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1.
This report describes the synthesis and structural analysis of stable copper(II) cysteine complexes. Pale pink copper(II) cysteine complexes were synthesized in mole ratios of 1:2, 1:4, and 1:6 of copper(II):cysteine in ethanol. Infrared spectroscopy and X-ray absorption spectroscopy confirmed that copper(II) binding occurred via the thiol ligand of cysteine. XANES analysis showed that the oxidation state of copper remained as copper(II) and the local atomic geometry was similar in all of the cysteine complexes. The EXAFS data indicate that the copper(II) cysteine complexes are forming ring type structures with sulfur ligands from the cysteines acting as bridging ligands. X-ray diffraction revealed that the copper(II) cysteine complexes formed monoclinic cells with maximum crystallinity found in the 1:4 copper(II):cysteine complex. 相似文献
2.
Siti Mutrofin Peter C. Healy Jean Ngoune Riccardo Pettinari Brian W. Skelton 《Inorganica chimica acta》2008,361(8):2365-2374
Syntheses, spectroscopic and structural characterizations of a series of Cu(I)-phenanthroline complexes are reported. A single crystal X-ray structure determination is recorded for CuNO3:dmp:MeCN (1:1:1), ‘dmp’ = 2,9-dimethyl-1,10-phenanthroline, showing it to be isomorphous with its previously studied tetrafluoroborate, perchlorate and hexafluorophosphate, and silver(I) perchlorate counterparts, the metal atom lying in a trigonal planar [(N∧N)Cu(NCMe)] coordination environment, the anion not being coordinated. Structure (re-) determinations are also reported for a number of salts of the [Cu(dmp)2]+ cation: the perchlorate, isomorphous with numerous other salts, not only of copper(I), but also lithium(I)), also the unsolvated nitrate, and a solvated form of the chloride. 相似文献
3.
New 1,10-phenanthroline derivatives bearing diarylamino and heteroaromatic moieties in the 3,8-position have been prepared by a palladium-catalyzed C-N bond formation reaction. Formation of Ru(II) complexes with the chelating ligands and their photophysical and electrochemical redox properties have been examined. 相似文献
4.
《Journal of enzyme inhibition and medicinal chemistry》2013,28(3):359-366
A series of ternary copper(II) complexes have been derived using levofloxacin and five phenanthroline derivatives. Complexes were characterized using infrared spectroscopy, Thermogravimetric (TG)-analysis, fast atom bombardment mass spectroscopy and reflectance spectra. Synthesized complexes exhibit the only d-d band at ~ 666?nm points toward a distorted square pyramidal geometry at metal centre with one unpaired electron responsible for paramagnetic behaviour of whole moiety. Binding behaviour of the complexes toward Herring Sperm DNA were determined using ultraviolet-Vis (UV-Vis) absorption titration and viscometric titration experiment, where as the cleavage efficacy of the complexes toward pUC19 DNA was determined by electrophoresis in presence of ethidium bromide. Complexes exhibit superoxide dismutase–like activity with their IC50 values ranging from 0.7917 to 1.7432 µM. 相似文献
5.
Ruíz P Ortiz R Perelló L Alzuet G González-Alvarez M Liu-González M Sanz-Ruíz F 《Journal of inorganic biochemistry》2007,101(5):831-840
Three new binary Cu(II) complexes of norfloxacin have been synthesized and characterized. We also report the synthesis, characterization and X-ray crystallographic structures of a new binary compound, [Cu(HNor)(2)]Cl(2).2H(2)O (2) and two new ternary complexes norfloxacin-copper(II)-phen, [Cu(Nor)(phen)(H(2)O)](NO(3)).3H(2)O (4), and [Cu(HNor)(phen)(NO(3))](NO(3)).3H(2)O (5). The structure of 2 consists of two crystallographically independent cationic monomeric units of [Cu(HNor)(2)](2+), chloride anions, and uncoordinated water molecules. The Cu(II) ion is placed at a center of symmetry and is coordinated to two norfloxacin ligands which are related through the inversion center. The structures of 4 and 5 consist of cationic units ([Cu(Nor)(phen)(H(2)O)](+) for 4 and [Cu(HNor)(phen)(NO(3))](+) for 5), nitrate counteranions, and lattice water molecules that provide crystalline stability through a network of hydrogen-bond interactions. The complexes exhibit a five coordinated motif in a square pyramidal environment around the metal center. The ability of compounds 4 and 5 to cleave DNA has also been studied. Mechanistic studies with different inhibiting reagents reveal that hydroxyl radicals, singlet oxygen, and superoxide radicals are all involved in the DNA scission process mediated by these compounds. 相似文献
6.
Cytotoxic tests recently performed at National Cancer Institute, NCI (USA), on [Cu(HPIR)(2)(DMF)(2)], 1, (H(2)PIR=piroxicam, 4-hydroxy-2-methyl-N-pyridin-2-yl-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide) a widely used non-steroidal anti-inflammatory drug, NSAID [see R. Cini, G. Giorgi, A. Cinquantini, C. Rossi, M. Sabat, Inorg. Chem. 29 (1990) 5197-5200, for synthesis and structural characterization, DMF=dimethylformamide] (NSC #624662) by using a panel of ca. 50 human cancer cells, showed growth inhibition factor GI(50) values as low as 20microM against several cancer lines, with an average value 54.4microM. The activity of 1 is larger against ovarian cancer cells, non-small lung cancer cells, melanoma cancer cells, and central nervous system cancer cells. The widely used anticancer drug carboplatin (cis-diammine(1,1-cyclobutanedicarboxylato)platinum(II)) (NSC #241240) has average GI(50) value of 102microM. The reactions of copper(II)-acetate with other NSAIDs from the oxicam family were tested and crystalline complexes were obtained and characterized. Isoxicam (H(2)ISO=4-hydroxy-2-methyl-N-(5-methylisoxazol-3-yl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide) produced [Cu(HISO)(2)].0.5DMF, 2.0.5DMF (DMF=dimethylfomamide). The coordination arrangement is square-planar and the HISO(-) anions behave as ambi-dentate chelators via O(amide),N(isoxazole) and O(enolate),O(amide) donors. Meloxicam (H(2)MEL=4-hydroxy-2-methyl-N-(5-methyl-1,3-thiazol-2-yl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide) produced [Cu(HMEL)(2)(DMF)].0.25H(2)O, 3.0.25H(2)O. The coordination arrangement is square-pyramidal, the equatorial donors being O(amide),N(thiazole) from two HMEL(-) anions and the apical donor being O(DMF). Unexpectedly, cinnoxicam (HCIN=2-methyl-1,1-dioxido-3-[(pyridin-2-ylamino)carbonyl]-2H-1,2-benzothiazin-4-yl-(3-phenylacrylate)) produced [Cu(MBT)(2)(PPA)(2)] (MBT=3-(methoxycarbonyl)-2-methyl-2H-1,2-benzothiazin-4-olate 1,1-dioxide, PPA=3-phenyl-N-pyridin-2-ylacrylamide). 相似文献
7.
The mononuclear dipeptide‐based CuII complexes [CuII(trp‐phe)(phen)(H2O)] ⋅ ClO4 ( 1 ) and [CuII(trp‐phe)(bpy)(H2O)] ⋅ ClO4 ( 2 ) (trp‐phe=tryptophanphenylalanine, phen=1,10‐phenanthroline, bpy=2,2′‐bipyridine) were isolated, and their interaction with DNA was studied. They exhibit intercalative mode of interaction with DNA. The intercalative interaction was quantified by Stern Volmer quenching constant (Ksq=0.14 for 1 and 0.08 for 2 ). The CuII complexes convert supercoiled plasmid DNA into its nicked circular form hydrolytically at physiological conditions at a concentration as low as 5 μM (for 1 ) and 10 μM (for 2 ). The DNA hydrolysis rates at a complex concentration of 50 μM were determined as 1.74 h−1 (R=0.985) for 1 and 0.65 h−1 (R=0.965) for 2 . The rate enhancement in the range of 2.40–4.10×107‐fold compared to non‐catalyzed double‐stranded DNA is significant. This was attributed to the presence of a H2O molecule in the axial position of the Cu complexes. 相似文献
8.
Eleni K. Efthimiadou Nikos Katsaros Alexandra Karaliota George Psomas 《Inorganica chimica acta》2007,360(15):4093-4102
The neutral mononuclear copper(II) complexes with the quinolone antibacterial drugs, pipemidic acid and N-propyl-norfloxacin, in the presence or absence of nitrogen-donor heterocyclic ligands, 2,2′-bipyridine, 1,10-phenanthroline or 2,2′-dipyridylamine, have been prepared and characterized spectroscopically. The interaction of copper(II) with the deprotonated quinolone ligand leads to the formation of the neutral mononuclear complexes of the type [Cu(quinolone)2(H2O)] (1)–(2) while the presence of the N-donor ligand leads to the formation of the neutral mononuclear complexes of the type [Cu(quinolone)(N-donor)Cl] (3)–(8). In all the complexes, copper(II) is pentacoordinate having a distorted square pyramidal geometry. The electron paramagnetic resonance spectra of 1 and 2 are typical of mononuclear Cu(II) complexes, while for the mixed-ligands complexes 3–8 a mixture of dimeric and monomeric species is indicated. The interaction of the complexes with calf-thymus DNA has been investigated with diverse spectroscopic techniques and has shown that the complexes can be bound to calf-thymus DNA by the intercalative mode. The antimicrobial activity of the complexes has been tested on three different microorganisms. All the complexes show an increased biological activity in comparison to the corresponding free quinolone ligand. 相似文献
9.
The reaction of CuCl2 · 2H2O with 2,6-bis(1-phenyliminoethyl)pyridine (referred hereafter as L) in 1:1 molar ratio in methanol or acetronitrile at room temperature afforded distorted trigonal-bipyramidal complex [Cu(κ3-L)Cl2]. On the other hand, the reaction of NiCl2 · 6H2O with 2 equivalents of L gave an octahedral complex [Ni(κ3-L)2]2+, which was isolated as [Ni(κ3-L)2][BF4]2 using NH4BF4. The complexes have been characterized by elemental analyses, FAB-MS, IR, EPR and electronic spectral studies. Molecular structures of both the [Cu(κ3-L)Cl2] (1) and [Ni(κ3-L)2](BF4)2 (2) have been determined by single crystal X-ray analyses. Weak interaction studies on 1 and 2 revealed stabilisation of the crystal packing by inter and intra-molecular C-H?X (X = F, Cl, π) interactions. In complex 2 ortho C-H bond from phenyl rings leads to unexpected C-H?π interaction with nickel α,α′-diimine chelate ring. This provides structural support for metalloaromaticity in the chelate ring of complex 2. 相似文献
10.
Nenad Filipovi? Tamara Todorovi? Vojislav Spasojevi? Irena Novakovi? 《Inorganica chimica acta》2009,362(6):1996-28
Three novel copper(II) complexes as condensation derivatives of 2-pyridinecarboxaldehyde, 2-acetylpyridine or 2-quinolinecarboxaldehyde with ethyl hydrazinoacetate hydrochloride were synthesized. X-ray crystal structures of all three complexes were determined. Crystallographic data indicate a common basis of the structures with some major differences. Both pyridine derivatives form complexes of the type [CuCl2L] with distorted square-planar geometry around copper(II), but show a decisive difference in the side chain orientation. The quinoline derivative forms a dimeric complex of type [Cu2Cl4L2] with distorted trigonal bipyramidal geometry around copper(II), but a rather short Cu···Cu contact, which is reflected in its magnetic properties. All three complexes showed antibacterial activity. 相似文献
11.
A yet unreported polymorph of [PtCl2(1,10-phenanthroline)] was obtained by slow decomposition, in CH2Cl2 solution, of [Pt{CH2CH2N(CH2CH3)2-κC,κN}(1,10-phenanthroline)](ClO4). The structure of the new orthorhombic form, III, (space group Pna21), is described and compared to those of the two already reported forms, I and II, which are monoclinic (space group P21/c) and orthorhombic (space group Pca21), respectively [21]. Polymorph III appears to be the least stable of the three. 相似文献
12.
A series of new binuclear copper (II) and nickel (II) complexes of the macrocyclic ligands bis(1,4,7-triazacyclononan-1-yl)butane (Lbut) and bis(1,4,7-triazacyclononan-1-yl)-m-xylene (Lmx) have been synthesized: [Cu2LbutBr4] (1), [Cu2Lbut(imidazole)2Br2](ClO4)2 (2), [Cu2Lmx(μ-OH)(imidazole)2](ClO4)3 (3), [Cu2Lbut(imidazole)4](ClO4)4 · H2O (4), [Cu2Lmx(imidazole)4](ClO4)4 (5), [Ni2 Lbut(H2O)6](ClO4)4 · 2H2O (6), [Ni2Lbut(imidazole)6](ClO4)4 · 2H2O (7) and [Ni2Lmx (imidazole)4(H2O)2](ClO4)4 · 3H2O (8). Complexes 1, 2, 7 and 8 have been characterized by single crystal X-ray studies. In each of the complexes, the two tridentate 1,4,7-triazacyclononane rings of the ligand facially coordinate to separate metal centres. The distorted square-pyramidal coordination sphere of the copper (II) centres is completed by bromide anions in the case of 1 and/or monodentate imidazole ligands in complexes 2, 4 and 5. Complex 3 has been formulated as a monohydroxo-bridged complex featuring two terminal imidazole ligands. Complexes 6-8 feature distorted octahedral nickel (II) centres with water and/or monodentate imidazole ligands occupying the remaining coordination sites. Within the crystal structures, the ligands adopt trans conformations, with the two metal binding compartments widely separated, perhaps as a consequence of electrostatic repulsion between the cationic metal centres. The imidazole-bearing complexes may be viewed as simple models for the coordinative interaction of the binuclear complexes of bis (tacn) ligands with protein molecules bearing multiple surface-exposed histidine residues. 相似文献
13.
Chin LF Kong SM Seng HL Khoo KS Vikneswaran R Teoh SG Ahmad M Khoo SB Maah MJ Ng CH 《Journal of inorganic biochemistry》2011,105(3):339-347
The synthesis and characterization of two cobalt(II) complexes, Co(phen)(ma)Cl 1 and Co(ma)2(phen) 2, (phen = 1,10-phenanthroline, ma− = maltolate or 2-methyl-4-oxo-4H-pyran-3-olate) are reported herein. The complexes have been characterized by FTIR, CHN analysis, fluorescence spectroscopy, UV-visible spectroscopy, conductivity measurement and X-ray crystallography. The number of chelated maltolate ligands seems to influence their DNA recognition, topoisomerase I inhibition and antiproliferative properties. 相似文献
14.
Panayot R. Bontchev Ivayla N. Pantcheva Ranko P. Bontchev Darvin S. Ivanov Nikolay D. Danchev 《Biometals》2002,15(1):79-85
The complex formation between copper(II) and the antihypertensive drug pindolol (HPin) was studied both in aqueous and methanolic media. Two complexes are formed at different metal-to-ligand molar ratios. The mononuclear complex Cu(Pin)2(HPin)2 contains two ligands in an anionic bidentate form and two - in a neutral form bound monodentately. The second complex Cu2Pin2Cl2 is dinuclear and its structure was determined by X-ray diffraction. The compound crystallizes in the monoclinic group C2/c with cell components a = 14.4998(13)Å, b = 18.511(2)Å, c = 14.2982(13)Å, =90 °, =109.556(2)°, =90 ° and Z = 12 at 293K. A pharmacological study on the influence of pindolol and its mononuclear complex on the heart rate of rats was performed. The complex is more active and has a longer effect in comparison with the pure non-coordinated pindolol in equitoxic doses. 相似文献
15.
Nirmal K. Shee F.A. Oluwafunmilayo Adekunle Michael G.B. Drew 《Inorganica chimica acta》2011,366(1):198-202
Reaction of 5,6-dihydro-5,6-epoxy-1,10-phenanthroline (L) with Cu(ClO4)2·6H2O in methanol in 3:1 M ratio at room temperature yields light green [CuL3](ClO4)2·H2O (1). The X-ray crystal structure of the hemi acetonitrile solvate [CuL3](ClO4)2·0.5CH3CN has been determined which shows Jahn-Teller distortion in the CuN6 core present in the cation [CuL3]2+. Complex 1 gives an axial EPR spectrum in acetonitrile-toluene glass with g|| = 2.262 (A|| = 169 × 10−4 cm−1) and g⊥ = 2.069. The Cu(II/I) potential in 1 in CH2Cl2 at a glassy carbon electrode is 0.32 V versus NHE. This potential does not change with the addition of extra L in the medium implicating generation of a six-coordinate copper(I) species [CuL3]+ in solution. B3LYP/LanL2DZ calculations show that the six Cu-N bond distances in [CuL3]+ are 2.33, 2.25, 2.32, 2.25, 2.28 and 2.25 Å while the ideal Cu(I)-N bond length in a symmetric Cu(I)N6 moiety is estimated as 2.25 Å. Reaction of L with Cu(CH3CN)4ClO4 in dehydrated methanol at room temperature even in 4:1 M proportion yields [CuL2]ClO4 (2). Its 1H NMR spectrum indicates that the metal in [CuL2]+ is tetrahedral. The Cu(II/I) potential in 2 is found to be 0.68 V versus NHE in CH2Cl2 at a glassy carbon electrode. In presence of excess L, 2 yields the cyclic voltammogram of 1. From 1H NMR titration, the free energy of binding of L to [CuL2]+ to produce [CuL3]+ in CD2Cl2 at 298 K is estimated as −11.7 (±0.2) kJ mol−1. 相似文献
16.
Zala Mahendrasinh Sujit B. Kumar Albert Escuer E. Suresh 《Inorganica chimica acta》2011,375(1):333-337
Binuclear cyanate bridged nickel(II) complex [Ni(L)(NCO)]2(PF6)2 (1) and copper(II) complex [Cu(L)(NCO)]2(PF6)2 (2), where L is N,N-bis(3,5-dimethylpyrazol-1-ylmethyl)aminomethylpyridine, a tetradentate N4-coordinated ligand have been synthesized and characterized by physicochemical method. The structures of complexes 1 and 2 have been studied by single crystal X-ray diffraction analysis. The structure analysis reveals that both nickel(II) and copper(II) center are coordinated in distorted octahedral fashion and coordination mode of cyanate ligand is end-to-end (μ-1,3) for complex 1 but it is double end-on (μ-1,1) mode for complex 2. The variable temperature magnetic susceptibility data, measured from 2 to 300 K, show weak antiferromagnetic interaction with J value −6.2(1) cm−1 for complex 1, whereas complex 2 has very weak ferromagnetic interaction with J value +0.5(1) cm−1. 相似文献
17.
Two new copper(II) complexes of the type [Cu(L)X2), where L = (E)-N-phenyl-2-[phenyl (pyridine-2-yl)methylene]hydrazinecarboxamide X = Cl/Br have been synthesized and characterized by elemental analyses, FAB (fast atomic bombardment) magnetic measurements, electronic absorption, conductivity measurements cyclic voltammetry (CV) and Electron paramagnetic resonance (epr) spectroscopy. The structures of these complexes determined by single crystal X-ray crystallography show a distorted square based pyramidal (DSBP) geometry around copper(II) metal center. The distorted CuN2OX (X = Cl/Br) basal plane in them is comprised of two nitrogen and one oxygen atoms of the meridionally coordinated ligand and a chloride or bromide ion and axial position is occupied by other halide ion. The epr spectra of these complexes in frozen solutions of DMSO showed a signal at g ca. 2. The trend in g-value (g|| > g⊥ > 2.00) suggest that the unpaired electron on copper(II) has dx2-y2 character. Biological activities in terms of superoxide dismutase (SOD) and antimicrobial properties of copper(II) complexes have also been measured. The superoxide dismutase activity reveals that these two complexes catalyze the fast disproportionation of superoxide in DMSO solution. 相似文献
18.
Ali Akbar Khandar Seyed Abolfazl Hosseini-Yazdi Seyed Amir Zarei 《Inorganica chimica acta》2005,358(11):3211-3217
Copper(II) and nickel(II) complexes of potentially N2O4 Schiff base ligands 2-({[2-(2-{2-[(1-{2-hydroxy-5-[2-phenyl-1-diazenyl]phenyl}methylidene)amino] phenoxy}ethoxy) phenyl]imino}methyl)4-[2-phenyl-1-diazenyl]phenol (H2L1) and 2-({[2-(4-{2-[(1-{2-hydroxy-5-[2-phenyl-1-diazenyl]phenyl}methylidene)amino] phenoxy}butoxy) phenyl]imino}methyl)4-[2-phenyl-1-diazenyl]phenol (H2L2) prepared of 5-phenylazo salicylaldehyde (1) and two various diamines 2-[2-(2-aminophenoxy)ethoxy]aniline (2) and 2-[4-(2-aminophenoxy)butoxy]aniline (3) were synthesized and characterized by a variety of physico-chemical techniques. The single-crystal X-ray diffractions are reported for CuL1 and NiL2. The CuL1 complex contains copper(II) in a near square-planar environment of N2O2 donors. The NiL2 complex contains nickel(II) in a distorted octahedral geometry coordination of N2O4 donors. In all complexes, H2L1 behaves as a tetradentate and H2L2 acts as a hexadentate ligand. Cyclic voltammetry of copper(II) complexes indicate a quasi-reversible redox wave in the negative potential range. 相似文献
19.
Copper(II), nickel(II) and cobalt(II) complexes of the aspirin metabolite salicylglycine (H2L), of stoichiometry M(HL)2·solvate, have been prepared and characterised. In these complexes salicylglycinate is coordinated to the metal via its carboxylato group and possibly also its amide oxygen in the copper(II) complex. Under basic conditions copper(II) forms the complex Cu(LH−1)·2H2O·MeOH, in which the ligand is coordinated to the metal via its carboxylate and phenolate oxygen atoms and the deprotonated peptide nitrogen atom. 相似文献
20.
Copper(II) cations coordinated with PMDTA (pentamethyldiethylenetriamine) and TMEDA (tetramethylethylenediamine) possess a high synthetic potential. The synthesis of these cations was carried out by metathesis reactions with silver salts. The cationic copper(II) complexes, [Cu(PMDTA)(Me2CO)Cl]+, [Cu(PMDTA)(H2O)Cl]+, [Cu(PMDTA)(DMF)]+, [Cu(PMDTA)Cl]+, [Cu(PMDTA)OAc]+, [Cu(PMDTA)(MeCN)2]2+, [Cu2(TMEDA)2Cl3]+ and [Cu(TMEDA)(MeCN)3]2+ were synthesised as PF6 salts, crystallised and characterised by single-crystal X-ray diffraction. 相似文献