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1.
A covalent mononuclear complex, [Cu(p–HOC6H4COO)2(cyclam)] (1), and two ionic mononuclear complexes, [Cu(cyclam)(H2O)2](p–CH3OC6H4COO)2 (2) and [Cu(cyclam)(H2O)2](p–CH3(CH2)15OC6H4COO)2·H2O (3), were formed from reaction of cyclam with [Cu2(p–HOC6H4COO)4(H2O)2], [Cu2(p–CH3OC6H4COO)4(H2O)2] and [Cu2(p-CH3(CH2)15OC6H4COO)4(H2O)2], respectively. These complexes were isolated as purple crystals with molecular structures showing distorted octahedral N4O2 geometry. Complexes 1 and 2 were irreversibly reduced to Cu(I) and oxidized to Cu(III), while 3 was redox inactive. Complex 2 reacted with N-(hexadecyl)isonicotinamide (L) to form [Cu(cyclam)(L)2](p–CH3OC6H4COO)2 (4). These complexes were thermally stable (Tdec > 200 °C for 13 and 174 °C for 4). Complexes 3 and 4 behaved as ionic liquids (melting temperatures lower than 100 °C) and exhibited mesomorphism.  相似文献   

2.
A new μ3-oxo trinuclear chromium(III) propionate cluster, [Cr33-O)(O2CCH2CH3)6(pyr)3]NO3·0.25(H2O) (1), has been synthesized by reaction of a μ3-oxo trinuclear chromium(III) propionate precursor [Cr33-O)(O2CCH2CH3)6(H2O)3]NO3 with a pyrazol ligand (pyr) and characterized by IR spectroscopy, single-crystal X-ray structure determination, and thermal analysis. Magnetic susceptibility and magnetization studies revealed antiferromagnetic exchange interactions within the trinuclear Cr(III) cluster (J = ?11.9 cm?1) and determined the electronic ground state (S = ½) of the compound.  相似文献   

3.
By selecting appropriate ligands, two polyoxidovanadate complexes, [Ni(en)2]3[V18O42Cl]·7H2O·2H3O+ (1) and [H2N(CH3)2]3[PV14O42]·2TMP·6H3O+ (2), have been synthesized at different pH values using V2(SO4)3, Ni(CH3COO)2, and H6TTHA (for 1), VO(acac)2 and TPP (for 2) (en = C2H8N2, TPP = thiamine pyrophosphate, TMP = thiamine monophosphate, H6TTHA = 1,3,5-triazine-2,4,6-triamine hexaacetic acid). The complexes have been characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis (TG), and single crystal X-ray diffraction. The complexes catalyze the oxidation of the organic substrate phenol red in the presence of H2O2 and bromide, and the reaction system is considered as a model for hydrogen peroxide determination. The reaction rate constants (k) for 1 and 2 are calculated as 3.729 × 103 and 4.083 × 103 (mol L)?2 s?1. The maximum conversion rate of phenol red for 1 is 83.32%, while for 2 is 81.12%.  相似文献   

4.
Three new dialkytin complexes, {[o-OH–C6H4(O)C=N–N=C(CH2Ph)COO](n-Bu2Sn)}n (1), {[o-OH–C6H4(O)C=N–N=C(CH2Ph)COO](MeOH)(p-MeC6H5CH2)2Sn}2 (2), and {[o-OH–C6H4(O)C=N–N=C(CH2Ph)COO](EtOH)(C6H5CH2)2Sn}2 (3), were synthesized by reactions of 2-oxo-3-phenylpropionic acid salicyloylhydrazone with the corresponding diorganotin(IV) complex, respectively. All the complexes were characterized by IR, 1H, 13C, 119Sn NMR spectra, elemental analysis, X-ray single crystal diffraction and TGA. For in vitro antitumor activities, complexes were evaluated by the MTT assay against three human cancer cell lines (NCI-H460, HepG2 and MCF7) and human cell line (HL7702). The results showed that 1 may be a better potential candidate for further chemical optimization and cancer therapy than 2 and 3. The interactions between the complexes and calf thymus DNA were studied; the interaction of 1 with calf thymus DNA was intercalation, 2 and 3 were intercalation and electrostatic binding.  相似文献   

5.
A family of phenoxo-bridged heterometallic Schiff base trinuclear complexes, [Fe2LnL2(C3H7COO)(H2O)]·CH3OH·CH3CN·H2O (Ln = Sm, 1; Gd, 2; Tb, 3; Dy, 4) is reported. Those complexes were afforded by “one-pot” reaction of a polydentate Schiff base ligand 2-hydroxy-3-methoxy-phenylsalicylaldimine (H2L) with Fe(NO3)3·9H2O, Ln(NO3)3·6H2O and sodium butyrate (C3H7COONa) in a mixture of methanol and acetonitrile in the presence of triethylamine as a base. Single-crystal X-ray diffraction analysis reveals that the structures of the four complexes are isomorphic. In each complex, two anionic [FeL2]? units coordinate to the central lanthanide ion as a tetradentate ligand using its four phenoxo oxygens, forming a two-blade propeller-like molecular shape. Magnetic properties of 1–4 were investigated using variable temperature magnetic susceptibility, and weak ferromagnetic exchange between the FeIII and LnIII ions has been established for the Gd derivative. The Tb and Dy complexes show no evidence of slow relaxation behavior above 2.0 K.  相似文献   

6.
Three new polynuclear compounds based on a dicarboxylic acid ligand are reported. In particular, two Cu(II) coordination compounds, [Cu2(H2O)6(Hbzlidp)2](CF3SO3)2·2H2O (1) and [Cu(NO3)(Hbzlidp)] (2) (bzlidp2? = N-benzyliminodipropionate anion), and a Ni(II) dinuclear compound, [Ni2(H2O)4(bzlidp)2] (3), were synthesized and characterized by IR spectroscopy, elemental analysis and single crystal X-ray diffraction. Different structures were obtained depending on the reaction conditions. The structural analyses reveal that 1 was formed by dinuclear [Cu2(H2O)6(Hbzlidp)2]2+ units built by two copper(II) ions joined through two Hbzlidp? ligands, while 2 was formed by pairs of Cu(II) centers bridged by four syn,syn carboxylate groups to generate “paddle wheel” units. The dinuclear copper units are arranged in a rhombus type grid, in a 2-D layer structure. In both cases, the N was protonated and not coordinated to the metal center. Compound 3 was formed by [Ni2(H2O)4(bzlidp)2] neutral dinuclear units, with octahedral Ni(II) centers. Solution studies of the ligand–M(II) systems (M(II) = Mn, Co, Ni, Cu, Zn, Cd, and Pb) were also carried out.  相似文献   

7.
Two cadmium(II) coordination compounds, [Cd3(CH3CO2)4(ad)2(CH3CN)2]n (1) and [Cd3(5-SIP)2(H-ad)2(H2O)6]n (2) (H-ad = adenine and 5-SIP = 5-sulfoisophthalate), were synthesized and characterized. Compound 1 features a two-dimensional (2-D) layered structure based on linear trinuclear [Cd3(CH3CO2)4] units bridged by monoanionic adenine ligands. In 2, the 5-SIP3? ligands link Cd(II) ions to form a one-dimensional (1-D) ladder, which is further linked by neutral adenine ligands to give a 2-D layered structure. In both structures, the carboxylate ligands link Cd(II) ions to form low-dimensional structures, which are further connected by adenine ligands to give high-dimensional structures. Compounds 1 and 2 exhibit emissions centered at 382 and 416 nm, respectively, which can be attributed to the ligand centered ππ* transition.  相似文献   

8.
Three pyridylbenzimidazoles (2-PBIM, 3-PBIM, and 4-PBIM) have been prepared (2-PBIM: 2-(2-pyridyl)-benzimidazole, 3-PBIM: 2-(3-pyridyl)-benzimidazole, 4-PBIM: 2-(4-pyridyl)-benzimidazole). Reactions of several transition metals (Cd2+, Cu2+, Fe2+) with the three ligands gave four new coordination complexes, [(Cd)2(2-PBIM)2(CH3COO)4] (1), [Cu(3-PBIM)2(CH3COO)2]?·?2H2O (2), [Cu(4-PBIM)2(CH3COO)2(H2O)]?·?H2O (3), and [Fe(4-PBIM)2(Cl)2(H2O)2] (4), respectively. These four complexes have been characterized by X-ray crystallography, IR spectroscopy, and UV absorption spectroscopy. Thermogravimetric properties of 2 and 4 were also measured. X-ray crystallographic studies reveal that these four complexes are very different, although the ligands are similar in structure. The role of hydrogen-bonding and π–π interactions in extending dimensionality of simple complexes has been discussed.  相似文献   

9.
Two tetranuclear nickel(II) complexes, [Ni4 (p-BrPhHIDC)4(py)4(H2O)4]·CH3OH (p-BrPhH3IDC = 2-(p-bromophenyl)-1H-imidazole-4,5-dicarboxylic acid) (1) and [Ni4(p-ClPhHIDC)4 (CH3CN)4(H2O)4]·4H2O (p-ClPhH3IDC = 2-(p-chlorophenyl)-1H-imidazole-4,5-dicarboxylic acid, py = pyridine) (2), have been solvothermally synthesised and structurally characterised. Both compounds consist of similar tetranuclear Ni(II) cores, in which the imidazole dicarboxylate ligands adopt the similar coordination mode. The thermal properties of 1 and 2 have been investigated. Also, it is discovered that there exists antiferromagnetic coupling between the Ni(II) ions in 1 and 2; the best fittings to the experimental magnetic susceptibilities gave J = ? 9.89 cm? 1 and g = 2.18 for 1, and J = ? 10.54 cm? 1 and g = 2.14 for 2.  相似文献   

10.
A series of cation–anion complexes derived by 2,2′-dipyridylamine (Hdpa) and carboxylate ligands with formulas [Ni(Hdpa)2(CH3COO)]Cl(CH3OH) (1), [Co(Hdpa)2(CH3COO)]Cl(CH3OH) (2), [Ni(Hdpa)2(CH3CH2CH2COO)]Cl (3), [Co(Hdpa)2(CH3CH2CH2COO)]Cl (4), [Ni(Hdpa)2(C6H5COO)]Cl (5), and [Co(Hdpa)2(C6H5COO)]Cl (6), were synthesized and characterized by IR, elemental analysis, MS(ESI), TG analysis, UV-Vis, and fluorescence spectra. X-ray single crystal structural analysis showed that the coordination geometries of metal ions in these complexes are similar and they are cation–anion species. The hydrogen-bonding structures are 1-D chains through the N–H···Cl bonds. There are weak stacking interactions between pyridine rings in 14, while there are no stacking interactions in 5 and 6. We have investigated the transesterification of phenyl acetate with methanol catalyzed by 16 under mild conditions; 14 are homogeneous catalysts while 5 and 6 are heterogeneous catalysts due to their poor solubility in methanol. Cobalt complexes exhibit higher catalytic activities than corresponding nickel complexes. Complex 4 is the best catalyst of these six complexes.  相似文献   

11.
Four diiron toluenedithiolate complexes 25 with monophosphine ligands are reported. Treatment of [μ-SC6H3(CH3)S-μ]Fe2(CO)6 (1) with tris(3-chlorophenyl)phosphine, tris(4-chlorophenyl)phosphine, tris(4-methylphenyl)phosphine or 2-(diphenylphosphino)benzaldehyde, and Me3NO?2H2O in MeCN resulted in the formation of [μ-SC6H3(CH3)S-μ]Fe2(CO)5[P(3-C6H4Cl)3] (2), [μ-SC6H3(CH3)S-μ]Fe2(CO)5[P(4-C6H4Cl)3] (3), [μ-SC6H3(CH3)S-μ]Fe2(CO)5[P(4-C6H4CH3)3] (4), and [μ-SC6H3(CH3)S-μ]Fe2(CO)5[Ph2P(2-C6H4CHO)] (5) in 64–82% yields. Complexes 25 have been characterized by elemental analysis, IR, 1H NMR, 31P{1H} NMR, 13C{1H} NMR and further confirmed by single crystal X-ray diffraction analysis. The molecular structures show that 25 contain a butterfly diiron toluenedithiolate cluster coordinated by five terminal carbonyls and an apical monophosphine.  相似文献   

12.

Crystal structure determinations on the uranyl ion complexes [H2N(CH3)2]2[UO2(bpdc)2], (1), (bpdc?=?2,2′-bipyridine-3,3′-dicarboxylate), [pyH]2[UO2(btfac)(NO3)2](NO3), (2), (btfac?=?1-phenyl-4,4,4-trifluorobutane-1,3-dionate), [H2dabco][UO2(nta)]2·3H2O, (3), (dabco?=?1,4-diazabicyclo[2.2.2]octane; nta?=?nitrilotriacetate) and [Ni(cyclam)UO2(edta)].2H2O, (4), (cyclam?=?1,4,8,11-tetrazacyclotetradecane; edta?=?ethylenediaminetetraacetate) have provided further examples of U(VI) in tetragonal-, pentagonal and hexagonal-bipyramidal coordination environments. Consideration of each structure within the context of those of known relatives has been used to assess the influence of factors in addition to repulsions within the primary coordination sphere on the equatorial coordination number of U(VI).

  相似文献   

13.
A series of novel cationic gemini surfactants, p-[C n H2n+1N+(CH3)2CH2CH(OH)CH2O]2C6H4·2Cl? [A(n = 12), B(n = 14) and C(n = 16)], containing a spacer group with two flexible and hydrophilic groups (2-hydroxy-1,3-propylene) on both sides of a rigid and hydrophobic group (1,4-dioxyphenylene) has been synthesized by the reaction of hydroquinone diglycidyl ether with N,N-dimethylalkylamine and N,N-dimethylalkylamine hydrochloride. Their surface-active properties have been investigated by surface tension measurement. The critical micelle concentration (cmc) values of the synthesized cationic gemini surfactants are one order of magnitude lower than those of their corresponding monomeric surfactants (C n H2n + 1N+(CH3)3·Cl?). Both the cmc and surface tension at the cmc (γcmc) of A are lower than those of p-[C12H25N+(CH3)2CH2]2C6H4·2Cl? (D). The novel cationic gemini surfactants A and B also show good foaming properties.  相似文献   

14.
Three kinds of trinuclear metal string complexes, [Ni3(dpa)4(L1)2]?·?H2O?·?C2H5OH (L1?=?(E)-3-(2-hydroxyl-phenyl)-acrylic acid) (1), [Ni3(dpa)4(L2)2]?·?2C2H5OC2H5 (L2?=?(E)-3-(3-hydroxyl-phenyl)-acrylic acid) (2) and [Ni3(dpa)4(L3)2]?·?3CH2Cl2?·?1.5CH3OH (L3?=?(E)-3-(4-hydroxyl-phenyl)-acrylic acid) (3). (dpa??=?bis(2-pyridyl)amido), have been synthesized. The structures of 1 and 2 have been analyzed by the X-ray single-crystal diffraction showing hydrogen-bonded networks.  相似文献   

15.
16.
Single crystals of (H3O)[UO2(CH3COO)3] (I) and (NH(C2H5)3)[UO2(CH3COO)3] (II) are synthesized, and their structures are studied by X-ray crystallography. Compound I crystallizes in the tetragonal crystal system with the unit cell parameters a = 13.70640(10) ?, c = 27.5258(5) ?, V = 5171.14(11) ?3, space group I41/a, Z = 16, R = 0.0238. The crystals of compound II are orthorhombic with the parameters a = 13.3685(3) ?, b = 10.6990(3) ?, c = 12.2616(3) ?, V = 1753.77(8) ?3, space group Pna21, Z = 4, R = 0.0228. The uranium-containing structural units of crystals I and II are [UO2(CH3COO)3] island mononuclear groups belonging to the A B301(A = UO22+, B01 = CH3COO) crystal-chemical group of uranyl complexes. [UO2(CH3COO)3] complexes are linked into a three-dimensional framework by electrostatic interactions with the outer-sphere cations and by hydrogen bonds involving the hydrogen atoms of hydroxonium (I) or triethylammonium (II) with the oxygen atoms of the acetato groups.  相似文献   

17.
The title dinuclear CuII complex, [Cu2(C7H8NO2)2(C7H9NO2)2](CH3COO)2, has been synthesized by the reaction of Cu(CH3COO)2·H2O with pdmH2 (pdmH2 is pyridine‐2,6‐diyldi­methanol) in the presence of tetra­butyl­ammonium hydro­xide. The title complex contains a centrosymmetric Cu2O2 core and each CuII atom has distorted octahedral geometry. Molecular [Cu2(pdmH)2(pdmH2)]2+ cations are connected by hydrogen bonds involving the CH3COO anions, forming one‐dimensional chains along the a axis.  相似文献   

18.
Abstract

We report the two-step synthesis of a chiral rod-like metal-organic framework (MOF). The chemical approach consists on the use of a previously prepared oxamato-based homochiral hexanuclear wheel, the ligand being a derivative of the natural amino acid l-alanine, with formula (Me4N)6{CuII6[(S)-alama])6}·10H2O (1) [where (S)-alama=(S)-N-(ethyl oxoacetate)alanine]. The anionic hexacopper(II) wheels, stabilized by the presence of templating tetramethylammonium counter-cations, disassemble in the presence of cationic square-planar [Ni(cyclam)]2+ complexes to yield, after a supramolecular reorganization process that involves axial coordination of the [Ni(cyclam)]2+ cations through the free carbonyl groups of the copper(II) moieties, a neutral chiral rod-like, three-dimensional (3D) MOF with formula [Ni(cyclam)][Cu(S)-alama]2·16H2O (2). The resulting MOF constitutes one of the few examples where such a high-nuclearity metal complex is used as precursor for the construction of rod-like MOFs.  相似文献   

19.
Coordination Polymeric 1, 2‐Dithiooxalato and 1, 2‐Dithiosquarato Complexes. Syntheses and Structures of [BaCr2(bipy)2(1, 2‐dtox)4(H2O)2], [Ni(cyclam)(1, 2‐dtsq)]·2DMF, [Ni(cyclam)Mn(1, 2‐dtsq)2(H2O)2]·2H22, and [H3O][H5O2][Cu(cyclam)]3[Cu2(1, 2‐dtsq)3]2 1, 2‐Dithioxalate and 1, 2‐dithiosquarate ions have a pair of soft and hard donor centers and thus are suited for the formation of coordination polymeric complexes containing soft and hard metal ions. The structures of four compounds with building blocks containing these ligands are reported: In [BaCr2(bipy)2(1, 2‐dtox)4(H2O)2] Barium ions and pairs of Cr(bipy)(1, 2‐dtox)2 complexes form linear chains by the bisbidentate coordination of the dithiooxalate ligands towards Ba2+ and Cr3+. In [Ni(cyclam)(1, 2‐dtsq)]·2DMF short NÖH···O hydrogen bonds link the NiS2N4‐octahedra with C2v‐symmetry to an infinite chain. In [Ni(cyclam)Mn(1, 2‐dtsq)2(H2O)2]·2H2O the 1, 2‐dithiosquarato ligand shows a rare example of S‐coordination towards manganese(II). The sulfur atoms of cis‐MnO2S4‐polyedra are weakly coordinated towards the axial sites of square‐planar NiN4‐centers, thus forming a zig‐zag‐chain of Mn···Ni···Mn···Ni polyhedra. [H3O][H5O2][Cu (cyclam)]3[Cu2(1, 2‐dtsq)3]2 contains square planar [CuII(cyclam)]2+ ions and dinuclear [CuI2(1, 2‐dtsq)3]4— ions. Here each copper atom is trigonally planar coordinated by S‐donor atoms of the ligands. The Cu…Cu distance is 2.861(4)Å.  相似文献   

20.

Abstract  

Reactions of the pyridyl side-chain-functionalized cyclopentadiene [C5H5CR2(CH2C5H4N)] [R 2 = Et2 (1), (CH2)4 (2)] with Ru3(CO)12 in refluxing xylene gave the new intramolecular C–H activated trinuclear product [μ-(C5H3N)CH2C(C2H5)2(C5H4)Ru(CO)]2Ru(CO)2 (3) and the normal dinuclear metal complex [(C5H4N)CH2C(CH2)4(C5H4)Ru(CO)]2(μ-CO)2 (4). The structures of the trinuclear complex 3 and dinuclear complex 4 were characterized by elemental analysis, IR spectra, 1H-NMR and X-ray diffraction.  相似文献   

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