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1.  Novel Organotin(IV)-Schiff Base Complexes: Synthesis, Characterization, Antimicrobial Activity, and DNA Interaction Studies 
Four organotin(IV) complexes with 2-(2-hydroxybenzylideneamino)isoindoline-1,3-dione (L1), and 4-(4-hydroxy-3-methoxybenzylideneamino-N-(pyrimidin-2-yl)benzenesulfonamide (L2) were synthesized and well characterized by analytical and spectral studies. The synthesized compounds were tested for antimicrobial activity by disc diffusion method. The DNA binding of the complexes 1 and 3 with CT-DNA has been performed with absorption spectroscopy, which showed that both the complexes are avid binders of CT-DNA. Also the nuclease activity of complexes 1 and 3 with plasmid DNA (pUC19) was studied using agarose gel electrophoresis. The complex 1 can act as effective DNA cleaving agent when compared to complex 3 resulting in the nicked form of DNA under physiological conditions. The gel was run both in the absence and presence of the oxidizing agent.
PMCID: PMC3021846  PMID: 21253533
2.  Stem Cells Grown in Osteogenic Medium on PLGA, PLGA/HA, and Titanium Scaffolds for Surgical Applications 
Pluripotent adipose tissue-derived stem cells (hASCs) can differentiate into various mesodermal cell types such as osteoblasts, chondroblasts, and myoblasts. We isolated hASCs from subcutaneous adipose tissue during orthopaedic surgery and induced the osteogenic differentiation for 28 days on three different synthetic scaffolds such as polylactide-co-glycolide (PLGA), polylactide-co-glycolide/hydroxyapatite (PLGA/HA), and trabecular titanium scaffolds (Ti6Al4V). Pore size can influence certain criteria such as cell attachment, infiltration, and vascularization. The aim of this study was to investigate the performance of PLGA and PLGA/HA scaffolds with a higher porosity, ranging between 75% and 84%, with respect to Ti scaffolds but with smaller pore size, seeded with hASCs to develop a model that could be used in the treatment of bone defects and fractures. Osteogenesis was assessed by ELISA quantitation of extracellular matrix protein expression, von Kossa staining, X-ray microanalysis, and scanning electron microscopy. The higher amount of protein matrix on the Ti scaffold with respect to PLGA and PLGA/HA leads to the conclusion that not only the type of material but the structure significantly affects cell proliferation.
PMCID: PMC3017899  PMID: 21234383
3.  Synthesis and Crystal Structure Characterization of Zinc (II) Tetronic Acid Complexes 
The synthesis and characterization of two new tetronic acid zinc (II) complexes of the empirical formulae [Zn(L–H)2(H2O)2] (1) and [Zn(L–H)2(H2O)(MeOH)]H2O (2) found within the same crystal are reported. The zinc ions bind through alkoxide and carbonyl groups of the ligand 3-methoxycarbonyl-5-phenyl tetronic acid (LH) as indicated by 1H NMR and X-ray crystallographic studies. These complexes promote intra- and intermolecular interactions, such as hydrogen bonding and π stacking, giving place to the formation of molecular aggregates.
PMCID: PMC2975069  PMID: 21076524
4.  Synthesis, Crystal Structures, and DNA Binding Properties of Zinc(II) Complexes with 3-Pyridine Aldoxime 
The employment of 3-pyridine aldoxime, (3-py)CHNOH, in ZnII chemistry has afforded two novel compounds: [Zn(acac)2{(3-py)CHNOH}]·H2O (1·H2O) [where acac− is the pentane-2,4-dionato(-1) ion] and [Zn2(O2CMe)4{(3-py)CHNOH}2] (2). Complex 1·H2O crystallizes in the monoclinic space group P21/n. The ZnII ion is five-coordinated, surrounded by four oxygen atoms of two acac− moieties and by the pyridyl nitrogen atom of the (3-py)CHNOH ligand. Molecules of 1 interact with the water lattice molecules forming a 2D hydrogen-bonding network. Complex 2 crystallizes in the triclinic P-1 space group and displays a dinuclear paddle-wheel structure. Each ZnII exhibits a perfect square pyramidal geometry, with four carboxylate oxygen atoms at the basal plane and the pyridyl nitrogen of one monodentate (3-py)CHNOH ligand at the apex. DNA mobility shift assays were performed for the determination of the in vitro effect of both complexes on the integrity and the electrophoretic mobility of pDNA.
PMCID: PMC2971566  PMID: 21076521
5.  Biosorption of Lanthanides from Aqueous Solutions Using Pretreated Buccinum tenuissimum Shell Biomass 
Biosorption experiment from aqueous solutions containing known amount of rare earth elements (REEs) using pre-treated Buccinum tenuissimum shell was explored to evaluate the efficiency of shell biomass as sorbent for REEs. In this work, four kinds of sieved shell samples: (a) “Ground original sample”, (b) “Heat-treatment (480°C, 6 hours) sample”, (c) “Heat-treatment (950°C, 6 hours) sample” and (d) “Heat-treatment (950°C, 6 hours) and water added sample” were used. Furthermore, to confirm the characteristics of the shell biomass, the crystal structure, the surface morphology, and the specific surface area of these shell samples were determined. Consequently, the following matters have been mainly clarified. (1) The crystal structure of the shell biomass was transformed from aragonite (CaCO3) into calcite (CaCO3) phase by heat-treatment (480°C, 6 hours); then mainly transformed into calcium oxide (CaO) by heat-treatment (950°C, 6 hours), and calcium hydroxide (Ca(OH)2) by heat-treatment (950°C, 6 hours) and adding water. (2) The shell biomass showed excellent sorption capacity for lanthanides. (3) Adsorption isotherms using the shell biomass can be described by Langmuir and Freundlich isotherms satisfactorily for lanthanides except “heat-treatment (950°C, 6 hours) sample”. (4) Shell biomass (usually treated as waste material) can be an efficient sorbent for lanthanides in future.
PMCID: PMC2963800  PMID: 20981250
6.  Synthesis, X-Ray Structure, and Characterization of Catena-bis(benzoate)bis{N,N-bis(2-hydroxyethyl)glycinate}cadmium(II) 
The reaction of N, N-bis(2-hydroxyethyl)glycine (bicine; bicH3) with Cd(O2CPh)2 · 2H2O in MeOH yielded the polymeric compound [Cd2(O2CPh)2(bicH2)2]n(1). The complex crystallizes in the tetragonal space group P41212. The lattice constants are a = b = 12.737(5) and c = 18.288(7) Å. The compound contains chains of repeating {Cd2(O2CPh)2(bicH2)2} units. One CdII atom is coordinated by two carboxylate oxygen, four hydroxyl oxygen, and two nitrogen atoms from two symmetry-related 2.21111 (Harris notation) bicH2− ligands. The other CdII atom is coordinated by six carboxylate oxygen atoms, four from two bicH2− ligands and two from the monodentate benzoate groups. Each bicinate(-1) ligand chelates the 8-coordinate, square antiprismatic CdII atom through one carboxylate oxygen, the nitrogen, and both hydroxyl oxygen atoms and bridges the second, six-coordinate trigonal prismatic CdII center through its carboxylate oxygen atoms. Compound 1 is the first structurally characterized cadmium(II) complex containing any anionic form of bicine as ligand. IR data of 1 are discussed in terms of the coordination modes of the ligands and the known structure.
PMCID: PMC2952795  PMID: 20976297
7.  Computational Modeling of the Mechanism of Urease 
In order to elucidate aspects of the mechanism of the hydrolytic enzyme urease, theoretical calculations were undertaken on a model of the active site, using density functional theory. The bridging oxygen donor that has been found in the crystal structures was determined to be a hydroxide ion. The initial coordination of urea at the active site occurs most likely through the urea oxygen to the nickel ion with the lowest coordination number. This coordination can be made without much gain in energy. The calculations also showed that weak coordination of one of the urea amine nitrogen atoms to the second nickel atom is energetically feasible. Furthermore, a proposed mechanism including a tetrahedral intermediate generated by hydrolytic attack on the urea carbon by the bridging hydroxide was modeled, and the tetrahedral intermediate was found to be energetically unfavorable relative to terminal coordination of the substrate (urea).
PMCID: PMC2945649  PMID: 20886006
8.  Coordination Reactions and Noncovalent Interactions of Polyamines with Nucleotides in Binary Systems and with Nucleotides and Copper(II) Ion in Ternary Systems 
Interactions of nucleotides (AMP, CMP) and 1,2-diaminopropane (tn-1) or 2-methyl-1,2-diaminopropane (tn-2) in metal-free systems as well as in the systems including copper(II) ions were studied. The composition and overall stability constants of the complexes formed were determined by the potentiometric method, whereas the interaction centres and coordination sites were identified by spectroscopic methods. It was found that phosphate groups of nucleotides and the protonated amine groups of polyamines are the centres of interaction. The differences in the interactions with the polyamines which act as models of biogenic amines are impacted by the presence of lateral chains (methylene groups) in tn-1 and tn-2. In the ternary systems with Cu(II) ions, the heteroligand complexes are mainly of the ML⋯L' type, in which the protonated polyamine is engaged in noncovalent interactions with the anchoring Cu(II)-nucleotide complex. The complexes formed in the Cu/NMP)/tn-1 system are more stable than those formed in the system with tn-2. The mode of coordination in the complex is realised mainly through the phosphate groups of the nucleotide with involvement of the endocyclic nitrogen atoms in a manner which depends upon the steric conditions and in particular on the number of the methylene groups in the polyamine molecule.
PMCID: PMC2946580  PMID: 20885917
9.  Zinc(II) and Nickel(II) Benzoate Complexes from the Use of 1-methyl-4,5-diphenylimidazole 
Two new complexes, [Zn(O2CPh)2(L)2]·2MeOH (1·2MeOH) and [Ni2(O2CPh))4(L)2]·2MeCN (2·2MeCN), have been synthesized and characterized by X-ray analysis in the course of an ongoing investigation of the MII/X−/L [MII = Co, Ni, Cu, Zn; X− = Cl−, Br−, I−, NCS−, NO3−, N3−, PhCO2−; L = 1-methyl-4,5-diphenylimidazole] reaction system, aiming at understanding and assessing the relative strength and the way in which the intermolecular interactions control the supramolecular organization of these compounds. In the mononuclear complex 1·2MeOH, the benzoate ion acts as a monodentate ligand resulting in a distorted tetrahedral N2O2 coordination environment. Complex 2·2MeCN exhibits a dinuclear paddle-wheel structure; each NiII has a square pyramidal NiNO4 chromophore with four benzoate oxygens in the basal plane and the pyridine-type nitrogen atom of one ligand L at the apex. The structure of 1·2MeOH is stabilized by intramolecular π-π interactions between aromatic rings of adjacent 4,5-diphenylimidazole moieties; it is a feature also evidenced in similar compounds of the type [MX2L2].
PMCID: PMC2927736  PMID: 20811497
10.  Use of the 2-Pyridinealdoxime/N,N′-Donor Ligand Combination in Cobalt(III) Chemistry: Synthesis and Characterization of Two Cationic Mononuclear Cobalt(III) Complexes 
The use of 2-pyridinealdoxime (paoH)/N,N′-donor ligand (L-L) “blend” in cobalt chemistry has afforded two cationic mononuclear cobalt(III) complexes of the general type [Co(pao)2(L-L)]+, where L-L = 1,10-phenanthroline (phen) and 2,2′-bipyridine (bpy). The CoCl2/paoH/L-L (1 : 2 : 1) reaction system in MeOH gives complexes [CoIII(pao)2(phen)]Cl·2H2O (1·2H2O) and [CoIII(pao)2(bpy)]Cl·1.5MeOH (2·1.5MeOH). The structures of the complexes were determined by single-crystal X-ray crystallography. The CoIII ions are six-coordinate, surrounded by three bidentate chelating ligands, that is, two pao− and one phen or bpy. The deprotonated oxygen atom of the pao− ligand remains uncoordinated and participates in hydrogen bonding with the solvate molecules. IR data of the complexes are discussed in terms of the nature of bonding and the known structures.
PMCID: PMC2913532  PMID: 20721276
11.  Synthesis, Structure, and Antiproliferative Activity of Three Gallium(III) Azole Complexes 
As part of our interest into the bioinorganic chemistry of gallium, gallium(III) complexes of the azole ligands 2,1,3-benzothiadiazole (btd), 1,2,3-benzotriazole (btaH), and 1-methyl-4,5-diphenylimidazole (L) have been isolated. Reaction of btaH or btd with GaBr3 or GaCl3 resulted in the mononuclear complexes [GaBr3(btaH)2] (1) and [GaCl3(btd)2] (2), respectively, while treatment of GaCl3 with L resulted in the anionic complex (LH)2[GaCl4] (3). All three complexes were characterized by single-crystal X-ray crystallography and IR spectroscopy, while their antiproliferative activities were investigated against a series of human and mouse cancer cell lines.
PMCID: PMC2913727  PMID: 20721278
12.  Kinetic Studies and Mechanism of Hydrogen Peroxide Catalytic Decomposition by Cu(II) Complexes with Polyelectrolytes Derived from L-Alanine and Glycylglycine 
The catalytic decomposition of hydrogen peroxide by Cu(II) complexes with polymers bearing L-alanine (PAla) and glycylglycine (PGlygly) in their side chain was studied in alkaline aqueous media. The reactions were of pseudo-first order with respect to [H2O2] and [L-Cu(II)] (L stands for PAla or PGlygly) and the reaction rate was increased with pH increase. The energies of activation for the reactions were determined at pH 8.8, in a temperature range of 293–308 K. A suitable mechanism is proposed to account for the kinetic data, which involves the Cu(II)/Cu(I) redox pair, as has been demonstrated by ESR spectroscopy. The trend in catalytic efficiency is in the order PGlygly>PAla, due to differences in modes of complexation and in the conformation of the macromolecular ligands.
PMCID: PMC2913805  PMID: 20721280
13.  Kinetics and Mechanisms of the Chromium(III) Reactions with 2,4- and 2,5-Dihydroxybenzoic Acids in Weak Acidic Aqueous Solutions 
The reactions of 2,4- and 2,5-dihydroxybenzoic acids (dihydroxybenzoic acid, DHBA) with chromium(III) in weak acidic aqueous solutions have been shown to take place in at least two stages. The first stage of the reactions has an observed rate constant k1(obs) = k1[DHBA] + C and the corresponding activation parameters are ΔH1(2,4)≠ = 49, 5 kJ/mol−1, ΔS1(2,4)≠ = −103, 7 J mol−1 K−1, ΔH1(2,5)≠ = 60, 3 kJ/mol−1, and ΔS1(2,5)≠ = −68, 0 J mol−1 K−1. These are composite activation parameters and the breaking of the strong intramolecular hydrogen bonding in the two ligands is suggested to be the first step of the (composite) first stage of the reactions. The second stage is ligand concentration independent and is thus attributed to a chelation process. The corresponding activation parameters are ΔH2(2,4)≠ = 45, 13 kJ/mol−1, ΔS2(2,4)≠ = −185, 9 J mol−1 K−1, ΔH2(2,5)≠ = 54, 55 kJ/mol−1, and ΔS2(2,5)≠ = −154, 8 J mol−1 K−1. The activation parameters support an associative mechanism for the second stage of the reactions. The various substitution processes are accompanied by proton release, resulting in pH decrease.
PMCID: PMC2913840  PMID: 20721282
14.  Mononuclear and Dinuclear Manganese(II) Complexes from the Use of Methyl(2-pyridyl)ketone Oxime 
The reactions of methyl(2-pyridyl)ketone oxime, (py)C(Me)NOH, with manganese(II) sulfate monohydrate have been investigated. The reaction between equimolar quantities of MnSO4 · H2O and (py)C(Me)NOH in H2O lead to the dinuclear complex [Mn2(SO4)2{(py)C(Me)NOH}4] · (py)C(Me)NOH, 1 · (py)C(Me)NOH, while employment of NaOMe as base affords the compound [Mn(HCO2)2{(py)C(Me)NOH}2] (2). The structures of both compounds have been determined by single crystal X-ray diffraction. In both complexes, the organic ligand chelates through its nitrogen atoms. The IR data are discussed in terms of the nature of bonding and the structures of the two complexes.
PMCID: PMC2910486  PMID: 20671965
15.  The Effect of Stereochemistry on Sodium Ion Complexation in Nucleoside-Metallacarborane Conjugates 
Conjugates of purine and pyrimidine nucleosides: thymidine and 2′-deoxyguanosine with cobalt-metallacarborane were studied for their sodium ion complexing properties. Formation of stable complexes of 1 : 1 stoichiometry was proved by ESI MS spectroscopy and 23Na NMR. Equilibrium constants and energies of complex formation were calculated. Complexation of alkali-metals by nucleoside-metallacarborane conjugates may affect the physicochemical and biological properties of the conjugates and should be taken into consideration during biological evaluation of these types of modifications.
PMCID: PMC2909723  PMID: 20671972
16.  Antineoplastic Activity of New Transition Metal Complexes of 6-Methylpyridine-2-carbaldehyde-N(4)-ethylthiosemicarbazone: X-Ray Crystal Structures of [VO2(mpETSC)] and [Pt(mpETSC)Cl] 
New complexes of dioxovanadium(V), zinc(II), ruthenium(II), palladium(II), and platinum(II) with 6-methylpyridine-2-carbaldehyde-N(4)-ethylthiosemicarbazone (HmpETSC) have been synthesized. The composition of these complexes is discussed on the basis of elemental analyses, IR, Raman, NMR (1H, 13C, and 31P), and electronic spectral data. The X-ray crystal structures of [VO2(mpETSC)] and [Pt(mpETSC)Cl] are also reported. The HmpETSC and its [Zn(HmpETSC)Cl2] and [Pd(mpETSC)Cl] complexes exhibit antineoplastic activity against colon cancer human cell lines (HCT 116).
PMCID: PMC2909729  PMID: 20671978
17.  Investigation on the Interactions of NiCR and NiCR-2H with DNA 
We report here a biophysical and biochemical approach to determine the differences in interactions of NiCR and NiCR-2H with DNA. Our goal is to determine whether such interactions are responsible for the recently observed differences in their cytotoxicity toward MCF-7 cancer cells. Viscosity measurement and fluorescence displacement titration indicated that both NiCR and NiCR-2H bind weakly to duplex DNA in the grooves. The coordination of NiCR-2H with the N-7 of 2′-deoxyguanosine 5′-monophosphate (5′-dGMP) is stronger than that of NiCR as determined by 1H NMR. NiCR-2H, like NiCR, can selectively oxidize guanines present in distinctive DNA structures (e.g., bulges), and notably, NiCR-2H oxidizes guanines more efficiently than NiCR. In addition, UV and 1H NMR studies revealed that NiCR is oxidized into NiCR-2H in the presence of KHSO5 at low molar ratios with respect to NiCR (≤4).
PMCID: PMC2910472  PMID: 20671951
18.  Synthesis and Biological Evaluation of New CRH Analogues 
A series of 7 new human/rat Corticotropin Releasing Hormone (h/r-CRH) analogues were synthesized. The induced alterations include substitution of Phe at position 12 with D-Phe, Leu at positions 14 and 15 with Aib and Met at positions 21 and 38 with Cys(Et) and Cys(Pr). The analogues were tested regarding their binding affinity to the CRH-1 receptor and their activity which is represented by means of percentage of maximum response in comparison to the native molecule. The results indicated that the introduction of Aib, or Cys derivatives although altering the secondary structure of the molecule, did not hinder receptor recognition and binding.
PMCID: PMC2905701  PMID: 20689735
19.  Structurally Diverse Metal Coordination Compounds, Bearing Imidodiphosphinate and Diphosphinoamine Ligands, as Potential Inhibitors of the Platelet Activating Factor 
Metal complexes bearing dichalcogenated imidodiphosphinate [R2P(E)NP(E)R2′]− ligands (E = O, S, Se, Te), which act as (E,E) chelates, exhibit a remarkable variety of three-dimensional structures. A series of such complexes, namely, square-planar [Cu{(OPPh2)(OPPh2)N-O, O}2], tetrahedral [Zn{(EPPh2)(EPPh2)N-E,E}2], E = O, S, and octahedral [Ga{(OPPh2)(OPPh2)N-O,O}3], were tested as potential inhibitors of either the platelet activating factor (PAF)- or thrombin-induced aggregation in both washed rabbit platelets and rabbit platelet rich plasma. For comparison, square-planar [Ni{(Ph2P)2N-S-CHMePh-P, P}X2], X = Cl, Br, the corresponding metal salts of all complexes and the (OPPh2)(OPPh2)NH ligand were also investigated. Ga(O,O)3 showed the highest anti-PAF activity but did not inhibit the thrombin-related pathway, whereas Zn(S,S)2, with also a significant PAF inhibitory effect, exhibited the highest thrombin-related inhibition. Zn(O,O)2 and Cu(O,O)2 inhibited moderately both PAF and thrombin, being more effective towards PAF. This work shows that the PAF-inhibitory action depends on the structure of the complexes studied, with the bulkier Ga(O,O)3 being the most efficient and selective inhibitor.
PMCID: PMC2905917  PMID: 20689709
20.  Zinc Binding Properties of Engineered RING Finger Domain of Arkadia E3 Ubiquitin Ligase 
Human Arkadia is a nuclear protein consisted of 989 amino acid residues, with a characteristic RING domain in its C-terminus. The RING domain harbours the E3 ubiquitin ligase activity needed by Arkadia to ubiquitinate its substrates such as negative regulators of TGF-β signaling. The RING finger domain of Arkadia is a RING-H2 type and its structure and stability is strongly dependent on the presence of two bound Zn(II) ions attached to the protein frame through a defined Cys3-His2-Cys3 motif. In the present paper we transform the RING-H2 type of Arkadia finger domain to nonnative RING sequence, substituting the zinc-binding residues Cys955 or His960 to Arginine, through site-directed mutagenesis. The recombinant expression, in Escherichia coli, of the mutants C955R and H960R reveal significant lower yield in respect with the native polypeptide of Arkadia RING-H2 finger domain. In particular, only the C955R mutant exhibits expression yield sufficient for recombinant protein isolation and preliminary studies. Atomic absorption measurements and preliminary NMR data analysis reveal that the C955R point mutation in the RING Finger domain of Arkadia diminishes dramatically the zinc binding affinity, leading to the breakdown of the global structural integrity of the RING construct.
PMCID: PMC2905715  PMID: 20689703
21.  Hydrogen-Bonded Networks Based on Cobalt(II), Nickel(II), and Zinc(II) Complexes of N,N'-Diethylurea 
N,N'-diethylurea (DEU) was employed as a ligand to form the octahedral complexes [M(DEU)6]2+ (M=Co, Ni and Zn). Compounds [Co(DEU)6](BF4)2 (1), [Co(DEU)6](CIO4)2 (2), [Ni(DEU)6](CIO4)2 (3), and [Zn(DMU)6](CIO4)2 (4) have been prepared from the reactions of DEU and the appropriate hydrated metal(II) salts in EtOH in the presence of 2,2-dimethoxypropane. Crystal structure determinations demonstrate the existence of [M(DEU)6]2+ cations and CIO4− (in 2–4) or BF4− (in 1) counterions. The [M(DEU)6]2+ cations in the solid state are stabilized by a pseudochelate effect due to the existence of six strong intracationic N-H ⋯ O(DEU) hydrogen bonds. The [M(DEU)6]2+ cations and counterions self-assemble to form hydrogen-bonded 2D architectures in 2–4 that conform to the kgd (kagome dual) network, and a 3D hydrogen-bonded rtl (rutile) network in 1. The nature of the resulting supramolecular structures is influenced by the nature of the counter-ion. The complexes were also characterized by vibrational spectroscopy (IR).
PMCID: PMC2905724  PMID: 20689706
22.  The Catalytic Function of Nonheme Iron (III) Complex for Hydrocarbon Oxidation 
A detailed catalytic study of LFeIIICl (where L = 3-{2-[2-(3-hydroxy-1,3-diphenyl-allylideneamino)-ethylamino]-ethylimino}-1,3-diphenyl-propen-1-ol) for hydrocarbon oxidation was carried out, focusing on the role of solvent, atmospheric dioxygen, and oxidant on catalytic efficiency. The data showed that LFeIIICl catalyst was efficient in homogeneous hydrocarbon oxidations providing significant yields. Moreover, tert-BuOOH provided comparable oxidation yields with H2O2, slightly favoring the formation of alcohols and ketones versus epoxides. Dioxygen intervened in the catalytic reaction, influencing the nature of oxidation products. The polarity of solvent strongly influenced the reaction rates and the nature of oxidation products. A mechanistic model is postulated assuming that LFeIIICl functions via the formation of iron-hydroperoxo-species, followed by a radical-based mechanistic path.
PMCID: PMC2905942  PMID: 20689711
23.  New Thermal and Microbial Resistant Metal-Containing Epoxy Polymers 
A series of metal-containing epoxy polymers have been synthesized by the condensation of epichlorohydrin (1-chloro-2,3-epoxy propane) with Schiff base metal complexes in alkaline medium. Schiff base was initially prepared by the reaction of 2,6 dihydroxy 1-napthaldehyde and o-phenylenediamine in 1  :  2 molar ratio and then with metal acetate. All the synthesized compounds were characterized by elemental, spectral, and thermal analysis. The physicochemical properties, viz., epoxy value, hydroxyl content, and chlorine content [mol/100 g] were measured by standard procedures. The antimicrobial activities of these metal-containing epoxy polymers were carried out by using minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) methods against S. aureus, B. subtilis (Gram-positive bacteria), and E. coli, P. aeruginosa (Gram-negative bacteria). It was found that the ECu(II) showed higher antibacterial activity than other metal-chelated epoxy resin while EMn(II) exhibited reduced antibacterial activity against all bacteria.
PMCID: PMC2906153  PMID: 20689716
24.  In Search for Titanocene Complexes with Improved Cytotoxic Activity: Synthesis, X-Ray Structure, and Spectroscopic Study of Bis(η5-cyclopentadienyl)difluorotitanium(IV) 
The 1 : 2 reaction of [Ti(η5-C5H5)2Cl2] and AgF in CHCl3/H2O yielded the fluoro analog [Ti(η5-C5H5)2F2] (1) in almost quantitative yield (C5H5 is the cyclopentadienyl group). The coordination about the TiIV atom formed by two fluoro ligands and the centroids of the cyclopentadienyl rings is distorted tetrahedral. The compound crystallizes in the orthorhombic space group C2cm. The lattice constants are a = 5.9055(4), b = 10.3021(5), c = 14.2619(9) Å, and α = β = γ = 90°. The complex has been characterized by elemental analyses and spectroscopic (IR, 1H NMR) data. A structural comparison of the four members of the [Ti(η5-C5H5)2X2] family of complexes (X = F, Cl, Br, I) is attempted.
PMCID: PMC2905951  PMID: 20689714
25.  Interactions of Trivalent Lanthanide Cations with a New Hexadentate Di-Schiff Base: New Lanthanide(III) Complexes from (NE,N′E)-2,2′-(ethane-1,2-diylbis(oxy))bis(N-(pyridin-2-ylmethylene)ethanamine) 
The novel lanthanide(III) complexes [Ln(NO3)2L](NO3)·3MeOH (Ln = La 1, Pr 2) and [Ln(NO3)3L](NO3)·2MeOH (Ln = Gd 3, Yb 4), where L = (NE,N′E)-2,2′-(ethane-1,2-diylbis(oxy))bis(N-(pyridin-2-ylmethylene)ethanamine), have been obtained by direct reaction of the Schiff base ligand and the corresponding hydrated lanthanide(III) nitrates in methanol. All complexes were characterized spectroscopically and thermogravimetrically. Complex 4 was also characterized with crystallographic studies: orthorhombic P212121, a = 10.6683(14), b = 13.4752(15), c = 19.3320(26) Å. In the molecular structure of 4, Yb(III) is surrounded by all donor atoms of the Schiff base (four nitrogen and two oxygen atoms) and four oxygen atoms belonging to two bidentate chelating nitrato ligands.
PMCID: PMC2905721  PMID: 20689704

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