0000000001302636
AUTHOR
R. Ortiz
Cooperative H-bonds, π⋯π and anion⋯π interactions as driving forces in the construction of novel Cu(II) bis(imidazol-2-yl) supramolecular 3D frameworks
Abstract Two new Cu(II) complexes with bis(2-imidazolyl) based ligands, with the formula [Cu(BIM)2(SCN)2]·2H2O (BIM = bis(2-imidazol-2-yl)methane) and [Cu(HBIMAM)2(OH2)2](BF4)4·2H2O (BIMAM = bis(2-imidazol-2-yl)methylaminomethane) have been synthesized and characterized. Both compounds contain mononuclear entities as molecular building blocks (MBBs); neutral [Cu(BIM)2(SCN)2] in compound 1 and cationic [Cu(HBIMAM)2(OH2)2]4+ in compound 2. The coordination around the metal atoms shows a tetragonally-elongated octahedral geometry (CuN4S2 and CuN4O2 chromophores). The Q-band EPR spectra of both compounds are indicative of an essentially d x 2 - y 2 ground state for copper(II) ions. The analysis…
Cinoxacin complexes with divalent metal ions. Spectroscopic characterization. Crystal structure of a new dinuclear Cd(II) complex having two chelate-bridging carboxylate groups. Antibacterial studies.
Several cinoxacin (HCx) complexes with divalent metal ions have been prepared and characterized by spectroscopic techniques. The crystal structure of [Cd 2 (Cx) 4 (H 2 O) 2 ] · 10H 2 O has been determined by X-ray diffraction. The complex is triclinic, space group with unit-cell dimensions: a =10.412(2), b =11.119(2), c =13.143(6)A, α=76.78(4)°, β =74.59(3)°, γ =77.12(3)°, V =1406.0(8) A 3 . In this complex each cadmium atom is heptacoordinated; the metal environment is formed by two O keto and two O carbox atoms from two different cinoxacinate monoanions, two carboxylate oxygen atoms from a third cinoxacinate ligand and by one water oxygen atom on the seventh position. Two of the cinoxacin…
Antibacterial studies, DNA oxidative cleavage, and crystal structures of Cu(II) and Co(II) complexes with two quinolone family members, ciprofloxacin and enoxacin
Nine coordination compounds of Cu(II) and Co(II) with Ciprofloxacin (HCp) and Enoxacin (HEx) as ligands have been prepared and characterized. Single crystal structural determinations of [Cu(HCp)2(ClO4)2].6H2O (1) and [Co(HEx)2(Ex)]Cl.2CH(3)OH.12H2O (4) are reported. The crystal of 1 is composed of [Cu(HCp)2(ClO4)2] units with the two perchlorate anions semicoordinated, and uncoordinated water molecules. The copper ion, at a crystallographic inversion centre, is in a tetragonally distorted octahedral environment. The structure of 4 consists of cationic monomeric [Co(HEx)2(Ex)]+ units, chloride anions, and uncoordinated methanol and water molecules. The complex is six-coordinate, with a sligh…
A framework to analyse gender bias in epidemiological research
The design and analysis of research may cause systematic gender dependent errors to be produced in results because of gender insensitivity or androcentrism. Gender bias in research could be defined as a systematically erroneous gender dependent approach related to social construct, which incorrectly regards women and men as similar/different. Most gender bias can be found in the context of discovery (development of hypotheses), but it has also been found in the context of justification (methodological process), which must be improved. In fact, one of the main effects of gender bias in research is partial or incorrect knowledge in the results, which are systematically different from the real…
Coordination behavior of cinoxacine: Synthesis and crystal structure of tris (cinoxacinate) cobaltate(II) of sodium hexahydrate (HCx = 1-ethyl-4(1H) -oxo-(1,3) dioxolo-(4,5g) cinnoline-3-carboxylic acid)
The synthesis, crystal, and molecular structure of Co(Cx)3Na6H2O are reported. The Cobalt(II) compound crystallizes in the trigonal system, space group R 3 with Z = 6, in a cell of dimensions a= 18.688(7) (A), c= 20.142(6) A. Least-squares refinement of 1331 reflections [I≥3σ(I)] gave a final R = 0.088 for all observed reflections. The structure consists of anionic monomeric units of (Co(Cx)3−) and sodium cations. Three Cinoxacinate ions are chelated through Oceto and Ocarbox atoms. The Co(II) ion positioned on the third axis is bonded to six oxygen atoms in a slightly distorted octahedral environment.
Synthesis, structure, and nuclease properties of several binary and ternary complexes of copper(II) with norfloxacin and 1,10 phenantroline
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 struct…
Interactions of metal ions with two quinolone antimicrobial agents (cinoxacin and ciprofloxacin)
Several novel metal-quinolone compounds have been synthesized and characterized by analytical, spectroscopic and X-ray diffraction methods. The crystal structure of the four compounds, Na(2)[(Cd(Cx)3)(Cd(Cx)3(H2O))].12H2O, [Co(Cp)2(H2O)2].9H2O, [Zn(Cp)2(H2O)2].8H2O and [Cd(HCp)2(Cl)2].4H2O, is presented and discussed: HCx=1-ethyl-1,4-dihydro-4-oxo(1,3)-dioxolo(4,5-g)cinnoline-3-carboxylic acid and HCp=1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-3-quinoline carboxylic acid. In all these compounds the quinolone acts as a bidentate chelate ligand that binds through one carboxylate oxygen atom and the exocyclic carbonyl oxygen atom. Complexes of ciprofloxacin were screened for th…
Fluoroquinolone–metal complexes: A route to counteract bacterial resistance?
Abstract Microbial resistance to antibiotics is one of the biggest public health threats of the modern world. Antibiotic resistance is an area of much clinical relevance and therefore research that has the potential to identify agents that may circumvent it or treat resistant infections is paramount. Solution behavior of various fluoroquinolone (FQ) complexes with copper(II) in the presence and absence of 1,10-phenanthroline (phen) was studied in aqueous solution, by potentiometry and/or spectrophotometry, and are herein described. The results obtained showed that under physiological conditions (micromolar concentration range and pH 7.4) only copper(II):FQ:phen ternary complexes are stable.…
Ni(II) and Zn(II) complexes with cinoxacin. Synthesis and characterization of M(Cx)2(DMSO)n(H2O)m (n=0, 2; m=2, 4). Crystal structures of [M(Cx)2(DMSO)2]·4H2O (M=Ni(II), Zn(II))
Abstract New metal complexes of cinoxacin (HCx=1-ethyl-l,4-dihydro-4-oxo(1,3)dioxolo(4,5-g)cinnoline-3-carboxylic acid) were synthesized, isolated as [Zn(Cx)2(DMSO)2]·4H2O, [Ni(Cx)2(DMSO)2]·4H2O, Zn(Cx)2·4H20 and Ni(Cx)2·2H2O, and characterized by elemental analysis, TG studies, IR and UVVis spectroscopic techniques. The crystal and molecular structures of the complexes [M(Cx)2(DMSO)2]·4H2O (M=Zn(II), Ni(II)) have been determined by X-ray structure analysis. The crystals of [Zn(Cx)2(DMSO)2]·4H2O are triclinic, space group P 1 with unit cell dimensions a=8.950(4), b=9.168(5), c=11.650(6) A, α=69.06(1), β=82.05(1), γ=75.63(1)°, V=863.6(8) A3; [Ni(Cx)2(DMSO)2]·4H20 is monoclinic, space group …
Synthesis, structure and biological properties of several binary and ternary complexes of copper(II) with ciprofloxacin and 1,10 phenanthroline
In this study, a new binary complex [Cu(HCip) 2 ](NO 3 ) 2 · 6H 2 O ( 1 ) has been synthesized and then characterized by X-ray structure analyses. In this compound, each ciprofloxacin acts as a bidentate ligand resulting in a crystallographically planar configuration; the nitrate anions are located in apical positions with an axial distance significantly larger than the equatorial distances, which would be consistent with a very weak metal ion interaction due to the Jahn–Teller effect. In addition, both the synthesis and characterization of two new ternary complexes of ciprofloxacin–copper(II)–1,10-phenanthroline, [Cu(phen)(Cip)](NO 3 ) · 4H 2 O ( 2 ) and Cu(phen)(HCip)(NO 3 ) 2 · H 2 O (…
Interactions of metal ions with a 2,4-diaminopyrimidine derivative (trimethoprim)
The interaction of copper (II), zinc(II) and cadmium(II) with Trimethoprim (2,4-diamino-5-(3',4',5'-trimethoxybenzyl) pyrimidine) has been studied. The crystal structures of [Zn(Trim)2Cl2] (2) and [Cd(Trim)Cl2(CH3OH)]n (4) are reported. Compound (2) exhibits a distorted tetrahedral environment around the metal center and crystallizes in the triclinic space group P1 with a=10.2397(6), b=10.4500(6), c=16.3336(16) A, alpha=96.141(8), beta=106.085(5), gamma=96.551(5) degrees and Z=2. In complex (4), the Cd(II) centers are bridged sequentially by two chlorine ions to form infinite chains and present a six-coordinated environment; the compound crystallizes in the monoclinic P2(1)/C space group wi…
Synthesis, characterization, and crystal structure of [Cu(cinoxacinate)2] · 2H2O complex: A square-planar CuO4 chromophore. Antibacterial studies
The structural and spectroscopic properties of a new copper (II) complex of cinoxacin (HCx) have been investigated. The complex [Cu(Cx)2].2H2O crystallizes in the monoclinic system, space group P2(1)/c. The cell dimensions are: a = 7.998(2), b = 7.622(1), c = 18.955(6) A, beta = 94.38(2) degree, V = 1154.6(6) A3, Z = 2. The structure was refined to R = 0.051. The crystal is composed of [Cu(Cx)2] units and uncoordinated water molecules. The Cu(II) ion, at a center of symmetry, is coordinated to two cinoxacinate (Cx) ligands related by the inversion center. Each cinoxacinate acts as bidentate ligand bonded to the cation through its carboxylate oxygen atom and through its exocyclic carbonyl ox…
ChemInform Abstract: Ternary Complexes of Cimetidine and Phenobarbital with Cu(II) in Methanolic Solution.
The formation constants of the binary complexes Cu(CM)2+ and Cu(CM) 2 2+ as well as those of the ternary complexes Cu(CM)L + and Cu(CM)2 L + (CM=Cimetidine=N-Cyano-N′-methyl-N″[(5-methyl-1H-imidazol-4-yl)methyltioethyl]-guanidine; HL=Phenobarbital=5-ethyl-5-phenyl-barbituric acid) have been determined in 0.1 and 1.0 mol dm−3 NaClO4 methanol solutions at 25±0.2°C. The values of logX, log βstat.., and Δ logK confirm the stability of the ternary complexes.
Potentiometric and spectroscopic studies of transition-metal ions complexes with a quinolone derivative (cinoxacin). Crystal structures of new Cu(II) and Ni(II) cinoxacin complexes
Abstract The interaction of cobalt(II), nickel(II), copper(II), and zinc(II) with Cinoxacin (HCx = 1-ethyl-1,4-dihydro-4-oxo(1,3)dioxolo(4,5-g)cinnoline-3-carboxylic acid), a 4-quinolone derivative, has been studied at metal/ligand ratios of 1:1-1:3 by means of pH-metric, spectrophotometric, and ESR methods. The formation constants have been determined and the stereochemistry for the metal ions in the species present in aqueous solutions (at 37 ± 0.1°C and I = 0.1 mol dm −3 NaCl) is discussed. In all the studied systems, complexes with different stoichiometric ratios, in which cinoxacin acts both as neutral and deprotonated ligand, are formed. The anomalous sequence of the stepwise stabilit…
Copper(II) Complexes with Derivatives of Barbiturate
Abstract NaCuL2(OH).1,5H2O, KCuP2(OH).1H2O, Na2CuL4 and K2CuP4-8H2O (HL=Phenobarbitone and HP=Methyl Phenobarbitone) were prepared and characterized by elemental analysis, IR and electronic spectral data and magnetic susceptibility measurements. The ESR spectra show and octahedral environment for the Cu(II) ion.
New dinuclear copper complexes incorporating bis(imidazolyl) based ligands and bidentate–monodentate oxalate bridges. Crystal structure and magnetic properties of [Cu2(BIM)2(C2O4)2]·4H2O and [Cu2(BIK)2(C2O4)2] (BIM=bis(2-imidazolyl)methane), BIK=bis(2-imidazolyl)ketone). Exploring magneto-structural correlations
Abstract This paper reports the synthesis, X-ray crystal structure and magnetic characterization of two novel copper(II) dinuclear compounds including bis(imidazolyl) ligands and oxalate anions, [Cu2(BIM)2(C2O4)2]·4H2O (1) (BIM = bis(2-imidazolyl)methane) and [Cu2(BIK)2(C2O4)2] (2) (BIK = bis(2-imidazolyl)ketone). The oxalate anion acts as bidentate–monodentate in both cases, although it exhibits different coordination bridging modes: whereas in compound 1 a μ1,1,2-oxalato is observed, a μ1,2,3-oxalato is found in compound 2. In both cases, the 3D framework is held together by a combination of H-bonding and aromatic-aromatic interactions provided by the convenient structural features of BIM…
Ternary complexes of cimetidine and phenobarbital with Cu(II) in methanolic solution
The formation constants of the binary complexes Cu(CM)2+ and Cu(CM) 2 2+ as well as those of the ternary complexes Cu(CM)L + and Cu(CM)2 L + (CM=Cimetidine=N-Cyano-N′-methyl-N″[(5-methyl-1H-imidazol-4-yl)methyltioethyl]-guanidine; HL=Phenobarbital=5-ethyl-5-phenyl-barbituric acid) have been determined in 0.1 and 1.0 mol dm−3 NaClO4 methanol solutions at 25±0.2°C. The values of logX, log βstat.., and Δ logK confirm the stability of the ternary complexes.
CCDC 702889: Experimental Crystal Structure Determination
Related Article: J.Hernandez-Gil, L.Perello, R.Ortiz, G.Alzuet, M.Gonzalez-Alvarez, M.Liu-Gonzalez|2009|Polyhedron|28|138|doi:10.1016/j.poly.2008.09.018
CCDC 702890: Experimental Crystal Structure Determination
Related Article: J.Hernandez-Gil, L.Perello, R.Ortiz, G.Alzuet, M.Gonzalez-Alvarez, M.Liu-Gonzalez|2009|Polyhedron|28|138|doi:10.1016/j.poly.2008.09.018
CCDC 652238: Experimental Crystal Structure Determination
Related Article: M.Ruiz, R.Ortiz, L.Perello, J.Latorre, J.Server-Carrio|1997|J.Inorg.Biochem.|65|87|doi:10.1016/S0162-0134(96)00092-X
CCDC 652237: Experimental Crystal Structure Determination
Related Article: M.Ruiz, R.Ortiz, L.Perello, J.Latorre, J.Server-Carrio|1997|J.Inorg.Biochem.|65|87|doi:10.1016/S0162-0134(96)00092-X