Ivan Leban

Crystal structure and characterization of the bismuth(III) compound with quinolone family member (ciprofloxacin). Antibacterial study

Two bismuth(III) compounds of ciprofloxacin (cf) were synthesized. The crystal structure of one--(cfH2) (cfH) [BiCl6].2H2O (cfH2 = doubly protonated molecule of cf, cfH = protonated molecule of cf)--is presented and discussed. The compound crystallizes in the monoclinic space group P 21/c with a = 17.758(4), b = 7.600(10), c = 31.908(6) A, beta = 101.03(2)0, Z = 4. The charge of the isolated hexachlorobismuthate(III) anions is compensated with protonated of molecules (ionic interactions). One of the cf molecules is protonated at carbonyl oxygen O(1) and nitrogen N(24) of the piperazine residue, and the other at N(24) only. Two water molecules participate in the hydrogen bond network. Antimicrobial activity of this compound was tested against different microorganisms. The results of TG and FT-IR measurements are also included.

Synthesis, crystal structure, and characterization of three novel compounds of the quinolone family member (norfloxacin)

The synthesis of three novel compounds of norfloxacin (nf) is reported. Their crystal structures are presented and discussed. The first compound, (nfH2)Cl2. H2O (nfH2 = doubly protonated molecule of nf), crystallizes in the monoclinic space group P 21/c with a = 8.438(2), b = 14.281(3), c = 15.012(3) A, β = 93.87(3)°, Z = 4. The carbonyl oxygen O(1) is protonated, and this proton is bonded via intramolecular hydrogen bond to the oxygen O(11) of the carboxylic group (O(11) … O(1) = 2.605(4) A). The terminal nitrogen atom N(24) the piperazine group is also protonated. The positive charge of the nf molecule is neutralized by two chloride anions. The crystal structure is stabilized by numerous hydrogen bonds of the type OH … O, OH … Cl, NH … Cl. The compounds (nfH2)(nfH)[CuCl4]Cl.H2O and (nfH2)(nfH)[ZnCl4]Cl.H2O (nfH = monoprotonated molecule of nf) are isostructural and both crystallize in P 21/c. Both structures are ionic consisting of a tetrachlorometalate (II) anion and two nonequivalent, protonated nf molecules. It seems that in strongly acidic media, the proton is bonded between O(1) and carboxylic oxygen, which prevents the coordination of the metal ions to this position. The results of other measurements (TG, FT-IR, Raman spectroscopy) are also included.

Synthesis, characterization, and crystal structure of a copper(II) complex with quinolone family member (ciprofloxacin): bis(1)-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-piperazin-1ylquinoline-3-carboxylate) copper(II) chloride hexahydrate

The synthesis of the coordination compound [Cu(CF)2]Cl2.6H2O is reported. Its crystal structure is presented and discussed. The title compound crystallizes in the triclinic space group P1 with a = 9.369(2), b = 9.573(2), c = 11.206(2) A, α = 87.37(2), β = 80.58(2), γ = 86.25(2)°, Z = 988.8 A3 Z = 1, and Dc = 1.520 gcm−3. A structure determination, using three-dimensional MoKα x-ray data, resulted in conventional R and Rw values of 0.0399 and 0.0988, respectively, for 3495 unique reflexions for which I > 2σ(I). Refinement was based on F2. The copper atom at the center of inversion is surrounded in a plane by four oxygens (two of the carboxylate groups, two of the carbonyl groups), the corresponding CuO distances are 1.928(2) and 1.931(2) A, respectively. The two chlorine atoms are axially coordinated to Cu at larger distances than 2.688(2) A. The Cl atoms appeared to be disordered over three positions. The nearly planar moieties of Cu(CF)2 are packed parallel in the unit cell interconnected via hydrogen bonds of the type NH⋯O, OH⋯Cl and OH⋯O. The results of other physical measurements (TG, FT-IR, and various analyses) are also included.

COMPLEXES OF COPPER(II) ACETATE WITH NICOTINAMIDE : PREPARATION, CHARACTERIZATION AND FUNGICIDAL ACTIVITY; CRYSTAL STRUCTURES OF CU2(O2CCH3)4(NIA) AND CU2(O2CCH3)4(NIA)2

Abstract Three new copper (II) acetate complexes with nicotinamide (nia) were synthesized analyzed and characterized by standard chemical and physical methods and tested for fungicidal activity The crystal and molecular structures of the compounds [Cu2 (O2CCH3)4 (nia)] (1B) and [Cu2 (O2CCH3)4 (nia)2] (2) were determined by X-ray diffraction Both consist of binuclear units of bridging tetracarboxylate type however they differ in the bonding mode of nicotinamide molecules They are bonded at the apical positions of the dimers and connect them in an infinite chain in 1B On the other hand the dimers remain isolated in the structure of the compound 2 It seems that compound 1B is the first example where a nicotinamide molecule acts as a bidentate bridging ligand The results of EPR spectra agree with the dimeric nature of the complexes Dissolved in water or DMSO the compounds completely stop mycelial growth at a concentration of 50×10−3 mol l−1 Less concentrated solutions (up to 10×10−3 mol l−1) show weaker fungicidal activity.

SYNTHESIS, CRYSTAL STRUCTURE, AND CHARACTERIZATION OF TWO METAL-QUINOLONE COMPOUNDS

Two novel metal-quinolone compounds have been synthesized and characterized by analytical, spectroscopic, and X-ray diffraction methods. The crystal structure of both, (erxH2) [FeCl4]Cl and (kinoH2)[CuCl4]. H2O, is presented and discussed (erxH2 = doubly protonated form of enrofloxacin, kinoH2 = doubly protonated form of the second quinolone). In both compounds, the hydrogen atom is bonded between the 4-keto oxygen O(1) and carboxylic oxygen O(11), thus preventing the bonding of the metal to this part of the molecule. Antimicrobial activities of metal-quinolone compounds were tested against different microorganisms.

An Adduct of Magnesium Sulfate with a Member of the Quinolone Family (Ciprofloxacin)

In the title compound, 4-(3-carboxy-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-quinolinyl)-1- piperazinium—magnesium hexahydrate—sulfate—water(1/0.5/1/3), (C17H19FN3O3)[Mg(H2O)6]0.5SO4.3H2O, the Mg2+ ion lies on a twofold axis and adopts a nearly regular octahedral geometry. The quinolone is protonated at the terminal N atom of the piperazine residue. The H atom of the carboxylic group is hydrogen bonded to the carbonyl O atom, thus preventing the bonding of the metal to this part of the molecule.

Synthesis and the crystal structures of a monoanionic tetrafluorodentate ligand and its complex with lanthanum ion

Abstract New organotitanium fluorides [Hdmpy]+[(C5Me4R)2Ti2F7]− (R=Me 4, Et 5, dmpy=2,6-dimethylpyridine, lutidine) have been prepared from (C5Me4R)TiF3 and 2,6-dimethylpyridine·(HF)2. The compounds 4 and 5 react with La(CF3SO3)3 to give [La{(C5Me4R)2Ti2F7}3] (R=Me 6, Et 7) containing the [(C5Me4R)2Ti2F7]− anion as a tetrafluorodentate ligand in the crystal structures of 4 and 7. The cation–anion pair is connected by a hydrogen bond in 4 and the all-fluorine environment of 12 fluorine atoms coordinated to a lanthanum ion is found in 7.

Preparation and characterization of copper(II) coordination compounds with linear chain fatty acids with 7–12 carbon atoms and pyridine. Crystal structure of Cu(O2CC8H17)2(py)2(H2O)

Abstract Mononuclear compounds of the composition CuX2(py)2(H2O) and binuclear of the composition Cu2X4(py)2 (py = pyridine, X = heptanoate, octanoate, nonanoate, decanoate or dedecanoate) were prepared, analysed and characterized by vibrational spectroscopy and thermogravimetry. Generally, the complexes are unstable, the mononuclear being even less stable than binuclear, losing pyridine in air at room temperature. The X-ray crystal structure of the mononuclear adduct of copper(II) nonanoate with pyridine, Cu(O2CC8H17)2(py)2(H2O), was determined by X-ray diffraction. The copper(II) ion is in a square pyramidal environment with two pyridine nitrogen atoms and two oxygen atoms from unidentate nonaoato ligands forming the basal plane of the pyramid and a water molecule coordinated at the apex. The carboxylate oxygen O(2) is not coordinated to copper, but is bound to water from a neighbouring molecule by the OHO(2) hydrogen bond of 2.691 (5) A.

1,3-Dipolar Cycloadditions to (5Z)-1-Acyl-5-(cyanomethylidene)- imidazolidine-2,4-diones: Synthesis and Transformations of Spirohydantoin Derivatives

Cycloadditions of various 1,3-dipoles to (5Z)-1-acyl-5-(cyanomethylidene)-3-methylimidazolidine-2,4-diones 8 or 9, prepared in 3 steps from hydantoin (1) (Schemes 1 and 2), were studied. In all cases, reactions proceeded regio- and stereoselectively. The type of product depended on the 1,3-dipole and/or dipolarophile employed as well as on reaction conditions. Thus, with stable dipoles under neutral conditions, spirohydantoin derivatives 12 – 16 were obtained (Scheme 2), while under basic or acidic conditions, pyrazole- or isoxazole-5-carboxamides 18 and 23 – 26 and carboxylate 27 were formed via aromatization of the newly formed dihydroazole ring, followed by the simultaneous cleavage of the hydantoin ring (Schemes 3 – 5).

The crystal and molecular structure of tetrakis(μ-octanoato-O,O′)-bis(pyridine)dicopper(II)

Abstract The crystal structure of the adduct of copper(II) octanoate with pyridine, (Cu2(C7H15COO)4(C5H5N)2, has been determined by X-ray diffraction. The complex forms discrete centrosymmetric tetracarboxylate-bridged dimers with pyridine moieties in the apical positions.