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Perdih F.,University of Ljubljana | Perdih F.,CO EN FIST
Journal of Coordination Chemistry | Year: 2012

Three copper(II) bis(pentane-2,4-dionato- 2 O,O) compounds with 2-amino-3-methylpyridine (2,3-ampy) (1), 2-amino-5-methylpyridine (2,5-ampy) (2), and 2-amino-4-methylpyridine (2,4-ampy) (3) were prepared by reaction of bis(pentane-2,4-dionato- 2 O,O)copper(II) with selected methyl substituted 2-aminopyridines. The coordination of Cu(II) in all three compounds is square pyramidal and intramolecular N-HO hydrogen-bonding is present. X-ray crystallographic studies reveal different crystal aggregation influenced by a methyl substituent on pyridine. No intermolecular N-HO hydrogen-bonding is present in 1. Intermolecular N-HO hydrogen-bonding in 2 forms infinite chains and dimers are formed in 3. Extended 3-D aggregation was found in 2 via-and C-H (arene) interactions, while only chain formation was found in 1 and 3. © 2012 Copyright Taylor and Francis Group, LLC.


Kolesa-Dobravc T.,University of Ljubljana | Kolesa-Dobravc T.,CO EN FIST | Lodyga-Chruscinska E.,Technical University of Lodz | Symonowicz M.,Technical University of Lodz | And 4 more authors.
Inorganic Chemistry | Year: 2014

Oxidovanadium(IV) complexes with 5-cyanopyridine-2-carboxylic acid (HpicCN), 3,5-difluoropyridine-2-carboxylic acid (HpicFF), 3-hydroxypyridine-2- carboxylic acid (H2hypic), and pyrazine-2-carboxylic acid (Hprz) have been synthesized and characterized in the solid state and aqueous solution through elemental analysis, IR and EPR spectroscopy, potentiometric titrations, and DFT simulations. The crystal structures of the complexes (OC-6-23)-[VO(picCN)2(H2O)]·2H2O (1·2H2O), (OC-6-24)-[VO(picCN)2(H 2O)]·4H2O (2·4H2O), (OC-6-24)-Na[VO(Hhypic)3]·H2O (4), and two enantiomers of (OC-6-24)-[VO(prz)2(H2O)] (λ-5 and Δ-5) have been determined also by X-ray crystallography. 1 presents the first crystallographic evidence for the formation of a OC-6-23 isomer for bis(picolinato) VIVO complexes, whereas 2, 4, and 5 possess the more common OC-6-24 arrangement. The strength order of the ligands is H 2hypic ≫ HpicCN > Hprz > HpicFF, and this results in a different behavior at pH 7.40. In organic and aqueous solution the three isomers OC-6-23, OC-6-24, and OC-6-42 are formed, and this is confirmed by DFT simulations. In all the systems with apo-transferrin (VO)2(apo-hTf) is the main species in solution, with the hydrolytic VIVO species becoming more important with lowering the strength of the ligand. In the systems with albumin, (VO)xHSA (x = 5, 6) coexists with VOL2(HSA) and VOL(HSA)(H2O) when L = picCN, prz, with [VO(Hhypic)(hypic)] -, [VO(hypic)2]2-, and [(VO) 4(μ-hypic)4(H2O)4] when H 2hypic is studied, and with the hydrolytic VIVO species when HpicFF is examined. Finally, the consequence of the hydrolysis on the binding of VIVO2+ to the blood proteins, the possible uptake of V species by the cells, and the possible relationship with the insulin-enhancing activity are discussed. © 2014 American Chemical Society.


The influence of the introduced fluorine atoms to diketonato backbone exerted on the crystal packing was studied on cobalt(II) bis(4,4,4-trifluoro-1- phenylbutane-1,3-dionato-κ 2 O,O′) compounds with pyridine (1), 2,2′-bipyridine (2) and 1,10-phenanthroline (4), and cobalt(II) bis(benzoylacetonato-κ 2 O,O′) compound with 2,2′-bipyridine (3). The solid-state structures of 1-4 were determined by single crystal X-ray analysis. The coordination of Co(II) is octahedral in all four compounds. The differences in crystal packing of 1 with regard to the known complexes with non-fluorinated analogue and 4,4,4-trifluoro-1-(4-fluorophenyl) butane-1,3-dionate were observed. Unit cell parameters of 2·1/2C 7H8 and 3·1/2C7H8 slightly differ, but they have similar crystal packing dominated by the π-π interactions. Strong π-π interactions and weak C- H···π(arene) and C-F···π(arene) interactions are present in 2-4, while no significant intermolecular interactions are present in 1. © 2013 Springer Science+Business Media New York.


Perdih F.,University of Ljubljana | Perdih F.,CO EN FIST
Acta Crystallographica Section E: Structure Reports Online | Year: 2012

In the crystal structure of the title 1:1 co-crystal, C6H 7N2O+·C2Cl3O 2 -·C6H6N2O, the amide groups of the 4-carbamoylpyridin-1-ium ion and the isonicotinamide molecule are twisted out of the plane of the aromatic ring with C - C - C - N torsion angles of 21.5 (4) and -33.5 (4)°, respectively. The 4-carbamoylpyridin-1-ium and isonicotinamide amide groups form R 2 2(8) hydrogen-bonded dimers via N - H⋯O=C interactions. The two remaining amide H atoms (i) link dimers via the cation to an isonicotinamide and (ii) from the isonicotinamide to a trichloro-acetate anion. The pyridinium H atom also forms an N - H⋯O hydrogen bond with the trichloro-acetate anion. Due to the extended hydrogen bonding, including C - H⋯O and C - H⋯Cl interactions, all components in the structure aggregate into a three-dimensional supra-molecular framework.


Perdih F.,University of Ljubljana | Perdih F.,CO EN FIST
Acta Crystallographica Section E: Structure Reports Online | Year: 2012

In the asymmetric unit of the title salt, C6H7N 2O+·C2Cl3O2 -, there are two crystallographic independent ion pairs. The amide groups of the 4-carbamoylpyridin-1-ium ions are slightly twisted out of the plane of the aromatic ring with C - C - C - N torsion angles of 8.8 (9)° and 4.6 (8)°. In the crystal, the 4-carbamoylpyridin-1-ium ion is N - H⋯O hydrogen bonded to the trichloro-acetate ion via the pyridinium unit and amide group. Layers parallel to the ac plane are formed due to the N - H⋯O hydrogen bonding of the adjacent amide groups of 4-carbamoylpyridin- 1-ium ions. Weak C - H⋯O interactions also occur.


Perdih F.,University of Ljubljana | Perdih F.,CO EN FIST
Acta Crystallographica Section E: Structure Reports Online | Year: 2012

In the title compound, [Al(C5H6ClO2) 3], the AlIII cation is situated on a twofold rotation axis and is coordinated by six O atoms from three 3-chloropentane-2,4-dionate ligands in an octahedral environment. Al - O bond lengths are in the range 1.8741 (14)-1.8772 (14) Å. In the crystal, molecules are linked via C - H⋯Cl contacts.


Perdih F.,University of Ljubljana | Perdih F.,CO EN FIST
Acta Crystallographica Section E: Structure Reports Online | Year: 2012

In the title compound, [Al(C7H9O2) 3], the AlIII cation is coordinated by six O atoms from three 2-acetyl-cyclo-penta-nonate ligands in a slightly distorted octahedral environment, with Al - O bond lengths in the range 1.882 (2)-1.896 (2) Å. In the crystal, molecules are linked together via C - H⋯O interactions. One of the C atoms in one ring has a large thermal motion compared to the other atoms, indicating some possible disorder. However, the treatment of this C atom as disordered over two positions did not give a significant improvement.


Perdih F.,University of Ljubljana | Perdih F.,CO EN FIST
Acta Crystallographica Section E: Structure Reports Online | Year: 2012

In the title compound, [Fe(C5H6ClO2) 3], the FeIII cation is situated on a twofold rotation axis and is coordinated by six O atoms from three 3-chloropentane-2,4-dionate ligands in a slightly distorted octahedral environment. Fe - O bond lengths are in the range 1.9818 (18)-1.9957 (18) Å. The trans O - Fe - O angles are 169.06 (13) and 171.54 (8)°, whereas the corresponding cis angles are in the range 84.81 (10)-100.68 (12)°. In the crystal, molecules are linked via C - H⋯Cl interactions.


Perdih F.,University of Ljubljana | Perdih F.,CO EN FIST
Acta Crystallographica Section E: Structure Reports Online | Year: 2011

In the title compound, [Co(C5H7O2) 2(C12H8N2)], the CoII cation lies on a twofold rotation axis and is coordinated by four O atoms from two acetylacetonate (acac) ligands and two N atoms from a 1,10-phenanthroline (phen) ligand in a slightly distorted octahedral environment, with Co - O bond lengths of 2.0565 (11) and 2.0641 (11) Å and Co - N bond lengths of 2.1630 (12) Å. In the crystal, there are no significant hydrogen-bonding or π-π interactions.


Copper(II) bis(pentane-2,4-dionato-κ 2O,O′) compounds with 2-pyridone (1) and 3-hydroxypyridine (2) were prepared by the reaction of bis(pentane-2,4-dionato-κ 2O,O′) copper(II) with selected ligands. The coordination of Cu(II) in both compounds is square pyramidal with the fifth coordination site occupied by the carbonyl oxygen atom of the 2-pyridone ligand in 1 and by the nitrogen atom of 3-hydroxypyridine in 2. The X-ray crystallographic studies revealed different crystal aggregation influenced by the ability of the 2-pyridone ligand to act as a hydrogen bond donor and acceptor, and 3-hydroxypyridine acting only as a hydrogen bond donor. Intermolecular N-H⋯O hydrogen bonding forms dimers in 1 and infinite chains in 2. Three-dimensional aggregation is achieved by π-π interactions and C-H⋯π (arene) hydrogen bonding. © 2012 Springer-Verlag.

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