Characterized By Elemental Analysis Research Articles

Synthesis, Crystal Structure, Spectral and Thermal Studies of (E)-4-Dimethamino[(1-phenylethyl)iminomethyl]benzyne

Schiff-base compound (E)-4-dimethamino ((1-phenylethyl)iminomethyl)benzyne was synthesized and characterized by elemental analyses (CHN), FT-IR and 1 H-NMR spectroscopic techniques and thermogravimetric analyses (TG). Crystal structure of the title compound was obtained by single crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P21 with unit cell parameters: a = 8.5283(2), b = 6.0699(2), c = 13.6997(4) A ˚ , b = 91.471(2) ,V = 708.94(4) A ˚ 3 and Z = 2.

Identification of Binding Mode of a Platinum (II) Complex, (DIP), and Calf Thymus DNA

The Pt(II) complex, PtCl2(DIP) (DIP = chelating dinitrogen ligand: 4,7-diphenyl-1,10-phenanthroline), was synthesized and characterized by elemental analysis (CHN) and 1H NMR and UV-vis techniques. The binding of this complex to calf thymus DNA was investigated using various physicochemical methods such as spectrophotometric, circular dichroism, spectrofluorometric, melting temperature, and viscosimetric techniques. Upon addition of the complex, important changes were observed in the characteristic UV-Vis bands (hyperchromism) of calf thymus DNA (CT-DNA): increase in melting temperature, sharp increase in specific viscosity of DNA, and induced CD spectral changes. Also the fluorescence spectral characteristics and interaction of Pt complex with DNA have been studied. Pt bound to DNA showed a marked decrease in the fluorescence intensity. The results show that both the complex and the NR molecules can intercalate competitively into the DNA double-helix structure. The experimental results show that the mode of binding of the this complex to DNA is classical intercalation.

Synthesis and characterization of oxidomolybdenum(V) and dioxidomolybdeum(VI) complexes derived from isonicotinoyl(2-hydroxy-3-methoxybenzylidene)hydrazide

Several novel complexes of oxidomolybdenum(V) and dioxidomolybdenum(VI) were synthesized with the Schiff base, 3- methoxy salicylaldehydeisonicotinoylhydrazone (HL) derived from 3- methoxy salicylaldehyde and isonicotinoylhydrazide. The complexes were characterized by elemental analyses, molar conductance and magnetic susceptibility, as well as IR, 1H-NMR, Fmass and UV-Vis spectral studies. The complexes have the general formulae [MoO(L)XCl] and [MoO2(L)X], where X=NO3 or ClO4. The IR spectra of these complexes indicate that the ligand (HL) acts as a monoanionic tridentate chelating agent. The spectra indicate the monodentate mode of coordination for the nitrate and perchlorate groups. The X-ray diffraction studies of [MoO(L)NO3Cl] correspond to an orthorhombic crystal lattice with unit cell dimensions a = 15.49 ?, b = 12.44 ? and c = 10.11 ?. All the complexes were found to have distorted octahedral geometry. Thermal studies of the complex [MoO2(L)NO3] showed that it was stable up to 240 ?C, above which it started to decompose. The optimized geometry of ligand and one of its complexes, [MoO(L)NO3Cl], have been obtained by a molecular mechanics method. Antibacterial studies of the present complexes show that the oxidomolybdenum(V) complexes were more potent bactericides than the ligand and the dioxidomolybdenum(VI) complexes.

Cu2(μ-(3,4,5-meo-ba)2bn)(μ-I)2] n , a new 1D polymeric copper(I) chain

New 1D-chain copper(I) complex [Cu2(μ-(3,4,5-MeO-ba)2bn)(μ-I)2] n (1), where (3,4,5-MeO-ba)2bn = N,N′-bis(3,4-dimethoxybenzylidene)-butane-1,4-diamine, involving a new bidentate Schiff-base containing a flexible spacer (=N–C–C–C–C–N=) has been synthesized and characterized by elemental analyses (CHN) and FT-IR spectroscopy. The crystal structure of 1 was determined from single-crystal X-ray diffraction analyses and shows the (3,4,5-MeO-ba)2en acts as a bridging ligand with the nitrogen atoms of the two imine functions and leading to the dinuclear [Cu2((μ-(3,4,5-MeO-ba)2en)] groups. Such dinuclear [Cu2((μ-(3,4,5-MeO-ba)2en)] groups are bridged by two iodine anions [(μ-I)2] to form a neutral 1D-chain copper(I) iodide coordination polymer. The coordination polyhedron about the copper(I) center in 1 is best described as a distorted trigonal planar. Thermogravimetric analyses reveal the thermal stability and decomposition pattern of 1.

Synthesis, characterization, and crystal structure of two zinc(II) halide complexes with the symmetrical bidentate Schiff-base ligand (3,4-MeO-ba)2en

In this study two zinc(II) halide complexes with the Schiff-base ligand (3,4-MeO-ba)2en [N,N′-bis(3,4-dimethoxybenzylidene)ethane-1,2-diamine] have been synthesized and characterized by elemental analyses (CHN), single-crystal X-ray diffraction, Fourier-transform infrared (FT-IR), and 1H nuclear magnetic resonance (NMR) spectroscopy. The metal-to-ligand ratio was found to be 1:1 within the formula ZnX2((3,4-MeO-ba)2en) (X = Br, I). Crystal structure analysis reveals that the coordination geometry around the zinc(II) ions in the two isotypic complexes is distorted tetrahedral. The Schiff-base ligand (3,4-MeO-ba)2en acts as a chelating ligand and coordinates via two N atoms to the metal center and adopts an (E,E) conformation. The coordination spheres of the metal atoms are completed by the two halide atoms, which are also involved in weak non-classical hydrogen-bonding interactions of the type C–H···X–Zn.

Identification of a new anti-diabetic agent by combining VOSO 4 and vitamin E in a single molecule: Studies on its spectral, thermal and pharmacological properties

Vanadium(IV) complex of vitamin E (Vit E) ligand was reported. In this complex, binuclear ligand acts as a monodentate via oxygen of phenolic group. The vanadyl(II) ion is surrounded by two molecules of Vit E and two water molecules. The [VO(Vit E) 2(H 2O) 2]2H 2O complex was isolated by the reaction between VOSO 4 and vitamin E in ethanol/water solvent (50/50 w/w) at pH = 8. The solid vanadyl(II) complex has been characterized by elemental analyses (CHN), photometric titrations, infrared spectra, molar conductivity, electronic spectra, TGA/DSC, SEM and XRD studies. Electronic and magnetic measurements are confirmed that the speculated geometry of vanadyl(II) complex is square pyramidal geometry. The microbial test was performed for the vanadyl complex against some kinds of bacteria and fungi. The [VO(Vit E) 2(H 2O) 2]2H 2O complex was proved effective in addressing diabetic of type I in case of experimental animal than other compounds were prepared in the literature.

Preparation, Characterization and Luminescence Study of Chitosan Membrane and Powder Forms with Eu3 + and Tb3 +

Chitosan membranes with trivalent lanthanide ion Eu3 + were prepared at a ratio of 3:1 w/w (chitosan:lanthanide). There was no membrane formation at a ratio of 1:1 w/w (chitosan: Eu3 + or Tb3 +); in this case a white solid powder was obtained. Both chitosan compounds were characterized by elemental analysis (CHN), thermal analysis (TG/DTG), scanning electron microscopy (SEM) and luminescence spectroscopy. CHN analysis was performed only for chitosan compounds in powder form, suggesting that these compounds have the general formula QUILn.6H2O, where QUI = Chitosan and Ln = Eu3 + or Tb3 +. The results of TG/DTG curves for chitosan membranes with Eu3 + ion indicate that the introduction of this metal into the chitosan structure causes gradual degradation in residual carbons, showing lower weight loss in the Eu3 + membranes compared to pure chitosan membrane. Analysis of luminescence demonstrated that chitosan membranes with Eu3 + ion exhibit emission in the visible region, showing emission bands from chitosan and Eu3 + moieties. For chitosan with Eu3 + and Tb3 + ions compounds, in powder form, the analysis of luminescence suggested that chitosan is not transferring energy to the lanthanide ion; however, the chemical region where the lanthanide ion is found breaks the selection rules and favors the emission of these ions.

Preparation and characterization of novel oxo-centered basic p-chlorobenzoic bridging trinuclear complexes

Three new oxo-centered trinuclear complexes, one of them a mixed-valence complex [Mn3O(C7H4O2Cl)6(Py)3]Py (1) and the others, mixed-metal complexes of [Fe2MnO(C7H4O2Cl)6(Py)3]NO3 (2) and [Fe2CoO(C7H4O2Cl)6(Py)3] (3) were synthesized by the direct reaction between metal nitrates and p-chlorobenzoic acid. These complexes were characterized by elemental analyses (CHN), atomic absorption spectroscopy and spectral (IR, electronic) studies. These are new type of oxo-bridged mixed-metal complexes in which the carboxylate ligand is pchlorobenzoic acid. The UV spectra of the complexes exhibited a strong band in the region 42,500 cm-1 which is related to the (? ? ?*) transitions of the pyridine ligand. The IR spectra of these compounds showed two strong stretching vibrations bands, indicating a bridging coordination mode of the carboxylic group of the ligand in the complexes.

DNA Interaction with PtCl2(LL) (LL = Chelating Diamine Ligand: N,N-Dimethyltrimethylendiamine) Complex

The [PtCl(2)(LL)] complex, as a cisplatin derivative, which LL is diamine chelate ligand (N,N-dimethyltrimethylendiamine), was synthesized and characterized by elemental analysis (CHN) mass, (1)H, and (13)C nuclear magnetic resonance techniques. Then the binding of this complex to calf thymus DNA was investigated by various physicochemical methods such as spectrophotometric, circular dichroism, spectrofluorometric, melting temperature, and viscosimetric techniques. Upon addition of the complex, important changes were observed in the characteristic UV-Vis bands (hypochromism) of calf thymus DNA, increase in melting temperature and some changes in specific viscosity. Also, the fluorescence spectral characteristics showed an increase in the fluorescence intensity of methylene blue-DNA solutions in the presence of increasing amounts of metal complex, indicating PtCl(2)(LL) is able to displace the methylene blue bound to DNA but not as complete as intercalative molecules. The experimental results showed that the platinum complex is bound to DNA non-intercalatively, and an outside binding is the preferred mode of interaction.

Synthesis and characterization of novel oxo-bridged, trinuclear mixed-metal complexes of Cr(III) and Fe(III)

Two new heterotrinuclear p-chlorobenzoates, [Fe2CrO(C7H4O2Cl)6(py)3]NO3 (1) and [Cr2FeO(C7H4O2Cl)6(py)3]NO3 (2) were prepared as nitrate salts and characterized by elemental analyses (CHN), spectroscopic (infrared, electronic) studies and atomic absorption spectroscopy. These complexes are a new type of oxo-bridged mixed-metal complex in which the carboxylate ligand is p-chlorobenzoic acid. Bridging coordination modes for the carboxylates were indicated by the presence of ?asym (M2M'O) vibrations in the infrared spectra.

Synthesis and coordination chemistry of new tetradentate N 2S 2 donor Schiff-base ligand ca 2-dapte: Mononuclear and dinuclear copper(I) complexes [Cu(ca 2dapte)]ClO 4 and [{Cu(PPh 3)(X)} 2(ca 2dapte)] (X = I and Br)

A mononuclear copper(I) complex, [Cu(ca 2dapte)]ClO 4 ( 1), and two dinuclear copper(I) complexes, [{Cu(PPh 3)(X)} 2(ca 2dapte)] (X = I ( 2) and Br ( 3)), of a new tetradentate N 2S 2 donor Schiff-base ligand ca 2dapte have been prepared (ca 2dapte = N, N′-bis( trans-cinnamaldehyde)-1,2-di(o-iminophenylthio)ethane). These compounds have been characterized by elemental analyses (CHN), FT-IR, UV–Vis and 1H NMR spectroscopy. The crystal structures of these copper(I) complexes have been determined by single-crystal X-ray diffraction. The coordination geometry around Cu(I) centers in these complexes is a distorted tetrahedron. The ca 2dapte is coordinated to Cu(I) as a tetradentate ligand in 1, while it acts as a bis-bidentate bridging ligand in 2 and 3.

Deamination process in the formation of a copper(II) complex with glutamic acid and a new ligand derived from guanidinoacetic acid: Synthesis, characterization, and molecular modeling studies

A deamination process was observed after copper(II) complexation reaction with guanidinoacetic (Gaa) and glutamic acids (Glu), forming the binuclear copper(II) complex K 2Cu 2C 16H 23N 7O 12 · 1/2H 2O ( 1), which was characterized by elemental analysis (CHN), spectroscopy methods (IR and EPR), powder X-ray diffraction, thermogravimetric analysis (TGA), and mass spectrometry. A new ligand, namely biguanide-1,5-diethanoate (Bge) (C 6H 9N 5O 4), was formed during complexation, probably due to the reaction between two Gaa species and the consequent release of a significant amount of ammonia, thus, characterizing the deamination process. In complex 1, Bge behaved as a tetradentated ligand, using its oxygen and nitrogen atoms as coordinating sites to both Cu(II) ions. In addition, Glu has coordinated to Cu(II) through its α-N and O atoms. Theoretical calculations of the cis– cis, cis– trans, and trans– trans isomers of 1, considering three prototropic forms of the Bge ligand, were carried out using semi-empirical quantum mechanics (PM3/ d). DFT (B3LYP and B3P86) calculations of complex 1, in which a hydrogen atom replaced the side chain of Glu, were also carried out using the 6-31G(d) basis set and the LanL2DZ effective core potential for the transition metal. Based on experimental and theoretical data, we concluded that the trans– trans isomer of the binuclear copper(II) complex 1 should be the most stable, although the occurrence of other isomers, even if in minor quantities, should not be disregarded.

Designed Assemblies of Metal Halo and Pseudohalo Coordination Polymers with Bridging 1-Substituted Ditetrazoles

The simple reactions between inorganic salts [CuX 2 or M(SCN) 2 ] and 1-ditetrazoles [btzb = 1,4-bis(tetrazol-1 yl)butane or btze = 1,2-bis(tetrazol-1-yl)ethane] at room temperature produced seven new coordination polymers: three-dimensional (3-D) CuX 2 (1,4-btzb) (X - = Cl - 1, Br - 2), two-dimensional (2-D) Cd(SCN) 2 (1,4-btzb) (3) and Cd(SCN) 2 (1,2-btze) (4), and one-dimensional (1-D) M(SCN) 2 (1,4-btzb) 2 (M = Ni 5, Co 6) and Ni(SCN) 2 (1,2-btze) 2 (7). With 1-ditetrazoles as the bridges, the 2-D grid-like CuX 2 secondary building units (SBUs) are extended into 3-D network compounds 1 and 2, the 1-D chained Cd(SCN) 2 SBUs based on Cd(SCN) 2 Cd units are linked into 2-D layered compounds 3 and 4 with the macrocyclic rings, whereas the mononuclear trans-M(SCN) 2 units are connected into 1-D chained compounds 5-7 based on M(1-ditetrazole) 2 M macrocyclic rings. It deserves mentioning that 1-ditetrazoles show different shapes in different complexes: Z-shape in 1-4 and V-shape in 5-7. All the complexes are characterized by elemental analysis (CHNS), infrared spectroscopy, and thermogravimetric analysis.

1.10 – PHENANTHROLINE COMPLEXES OF THE RARE EARTH NITRATE: SYNTHESIS AND CHARACTERIZATION.

The interaction of lanthanide nitrates (Ln–Nd, Sm, Dy and Er) and 1.10–phenantroline were studied and complexes of the general formulae Ln(NO3)3(C12H8N2)2 or Ln(NO3)3(o-fen)2. The complexes were characterized by elemental analyses (CHN), titration with EDTA, IR spectra and thermogravimetric analysis. X-ray powder patterns further indicated that the complexes are isomorphous having the same d -interplanar spacing.

Synthesis and biological evaluation of 2-thiopyrimidine derivatives

Various 2-thiopyrimidine derivatives have been synthesized by an efficient, one-pot reaction of functionalized amines with either 4-isothiocyanato-4-methyl-2-pentanone or 3-isothiocyanatobutanal. All the synthesized compounds were fully characterized by elemental analysis (CHN), FT-IR, 1H NMR, and mass spectral data. One of the compounds, 7,7,8a-trimethyl-hexahydro-thiazolo[3,2- c]pyrimidine-5-thione ( 17) showed good anti-inflammatory (37.4% at 100 mg/kg p.o.) and analgesic activity (75% at 100 mg/kg p.o.). 7-(1-Mercapto-3,3,4a-trimethyl-4,4a,5,9b-tetrahydro-3 H-pyrido[4,3- b]indol-7-yl)-3,3,4a-trimethyl-3,4,4a,5-tetrahydro-benzo[4,5]imidazo[1,2- c]pyrimidine-1-thiol ( 3) showed moderate activity against CDK-1 (IC 50 = 5 μM). The other compounds showed moderate anti-inflammatory (5–20%), analgesic (25–75%) and protein kinase (CDK-5, GSK-3) inhibitory activities (IC 50 > 10 μM).

Synthesis, characterization, properties and structures of rhenium-(ii), -(iii), and -(v) complexes containing amino acids conjugated with a 2-aminothiazole ligand

The one-step reaction of KReO4 with benzoylhydrazine in the presence of concentrated HCl and PPh3 afforded [ReV(NNC(Ph)O)(PPh3)2Cl2] 1 which was converted with carbon monoxide into the dinitrogen Re(I) complex [ReN2(CO)2(PPh3)2Cl] 2 in good yield. A new class of ligands, of general formula HLn (n = 1–5), was obtained by conjugation of N-protected amino acids and benzoic acid with 2-aminothiazole. Complex 2 reacted with HLn to give neutral Re(II) chelate complexes [Re(Ln)(CO)(PPh3)2Cl] 5–9 (n = 1–5), by substitution of N2 and CO groups. The molecular structure of complex 9 was determined by X-ray diffraction. When reactions between [Re(NNC(Ph)O)(PPh3)2Cl2] 1 and HLn (n = 2, 5) were carried out in different stoichiometric ratios, neutral mono- and di-substituted Re(III) organodiazenido complexes [Re(NNCOPh)(L2,5)(PPh3)2Cl] 10, 11 and [Re(NNCOPh)(L5)2(PPh3)] 12 were obtained. In these complexes the organodiazenido Re–N–N moiety adopts a linear conformation, as has been authenticated by X-ray diffraction analysis for 11 and 12. Treatment of Re(I) dinitrogen precursors [ReN2(P)4Cl] (P = PMe2Ph, 3 and PMePh2, 4) with ligands resulted in interesting dinuclear oxo-(μ-oxo)-Re(V) species [Re2(O)3(Ln)2(P)2] (P = PMe2Ph, n = 1, 13; n = 2, 14; n = 4, 15. P = PMePh2, n = 2, 16). Suitable crystals for an X-ray analysis have been obtained for complex 14. The structure represents one of the few cases where, for steric reasons, the Re–O–Re bridging unit is not linear but rather bent. All the compounds have been characterized by elemental analyses, IR and NMR spectroscopy. The Re(II) complexes 5–7 and 9 were further characterized by electrochemical measurements.

Targeting Estrogen Receptor Sites in Human Breast Cancer Cell Line T47D With Copper Conjugates of Nonsteriodal Anti-inflammatory Drug Derivatives: Antiproliferative Activity of Ketoprofen Derivative and its Copper Complex

A square planar copper complex of derivatized NSAID drug (Ketoprofen thiosemicarbazone [3-benzoyl-α-methyl benzene acetic acid thiosemicarbazone]), is characterized by elemental analysis, spectroscopy, electrochemistry and magnetic susceptibility studies which exhibits dose-dependent and enhanced antiproliferative effects on human breast cancer cell line T47D rich in progesterone receptors.

Studies on Lanthanide Complexes of the Tripodal Ligand Tris(benzimidazol-2-ylmethyl)amine (ntb). Crystal Structures of [Ln(ntb)(NO3)3].H2O (Ln = Ce, Er)

The tripodal ligand tris(benzimidazol-2-ylmethyl)amine (ntb) reacts with lanthanide nitrates in methanol to give the mononuclear complexes [Ln(ntb)(NO3)3].H2O (Ln = La, Ce, Nd, Sm, Eu, Gd, Tb, Dy, Er) which have been characterized by elemental analyses, infrared, electronic and 1H n.m.r. spectroscopies, X-ray diffraction patterns, and conductivity measurements. The crystal and molecular structures of two complexes [Ln(ntb)(NO3)3].H2O (Ln = Ce, Er) have been determined. The cerium complex crystallizes in the monoclinic system, space group C2/c with a 26·79(1), b 14·497(8), c 17·20(1) Å, β 99·06(4)°, V 6596(6) Å3 , Z 8, while the erbium complex crystallizes in the cubic system, space group Pa-3 with a 18·2504(1) Å, V 6078·79(6) Å3, Z 8. In both cases the central metal ions are coordinated to the four nitrogen atoms of ntb and six oxygen atoms of three chelating nitrate groups. The total coordination number of the metal ion is 10. Spectroscopic analyses suggest that other complexes show a similar coordination mode. The fluorescence properties of the samarium(III), europium(III), terbium(III), and dysprosium(III) complexes were investigated.