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1.
The molecular structure of 23,24,25,26,27,29,30-heptamethyl-19,28-oxahexacyclo[15.13.18.017,18.013,14.08,9.05,10]tetracos-3-yl acetate III. Compound III C32H52O3 crystallizes in the monoclinic crystal system with the unit cell parameters a = 13.265(15) ?, b = 6.481(7) ?, c = 32.274(4) ?, β = 99.333(2)°, space group C2, Z = 4, d = 1.176 g/cm3. Original Russian Text Copyright ? 2009 by N. I. Medvedeva, O. B. Flechter, and A. A. Korlyukov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 399–401, March–April, 2009.  相似文献   

2.
A new Schiff base, H2L, was prepared by condensation of 4,6-diacetylresorcinol with o-phenylenediamine in molar ratio 1?:?1. The ligand reacted with copper(II), nickel(II), cobalt(II), iron(III), zinc(II), oxovanadium(IV), and dioxouranium(VI) ions in the absence and presence of LiOH to yield mononuclear and homobinuclear complexes. The mononuclear dioxouranium(VI) complex [(HL)-(UO2)(OAc)(H2O)]·5H2O was used to synthesize heterobinuclear complexes. The ligand and its metal complexes were characterized by elemental analyses, IR, 1H-, and 13C-NMR, electronic, ESR and mass spectra, conductivity, and magnetic susceptibility measurements as well as thermal analysis. In the absence of LiOH, mononuclear complexes (1, 4, and 9) were obtained; in the presence of LiOH, binuclear complexes (3, 5, 7, and 10) as well as mononuclear complexes (2, 6, and 8) were obtained. In the mononuclear complexes, the coordinating sites are the phenolic oxygen, azomethine nitrogen, and amino nitrogen. In addition to these coordinating sites, the free carbonyl and phenolic OH are involved in coordination in binuclear complexes. The metal complexes exhibited octahedral, tetrahedral, and square planar geometries while the uranium is seven-coordinate. The antimicrobial and antioxidant activities of the ligand and its complexes were investigated. The ligand and the metal complexes showed antitumor activity against Ehrlich Acites Carcinoma.  相似文献   

3.
Two lanthanide complexes, (mnH)2[EuIII(egta)]2·6H2O (1) (H4egta = ethyleneglycol-bis-(2aminoethylether)-N,N,N,N′-tetraacetic acid) and (mnH)4[EuIII2(dtpa)2]·6H2O (2) (H5dtpa = diethylenetriamine-N,N,N,N″,N″-pentaacetic acid), have been synthesized and characterized by FT-IR spectroscopy, thermal analysis, and single-crystal X-ray diffraction. X-ray diffraction reveals that 1 is multinuclear nine-coordinate and crystallizes in the monoclinic crystal system with space group C2/c. The obtained cell dimensions are a = 38.513(3)?Å, b = 13.5877(8)?Å, c = 8.7051(5)?Å, β = 99.6780(10)°, and 4490.6(5)?Å3. Each methylamine (mnH+) cation in 1, through hydrogen bonds, connects three adjacent [EuIII(egta)]? anions. The [EuIII(egta)]? anions connect one another forming a 1-D multinuclear zigzag chain structure along the c-axis. Complex 2 is nine-coordinate binuclear structure with tricapped trigonal prismatic conformation and crystallizing in the monoclinic crystal system, but with space group P21/n. The obtained cell dimensions are a = 9.9132(8)?Å, b = 24.1027(18)?Å, c = 10.7120(10)?Å, β = 109.1220(10)°, and 2418.2(3)?Å3. For 2, there are two kinds of methylamine cations (mnH+) connecting [EuIII2(dtpa)2]4? complex anions and lattice waters through hydrogen bonds, leading to formation of a 2-D ladder-like layer structure.  相似文献   

4.
In this study, the Schiff base ligands H2L1–H2L3 and their CuII, CoII, NiII, FeIII RuIII and VOIV complexes have been prepared and characterized by spectroscopic and analytical techniques. All the complexes are mononuclear. Keto-enol tautomeric forms of the ligands have been investigated in polar and apolar solvents. The ligands favor the keto-form in the C7H8 and C6H14. The C–C coupling reaction of the 2,6-di-t-butylphenol has been investigated by the CoII and CuII complexes. Thermal properties of the complexes have been assessed using thermal techniques and similar properties were found. In the FeIII and RuIII complexes, firstly, the coordinated water molecule is lost from the complex; in the second step, the chloride ion leaves the molecule in the 300–350 °C temperature range. Finally, the complexes decompose to the appropriate metal oxide at the higher temperature ranges. The electrochemical properties of the complexes have been studied in the two different solvents (DMF and CH3CN).  相似文献   

5.
Preparation of the ligands HL1 = 2,6-[(N-phenylpiperazin-1-yl)methyl]-p-ethylphenol; HL2 = 2,6-[(N-phenylpiperazin-1-yl)methyl]-p-methoxyphenol and HL3 = 2,6-[(N-phenylpiperazin-1-yl)methyl]-p-nitrophenol are described together with their Cu(II) complexes with different bridging units. The exogenous bridges incorporated into the complexes are: hydroxo [Cu2L(OH)(H2O)2](ClO4)2.H2O (L1=1a, L2 =1b, L3 =1c), acetato [Cu2L(OAc)2]ClO4.H2O (L1 =2a, L2 =2b, L3 =2c) and nitrito [Cu2L1(NO2)2(H2O)2]ClO4.H2O (L1=3a, L2 =3b, L3 =3c). Complexes1a,1b,1c and2a,2b,2c contain bridging exogenous groups, while3a,3b,3c possess only open μ-phenolate structures. Both the ligands and complexes were characterized by spectral studies. Cyclic voltammetric investigation of these complexes revealed that the reaction process involves two successive quasireversible one-electron steps at different potentials. The first reduction potential is sensitive to electronic effects of the substituents at the aromatic ring of the ligand system, shifting to positive potentials when the substituents are replaced by more electrophilic groups. EPR studies indicate very weak interaction between the two copper atoms. Various covalency parameters have been calculated.  相似文献   

6.
Reaction of Co(OAc)2 · 4H2O with N-(2-hydroxybenzyl)salicylaldimine (H2La) in dimethylformamide (DMF)–H2O yields a linear trinuclear mixed valence complex [CoIII(μ-La)(μ-Lb)(μ-OAc)]2CoII · 2DMF (1). Here, HLb is salicylaldimine, which is afforded by an in situ transformation of H2La via cleavage of the C–N bond. Complex 1 has been characterized by X-ray crystallography as well as elemental analysis, UV-Vis, and IR spectroscopy. The cathodic and anodic responses of 1 in DMF appeared at ?1.46 V (CoIII → CoII, quasi-irreversible) and +0.99 V (CoII → CoIII, irreversible) versus saturated calomel electrode, respectively. The magnetic behavior of 1 has been analyzed by the one-ion approximation with spin–orbit coupling in Oh symmetry giving λ = ?121 cm?1.  相似文献   

7.
Seven new mononuclear complexes have been synthesized from 2,4-diiodo-6-propyliminomethyl-phenol in pyridine and Cu(OAc)2 · H2O, Ni(OAc)2 · 4H2O, Co(OAc)2 · 4H2O, Zn(OAc)2 · 2H2O, Cd(OAc)2 · 2H2O, Mn(OAc)2 · 4H2O, and Hg(OAc)2. The complexes were characterized by UV, IR, ESI-MS, and elemental analyses; bis(2,4-diiodo-6-propyliminomethyl-phenol)-pyridine-copper(II) (1) was characterized by X-ray crystallography. The central metal in each complex is five-coordinate by two nitrogens and two oxygens from two 3,5-diiodosalicylaldehyde Schiff-base ligands and one nitrogen from pyridine. The 3,5-diiodosalicylaldehyde Schiff base is bidentate. All the complexes were assayed for antibacterial (Bacillus subtilis, Staphylococcus aureus, Streptococcus faecalis, Pseudomonas aeruginosa, Escherichia coli, and Enterobacter cloacae) activities by the MTT method. Complex 1 showed the most favorable antimicrobial activity with minimum inhibitory concentrations of 6.25, 3.125, 6.25, 3.125, 6.25, 3.125 µg mL?1 against B. subtilis, S. aureus, S. faecalis, P. aeruginosa, E. coli, and E. cloacae, respectively.  相似文献   

8.
Na[YbIII(Cydta)(H2O)2] · 5H2O (1) (H4Cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid) and [YbIII(Hegta)] · 2H2O (2) (H4egta = ethyleneglycol-bis-(2-aminoethylether)-N,N,N′,N′-tetraacetic acid) were prepared and their composition and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques. Complex 1 crystallized in the triclinic crystal system with space group P 1; the YbIII is eight-coordinate by a hexadentate Cydta and two water molecules. Complex 2 is a protonated egta complex, crystallized in the monoclinic crystal system with space group P 2 1 /c; YbIII is coordinated only by the octadentate Hegta ligand. Both these complexes adopt a pseudo-square antiprismatic conformation.  相似文献   

9.
The complexation reactions between Mg2+,Ca2+,Sr2+ and Ba2+ metal cations with macrocyclic ligand, dicyclohexano-18-crown-6 (DCH18C6) were studied in methanol (MeOH)–water (H2O) binary mixtures at different temperatures using conductometric method . In all cases, DCH18C6 forms 1:1 complexes with these metal cations. The values of stability constants of complexes which were obtained from conductometric data show that the stability of complexes is affected by the nature and composition of the mixed solvents. While the variation of stability constants of DCH18C6-Sr 2+ and DCH18C6-Ba2+versus the composition of MeOH–H2O mixed solvents is monotonic, an anomalous behavior was observed for variations of stability constants of DCH18C6-Mg2+ and DCH18C6-Ca2+ versus the composition of the mixed solvents. The values of thermodynamic parameters (ΔHc°, ΔSc°) for complexation reactions were obtained from temperature dependence of formation constants of complexes using the van’t Hoff plots. The results show that in most cases, the complexation reactions are enthalpy stabilized but entropy destabilized and the values of thermodynamic parameters are influenced by the nature and composition of the mixed solvents. The obtained results show that the order of selectivity of DCH18C6 ligand for metal cations in different concentrations of methanol in MeOH–H2O binary system is: Ba2+>Sr2+>Ca2+> Mg2+.  相似文献   

10.
The crystal and molecular structures of the [PrIII(nta)(H2O)2]·H2O (nta = nitrilotriacetic acids), K3[GdIII(nta)2(H2O)]·6H2O, and K3[YbIII(nta)2]·5H2O complexes have been determined by single-crystal X-ray structure analyses. In [PrIII(nta)(H2O)2]·H2O, the PrIIINO8 part forms a nine-coordinate pseudo-monocapped square antiprismatic structure in which one N and three O atoms are from one nta ligand in the same molecule, three O atoms from another nta ligand in the neighboring molecule and two O atoms from two coordinate water molecules. In K3[GdIII(nta)2(H2O)]·6H2O, the [GdIII(nta)2(H2O)3- complex anion has a nine-coordinate pseudo-monocapped square antiprismatic structure in which each nta acts as a tetradentate ligand with one N atom of the amino group and three O atoms of the carboxylic groups. In K3[YbIII(nta)2]·5H2O, each nta also acts as a tetradentate ligand with one N atom of amino group and three O atoms of the carboxylic groups, but the [YbIII(nta)2 3- complex anion has an eight-coordinate structure with a distorted square antiprismatic prism. All the results including those for [TmIII(nta)(H2O)2]·2H2O confirm the inferences on the coordinate structures and coordination numbers of rare earth metal complexes with the nta ligand.  相似文献   

11.
Two rare-earth metal coordination compounds, (NH4)4[SmIII2(Httha)2]·16H2O (1) (H6ttha?=?triethylenetetramine-N,N,N,N′′,N′′′,N′′′-hexaacetic acid) and (NH4)4[SmIII2(dtpa)2]·10H2O (2) (H5dtpa?=?diethylenetriamine-N,N,N,N′′,N′′-pentaacetic acid), have been synthesized through reflux and characterized by FT-IR spectroscopy, thermal analysis, and single-crystal X-ray diffraction techniques. SmIII of (NH4)4[SmIII2(Httha)2]·16H2O (1) is nine-coordinate, forming tricapped trigonal prismatic coordination with three amine nitrogens and six oxygens, in which four oxygens are from one ttha and two from the other ttha. (NH4)4[SmIII2(Httha)2]·16H2O (1) crystallizes in the monoclinic crystal system with P2(1)/c space group. The crystal data are: a?=?13.9340(13) Å, b?=?22.890(3) Å, c?=?20.708(2) (14) Å, β?=?99.521(2)°, and V?=?6513.7(13) Å3. There are two –NH+– groups in the [SmIII2(Httha)2]4?. The polymeric (NH4)4[SmIII2(dtpa)2]·10H2O (2) also is nine-coordinate with tricapped trigonal prismatic conformation and crystallizes in the triclinic crystal system with P–1 space group. The cell dimensions are: a?=?9.8240(8) Å, b?=?10.0329(9) Å, c?=?13.0941(11) Å, β?=?77.1640(10)°, and V?=?1227.30(18) Å3. In (NH4)4[SmIII2(dtpa)2]·10H2O, there are two types of ammonium cations, which connect [SmIII2(dtpa)2]4? and lattice water through hydrogen bonds, leading to a 2-D ladder-like layer structure.  相似文献   

12.
Hqpzc has been synthesized by a highly efficient procedure using the ionic liquid TBAB as an environmentally benign reaction medium. [Cu(qpzc)(OAc)]·H2O (1) and [Zn(qpzc)(OAc)(H2O)] (2), complexes of the deprotonated ligand, qpzc¯ [qpzc¯ = N-(quinolin-8-yl)pyrazine-2-carboxamide], have been synthesized and characterized by elemental analyses, spectroscopic methods, and X-ray crystallography. The coordination geometry around the metal ions in both complexes is distorted square pyramidal. The mono-anionic qpzc¯ is a tridentate unsymmetrical ligand furnishing an N3 set, occupying three of the four basal positions. Acetate is a bidentate ligand in 1 and unidentate in 2. The apical position in 2 is occupied by water. Quite strong O-H…O hydrogen bonds create columns of complexes [rod group p21(11)] in the copper complex, but in conjunction with π-π interactions, a 3D edifice in the zinc complex. The electrochemical behavior of the ligand and its copper and zinc complexes shows that the quinoline ring reduces at more positive potentials in these complexes relative to the free ligand. The in vitro antibacterial activities of these complexes were tested against Escherichia Coli and Staphylococcus Aureus.  相似文献   

13.
Two dysprosium coordination compounds, (mnH)2[DyIII(Httha)]·3H2O (1) (H6ttha?=?triethylenetetramine-N,N,N′,N″,N′′′,N′′′-hexaacetic acid and mn?=?methylamine) and (enH2)3[DyIII(ttha)]2·9H2O (2) (en?=?ethylenediamine), were synthesized through direct heating and characterized by elemental analysis, FT-IR, thermal analysis, and single-crystal X-ray diffraction. X-ray diffraction analysis displays that 1 is a mononuclear nine-coordinate complex with a pseudo-monocapped square antiprismatic conformation (MCSAP) crystallizing in the monoclinic crystal system with P2(1)/c space group. The crystal data are as follows: a?=?16.1363(19)?Å, b?=?13.9336(11)?Å, c?=?13.6619(14)?Å, β?=?102.2490(10)°, and V?=?3001.8(5)?Å3. There are two kinds of methylamine cation in 1. They connect [DyIII(Httha)]2?and crystal waters through hydrogen bonds, leading to formation of a 2-D ladder-like layer structure. The polymeric 2 also is a nine-coordinate structure with a pseudo-MCSAP crystallizing in the monoclinic crystal system with P2/c space group. The cell dimensions are: a?=?17.7801(16)?Å, b?=?9.7035(10)?Å, c?=?22.096(2)?Å, β?=?118.874(2)°, and V?=?3338.3(6)?Å3. In 2 there are also two types of ethylenediamine cations. One connects three adjacent [DyIII(ttha)]3? complex anions through hydrogen bonds and the other is symmetrical forming hydrogen bonds with two neighboring [DyIII(ttha)]3? complex anions. These hydrogen bonds result in formation of a 2-D ladder-like layer structure as well.  相似文献   

14.
The synthesis of 1,2-C6H4(NHCOCMe2NHCO)2-3,3′-(2,2′-bpy) (3), a TAML (tetraamido macrocyclic ligand) incorporating the peripheral 2,2′-bipyridine unit, is described. Its geometry after optimization by density functional theory (DFT) indicated a rather unfavorable conformation of four N–H amide units for forming macrocyclic transition metal complexes. This explains why the iron(III) derivative of 3 could not be obtained even after deprotonation of the N–H bonds by n-BuLi. Nevertheless, the macrocyclic complex of CoIII was synthesized in moderate yield, characterized, and explored by DFT. Our data suggest a strongly distorted square-planar geometry of the macrocyclic complex between CoIII and 3. The dihedral angle between the pyridine rings equals 80° ruling out the possibility of metal chelation by the bipyridine unit.  相似文献   

15.
Reaction of [AuIII(C6F5)3(tht)] with RaaiR′ in dichloromethane medium leads to [AuIII(C6F5)3 (RaaiR′)] [RaaiR′=p-R-C6H4-N=N-C3H2-NN-l-R′, (1-3), R = H (a), Me (b), Cl (c) and R′= Me (1), CH2CH3 (2), CH2Ph (3), tht is tetrahydrothiophen]. The nine new complexes are characterised by ES/MS as well as FAB, IR and multinuclear NMR (1H,13C,19F) spectroscopic studies. In addition to dimensional NMR studies as1H,1H COSY and1H13C HMQC permit complete assignment of the complexes in the solution phase.  相似文献   

16.
A series of dinuclear DyIII acetate complexes containing three different hydrazine‐functionalized Schiff‐base ligands ( hmb , hmi, and hb ) have been synthesized by one‐pot reaction with Dy(OAc)3·4H2O as the metal precursor. [Dy2( hmb )2(OAc)4]·MeCN ( 1 ·MeCN) and [Dy2( hmi )2(OAc)2(MeOH)2]·H2O ( 2 ·H2O) with keto and enol forms of the corresponding ligands, respectively, were shown the similar core structures but different ratio of DyIII to OAc. Moreover, the different coordination environments of complex [Dy2( hb )2(μ‐OAc)2(OAc)2(H2O)2]·DMF·H2O ( 3 ·DMF·H2O) also offered an opportunity to understand the relationship between structural model and catalytic properties. Bimetallic dysprosium complexes 1 – 3 were demonstrated to be active catalysts for copolymerization of carbon dioxide (CO2) and cyclohexene oxide (CHO) without cocatalysts. To the best of our knowledge, well‐defined catalyst 2 appears to be the first example of an air‐stable bimetallic dysprosium complex that is effective for CO2/CHO copolymerization and the formation of the perfectly alternating poly(cyclohexenecarbonate) with a high molecular weight. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2017 , 55, 321–328  相似文献   

17.
18.
(NH4)[EuIII(pdta)(H2O)]?·?H2O has been synthesized and characterized by infrared spectrum, fluorescence spectrum, elemental analyses and single-crystal X-ray diffraction techniques. It crystallizes in the monoclinic system with space group P21/n, a?=?12.7700(15)?Å, b?=?9.3885(11)?Å, c?=?14.4070(18)?Å, α?=?90°, β?=?95.950(2)°, γ?=?90°, V?=?1718.0(4)?Å3, Z?=?4, M?=?508.28, D c?=?1.965?g?cm?3, μ?=?3.708?mm?1, F(000)?=?1108. The structure was refined to R 1?=?0.0238 for 3469 observed reflections (I?>?2σ(I)). The EuIIIN2O6 part in the [EuIII(pdta)(H2O)]? complex anion has an eight-coordinate structure with a distorted square anti-prismatic conformation, in which six coordination positions, two nitrogen atoms and four oxygen atoms are from one pdta (=propylenediaminetetraacetic acid) ligand, the seventh position is an oxygen (O(8A)) from another pdta and the eighth coordination site is occupied by a water molecule. (NH4)[EuIII(pdta)(H2O)]?·?H2O is the first eight-coordinate complex with a six-member ring in the rare earth metal complexes with aminopolycarboxylic acid ligands.  相似文献   

19.
The complex [MnIV(napbh)2] (napbhH2 = N-(2-hydroxynaphthalen-1-yl)methylenebenzoylhydrazide) reacts with activated ruthenium(III) chloride in methanol in 1 : 1.2 molar ratio under reflux, giving heterobimetallic complexes, [MnIV(napbh)2RuIIICl3(H2O)] · [RuIII(napbhH)Cl2(H2O)] reacts with Mn(OAc)2·4H2O in methanol in 1 : 1.2 molar ratio under reflux to give [RuIII(napbhH)Cl2(H2O)MnII(OAc)2]. Replacement of aquo in these heterobimetallic complexes has been observed when the reactions are carried out in the presence of pyridine (py), 3-picoline (3-pic), or 4-picoline (4-pic). The molar conductances for these complexes in DMF indicates 1 : 1 electrolytes. Magnetic moment values suggest that these heterobimetallic complexes contain MnIV and RuIII or RuIII and MnII in the same structural unit. Electronic spectral studies suggest six coordinate metal ions. IR spectra reveal that the napbhH2 ligand coordinates in its enol form to MnIV and bridges to RuIII and in the keto form to RuIII and bridging to MnII.  相似文献   

20.
Four new azocalix[4]arenes {5,11,17,23-tetrakis[(2-hydroxy-5-tert-butylphenylazo)]-25,26,27,28-tetrahydroxycalix[4]arene (1), 5,11,17,23-tetrakis[(2-hydroxy-5-nitro phenylazo)]-25,26,27,28-tetrahydroxycalix[4]arene (2), 5,11,17,23-tetrakis[(2-amino-5-carboxylphenylazo)]-25,26,27,28-tetrahydroxycalix[4]arene (3) and 5,11,17,23-tetrakis[(1-amino-2-hydroxy-4-sulfonicacidnapthylazo)]-25,26,27,28-tetrahydroxycalix[4]arene (4)} have been synthesized from p-tert-butylphenol, p-nitrophenol, p-aminobenzoic acid and 1-amino-2-hydroxy-4-sulphonic acid by diazo coupling reaction with p-aminocalix[4]arene. The resulting ligands (14) were treated with three transition metal salts (e.g., CuCl2·2H2O, NiCl2·6H2O or CoCl2·6H2O). Cu(II), Ni(II) and Co(II) complexes of the azocalix[4]arene derivatives were obtained and characterized by UV-vis, IR, 1H-NMR spectroscopic techniques and elemental analysis. All the complexes have a metal:ligand ratio of 2:1. The Cu(II) and Ni(II) complexes of azocalix[4]arenes are square-planar, while the Co(II) complexes of azocalix[4]arenes are octahedral with water molecules as axial ligands. The solvent extraction of various transition metal cations from the aqueous phase to the organic phase was carried out by using azocalix[4]arenes (14). It was found that, azocalix[4]arenes 1, 2 and 3 examined selectivity for transition metal cations such as Ag+, Hg+ and Hg2+. In addition, the thermal stability of metal:azocalix[4]arene complexes were also reported. Dedicated to Prof. Dr. Mustafa Yılmaz on the occasion of his 50th birthday  相似文献   

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