibenzyl-N′-benzoylthiourea) and trans-[PdCl2(HL-S)2] (HL = N,N-diphenyl-N′-benzoylthiourea, N,N-di-n-butyl-N′-benzoylthiourea or N,N-diisopropyl-N′-benzoylthiourea) are reported. These complexes were formed from the reaction between PdCl2 and N,N-di(alky/aryl)-N′-benzoylthiourea in acetonitrile with the formulation dependent on the nature of HL. The new Pd(II) complexes have been characterized by analytical and spectral (FT-IR, UV-Vis, 1H NMR and 13C NMR, Mass) techniques. The molecular structures of two of the complexes (1 and 5) have been conformed by X-ray crystallography. Complex 1 shows cytotoxicity against human breast cancer cells. 相似文献
18.
Preparation, crystal structures and magnetic properties of new heterodinuclear CuIIGdIII (1) and CuIITbIII (2) complexes [CuLn(L)(NO3)2(H2O)3MeOH]NO3·MeOH (where Ln = Gd, Tb) with the hexadentate Schiff-base compartmental ligand N,N′-bis(5-bromo-3-methoxysalicylidene)propylene-1,3-diamine (H2L = C19H20N2O4Br2) (0) have been described. Crystal structure analysis of 1 and 2 revealed that they are isostructural and form discrete dinuclear units with dihedral angle between the O1Cu1O2 and O1Gd1/Tb1O2 planes equal to 2.5(1)° and 2.6(1)°, respectively. The variable-temperature and variable-field magnetic measurements indicate that the metal centers in 1 and 2 are ferromagnetically coupled (J = 7.89 cm−1 for 1). Crystal and molecular structure of the Schiff base ligand (0) has been also reported. The complex formation changes the conformation of Schiff base ligand molecule. 相似文献
19.
Franz A. Mautner Masahiro Mikuriya Hideaki Ishida Febee R. Louka Salah S. Massoud 《Inorganica chimica acta》2009,362(11):4073-145
The one pot aqueous reaction of M(ClO4)2 (M = Cu2+ or Ni2+) with N-methylbis[2-(2-pyridylethyl)]amine (MeDEPA) and N,N′-dimethyl-N,N′-bis(2-pyridylmethyl)ethylenediamine (bpmen) and 1,4,7,10-tetraazacyclododecane (cyclen) in presence of sodium dicyanamide (Nadca) yielded dicyanamido-bridged polynuclear complex {[Cu(MeDEPA)(μ-1,5-dca)]ClO4}n (1), and two dinuclear complexes [Cu2(bpmen)2(μ-1,5-dca)]2(ClO4)5dca (2) and [Ni(cyclen)(μ-1,5-dca)]2(ClO4)2 (3). These complexes were characterized by IR and UV-Vis spectroscopy. Room temperature single-crystal X-ray studies have confirmed that the Cu(II) centers in 1 and 2 adopt geometries that are more close to trigonal bipyramidal (TBP) in 1 and close to square pyramidal (SP) in 2, whereas in 3, the Ni(II) centers are located in octahedral environment with doubly bridged μ-1,5-dca bonding mode. The intermolecular M···M distances in these complexes are in the range of 7.3-8.6 Å. Variable temperature magnetic susceptibility studies have confirmed that the dca-bridges mediate very weak antiferromagnetic interaction between the M(II) centers with J values of −0.35, −0.18 and −0.43 cm−1 for 1, 2 and 3, respectively. The results are compared and discussed in the light of other related bridged μ-1,5-dca Cu(II) and Ni(II) complexes. 相似文献
20.
Daniela Pucci Anna Bellusci Alessandra Crispini Mauro Ghedini Massimo La Deda 《Inorganica chimica acta》2004,357(2):495-504
Multifunctional Schiff base ligands Ln, namely the tetradentate N,N′-bis[2-hydroxy-5-(azopyridine)benzylidene]propylendiamine and the bidentate N-dodecyl-5-(azopyridine)salicylaldimine, both containing a flexible azo spacer, a metallation site and a terminal pyridine group, were synthetised and fully characterised. Mesogenic structures, analysed by polarised optical microscopy, DSC and powder X-ray diffraction, were obtained from self-assembly of the mono or bifunctional hydrogen-bond acceptors Ln with carboxylic acid donors. Ni(II) mono and bis-chelate, four- and six-coordinated, Ln derivatives were synthetised. The octahedral structure of the [Ni(py)2(L2)2] complex was confirmed by single crystal X-ray analysis. H-bonded self-assembly of Ni(II) complexes and carboxylic acids results in the formation of supramolecular networks whose structure and thermal stability were studied by DSC and powder X-ray diffraction analysis at variable temperatures. 相似文献