scholarly journals Transition Metal Complexes with Flufenamic Acid for Pharmaceutical Applications—A Novel Three-Centered Coordination Polymer of Mn(II) Flufenamate

Materials ◽  
2020 ◽  
Vol 13 (17) ◽  
pp. 3705
Author(s):  
Michał Gacki ◽  
Karolina Kafarska ◽  
Anna Pietrzak ◽  
Małgorzata Szczesio ◽  
Izabela Korona-Głowniak ◽  
...  
Keyword(s):  
Free Ligand ◽  
Absorption Spectrometry ◽  
Antimicrobial Activities ◽  
Flufenamic Acid ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Metal Centers ◽  
Gram Positive Bacteria ◽  
Flame Atomic Absorption ◽  
Polymeric Chains

Five complexes of Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) with non-steroidal anti-inflammatory drug, flufenamic acid were synthesized: (1) [Mn3(fluf)6EtOH)(H2O)]·3EtOH; (2) [Co(fluf)2(EtOH)(H2O)]·H2O; (3) [Ni(fluf)2(EtOH)(H2O)]·H2O; (4) [Cu(fluf)2·H2O]; (5) [Zn(fluf)2·H2O]. All complexes were characterized by elemental analysis (EA), flame atomic absorption spectrometry (FAAS), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). The crystal structure of 1 was determined by the single crystal X-ray diffraction technique. It crystallizes in the triclinic space group P1¯ with three independent Mn(II) cations, six coordinated flufenamato ligands augmented with water and ethanol molecules in the inner coordination sphere. In this crystal, manganese atoms are multiplied by symmetry and form infinite, polymeric chains which extend along the [001] dimension. The Hirshfeld Surface analysis revealed changes in interaction assemblies around all metal centers. The antioxidant and antimicrobial activities were established for all complexes and free ligand for comparison. All compounds exhibit good or moderate bioactivity against Gram-positive bacteria and yeasts.

scholarly journals Quasi-Isostructural Co(II) and Ni(II) Complexes with Mefenamato Ligand: Synthesis, Characterization, and Biological Activity

Molecules ◽  
2020 ◽  
Vol 25 (13) ◽  
pp. 3099 ◽  
Author(s):  
Michał Gacki ◽  
Karolina Kafarska ◽  
Anna Pietrzak ◽  
Izabela Korona-Głowniak ◽  
Wojciech M. Wolf
Keyword(s):  
Absorption Spectrometry ◽  
Hirshfeld Surface ◽  
Polymeric Chain ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Gram Positive Bacteria ◽  
Flame Atomic Absorption ◽  
Intermolecular Contacts ◽  
Antioxidant And Antimicrobial Activity

Three metal complexes of mefenamato ligand 1 were synthesized: [Co2(mef)4(EtOH)2(H2O)4]: 2; [Co(mef)2(MeOH)4]∙2MeOH: 3; and [Ni(mef)2(MeOH)4]∙2MeOH: 4. Their compositions and properties were investigated by elemental analysis (EA), flame atomic absorption spectrometry (FAAS), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). Crystal structures were determined by the single crystal X-ray diffraction technique. Additionally, their antioxidant and antimicrobial activity were established, thus proving good/moderate bioactivity against Gram-positive bacteria and yeasts. In the crystal structure of 2, an apical water molecule is shared between two adjacent cobalt(II) ions, resulting in the formation of a polymeric chain extending along the [100] direction. Meanwhile, structures 3 and 4 have strong intermolecular hydrogen bonds with diverse topologies that yield unique quasi-isostructural arrangements. The packing topology is reflected by the Hirshfeld surface analysis of intermolecular contacts.

scholarly journals Double Palindrome Water Chain in Cu(II) Theophylline Complex. Synthesis, Characterization, Biological Activity of Cu(II), Zn(II) Complexes with Theophylline

Crystals ◽  
2020 ◽  
Vol 10 (2) ◽  
pp. 97 ◽  
Author(s):  
Michał Gacki ◽  
Karolina Kafarska ◽  
Anna Pietrzak ◽  
Izabela Korona-Głowniak ◽  
Wojciech M. Wolf
Keyword(s):  
Crystal Packing ◽  
Radical Scavenging ◽  
Absorption Spectrometry ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Flame Atomic Absorption ◽  
Hirshfeld Surfaces ◽  
Water Chain ◽  
Radical Scavenging Ability ◽  
Coordinated Water

Two metal complexes of theophylline were synthesized. Namely, 1 with the formula [Cu(theop)2(H2O)3]·2H2O and 2, [Zn(theop)2]∙H2O (where: theop = theophylline ion). Their properties were thoroughly investigated by the elemental analysis (EA), flame atomic absorption spectrometry (FAAS), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) that were augmented by antimicrobial and antioxidant analyses. Their radical scavenging ability (RSA) is notably higher than that of a pure theophylline itself. Similarly to theophylline complexes already studied by us 3, [Mn(theop)2(H2O)4] 4, [Co(theop)2(H2O)4] and 5, [Ni(theop)2(H2O)4] title compounds are inactive against Gram-negative bacteria, but they show moderate or mild activity against Gram-positive rods. The low temperature, single crystal X-ray diffraction technique determines the crystal structure of 1. Its supramolecular crystal topology is affected by the unique, double palindrome water chain that formed by two conserved and a sole coordinated water molecules. Crystal packing arrangements were characterized by fingerprint plots that were derived from the Hirshfeld surfaces (HS), as calculated for all structures in the series 1, 3, 4, 5.

A New Binuclear Lutetium(III) Dimethyl-N-trichloroacetylamidophosphate Complex with a γ, γ'-Dipyridyl Bridge, {Lu[CCl3C(O)NP(O)(OCH3)2]3}2-μ(γ,γ'-dipy)

2001 ◽  
Vol 56 (3) ◽  
pp. 249-254 ◽  
Author(s):  
Victor A. Trush ◽  
Jolanta Swiatek-Kozlowska ◽  
Victor V. Skopenko ◽  
Vladimir M. Amyrkhanov
Keyword(s):  
Crystal And Molecular Structure ◽  
Carbonyl Oxygen ◽  
Carbonyl Groups ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Metal Centers ◽  
X Ray ◽  
Heterocyclic Ligand ◽  
New Type ◽  
Ir Spectroscopic

Abstract A new type of binuclear coordination compound of lutetium, {Lu2L6 · μ-(γ,γ '-dipy)} (where L = dimethyl-N-trichloroacetylamidophosphate anion and γ,γ '-dipy = 4,4'-dipyridyl), has been obtained. The IR spectroscopic data reveal that the ambidentate phosphoryl ligand is coordinated to the metal center in a bidentate manner via the phosphoryl and carbonyl oxygen atoms. The crystal and molecular structure of {Ln2L6-μ-(γ ,γ '-dipy)} has been determined by means of X-ray diffraction (triclinic, space group P i with parameters: a = 9.259(2), b = 12.530(3), c = 16.548(3) Å, α = 85.44(3)°, β = 75.64(3)°, γ = 70.56(3)°, Z = 1). The structure is made up of centrosymmetric binuclear molecules, in which the neutral heterocyclic ligand is coordinated to the metal centers in a bidentate bridging manner via its nitrogen atoms. The coordination number of each Lu(III) atom is 7 [60(L-) + N((γ ,γ '-dipy)]. Phosphoryl and carbonyl groups of the L- ligands are disposed in syn-position and are included in the six-membered chelate metallocycles. The coordination polyhedron of lutetium can be described as distorted mono-capped octahedron.

scholarly journals Darstellung und Kristallstrukturen von (PH4P)4Sb8I28 und (Ph4P)Sb3I10(Ph = C6H5) / Synthesis and Crystal Structures of (PH4P)4Sb8I28 and (Ph4P)Sb3I10(Ph = C6H5)

1987 ◽  
Vol 42 (12) ◽  
pp. 1493-1499 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Detlev Haase
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Lone Pair ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Molar Ratios ◽  
Polymeric Chains ◽  
Bond Strengths

AbstractThe compounds (Pn4P)4Sb8I28 (1) and (Ph4P)Sb3I10 (2) were prepared by the reaction of SbI3 and Ph4PI in acetonitrile (molar ratios 2:1 and 3:1 respectively). The structures of 1 and 2 were determined from single crystal X-ray diffraction data.1 crystallizes in the triclinic space group P1̄ with a - 1321.7(5). b = 1346.7(5), c = 2201.8(8) pm, α = 104.18(2). β = 99.92(2), γ = 100.33(2)°; 2: monoclinic, C2/c, a = 2371.1(2), b = 745.0(1), c = 2495.1(2) pm, β = 100.75(1)°.Whereas 1 exhibits isolated Sb8I284- ions, the anions of 2 are built up of polymeric chains [Sb3I10- ]∞. In both compounds the distorted Sbl6 octahedra are linked by common edges. The Sb-I distances are in the range between 277.4 and 354.8 pm (1) and between 277.4 and 342.4 pm (2). The observed structures do not only depend on stoichiometry, the nature of the counter cations, and the possibility of oligomerisation but also on the wide variety of the Sb-I bond strengths and the different bridges formed by iodine.The lone pair of Sb(III) seems to be predominantly 5 s2.

Synthesis and Crystal Structure of a Novel Polymeric Lead(II) Complex with Thiosemicarbazonato and Thiocyanate Ligands

2001 ◽  
Vol 56 (6) ◽  
pp. 517-520 ◽  
Author(s):  
Alfonso Castiñeiras ◽  
Ricardo Domínguez ◽  
Leandro Bresolin ◽  
Jairo Bordinhão ◽  
Adaílton João Bortoluzzi ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Lead Atom ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Polymeric Chains

AbstractA novel heptacoordinated thiosemicarbazonato lead(II) complex [Pb(4ML)(SCN)] (4ML = 2-Acetylpyridine-4N-methylthiosemicarbazonato) was synthesized and characterized by conventional methods (IR and elemental analysis) and single-crystal X-ray diffraction. [Pb(4ML)(SCN)] shows an unusual polymeric structure in which the lead atom is hexa-coordinate, the deprotonated thiosemicarbazone both chelates and bridges, and the thiocyanate group acts as bridge between lead(II)-thiosemicarbazonate fragments. There is hydrogen-bonding between the polymeric chains. The complex crystallizes in the triclinic space group P 1̅̅ with a = 7.461(2), b = 9.572(2), c = 11.235(2) Å, α = 66.51(3), β = 84.01(3), γ = 68.75(3)°, V = 685.1(2) Å3, Z = 2.

CuIIand ZnIIβ-diketonate coordination polymers based on pyrimidin-2-amine, pyrazine and 1,2-bis(4-pyridyl)ethane

2016 ◽  
Vol 72 (6) ◽  
pp. 828-835 ◽  
Author(s):  
Franc Perdih
Keyword(s):  
Single Crystal ◽  
Coordination Polymers ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Metal Centers ◽  
Space Group ◽  
Π Interactions ◽  
Nitrogen Ligands ◽  
Polymeric Chains ◽  
Solid State Structures

Copper(II) and zinc(II) bis(4,4,4-trifluoro-1-phenylbutane-1,3-dionato) compounds with pyrimidin-2-amine (pyr2a), pyrazine (pyz) and 1,2-bis(4-pyridyl)ethane (dpet) were prepared and solid-state structures of coordination polymers [M(tfpb)2(pyr2a)]∞[M= Cu (1), Zn (2); tfpb = 4,4,4-trifluoro-1-phenylbutane-1,3-dionate], [M(tfpb)2(pyz)]∞[M= Cu (3), Zn (4a, 4b)] and [Cu(tfpb)2(dpet)]∞(5), respectively, were determined by single-crystal X-ray analysis. The coordination of metal centers in all compounds is octahedral with nitrogen ligands occupying the axial positions. Compound (1) crystallizes in the triclinic space group P\bar 1, whereas (2) crystallizes in the monoclinic space groupP2/n. Differences are due to the different orientation of adjacentM(tfpb)2units, whereas the orientation of pyrimidin-2-amine is the same in both compounds. Polymeric chains in (1) and (2) contain intramolecular N—H...O hydrogen bonding between amino and carbonyl groups. Room-temperature structures (3) and (4a) are isomorphous adopting the monoclinic space groupC2/m; however, on cooling crystals (4a) to 150 K a single-crystal-to-single-crystal transformation to (4b) possessing the triclinic space group P\bar 1 was observed. Compound (5) crystallizes in the triclinic space group P\bar 1 and contains a parallel aggregation of chains in contrast to the known structure of the non-fluorinated benzoylacetonato ligand, where chains aggregate in a perpendicular fashion. In the compounds studied intramolecular C—H...O and/or C—H...F interactions are present. The neighboring chains are linked by π...π interactions and in some compounds also by C—H...π interactions [(1), (4b), (5)].

scholarly journals Chitosan-S-triazinyl-bis(2-aminomethylpyridine) and Chitosan-S-triazinyl-bis(8-oxyquinoline) Derivatives: New Reagents for Silver Nanoparticle Preparation and Their Effect of Antimicrobial Evaluation

2020 ◽  
Vol 2020 ◽  
pp. 1-8
Author(s):  
Hessa H. Al-Rasheed ◽  
Kholood A. Dahlous ◽  
Essam N. Sholkamy ◽  
Sameh M. Osman ◽  
Omar H. Abd-Elkader ◽  
...  
Keyword(s):  
Particle Size ◽  
Silver Nanoparticles ◽  
Silver Ions ◽  
Antimicrobial Activities ◽  
X Ray Diffraction ◽  
X Ray ◽  
Modified Chitosan ◽  
Gram Positive Bacteria ◽  
Transmission Electron ◽  
Nanoparticle Preparation

Herein, we described the modification of chitosan with cyanuric chloride as a mediator for preparation of chitosan-s-triazinyl-bis(2-aminomethylpyridine) and chitosan-s-triazinyl-bis(8-oxyquinoline) derivatives to be used as reagents for preparation of silver nanoparticles under ecofriendly conditions. These two reagents are convenient and effective for reduction of silver ions to silver nanoparticles with particle size less than 10 nm that might be suitable for industrial and medicinal applications. The formation and particle size of AgNPs are characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), scanning electron microscope (SEM), and energy-dispersive X-ray analysis (EDX). The antimicrobial activity of the two modified chitosan-s-triazine-AgNPs was evaluated against activities against Gram-positive bacteria (M. luteus ATCC 10240 and MRSA ATCC 43300), Gram-negative bacteria (E. coli ATCC 25922 and P. aeruginosa ATCC 75853), and C. albicans. The results showed that chitosan-s-triazinyl-bis(2-aminomethylpyridine) AgNPs showed high antimicrobial activities against all the tested microorganisms, while their analogous chitosan-s-triazinyl-bis(8-oxyquinoline) AgNPs showed moderate activities.

scholarly journals Synthesis and Characterization of Novel Copper(II)-Sunitinib Complex: Molecular Docking, DFT Studies, Hirshfeld Analysis and Cytotoxicity Studies

Inorganics ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 3
Author(s):  
Facundo Tarasi ◽  
Priscila Ailín Lanza ◽  
Valeria Ferretti ◽  
Gustavo Alberto Echeverría ◽  
Oscar Enrique Piro ◽  
...  
Keyword(s):  
Molecular Docking ◽  
Solid State ◽  
Free Ligand ◽  
X Ray Diffraction ◽  
Allosteric Site ◽  
Triclinic Space Group ◽  
Atp Binding Site ◽  
Cytotoxicity Studies ◽  
Hirshfeld Analysis

The main goal of this work was to report the synthesis, characterization, and cytotoxicity study of a novel copper(II)-sunitinib complex, CuSun. It has been synthesized and characterized in solid state and in solution by different methods (such as DFT, FTIR, Raman, UV-vis, EPR, NMR, etc.). The solid-state molecular structure of trichlorosunitinibcopper(II), where sunitinib: N-[2-(diethylamino)ethyl]-5-[(Z)-(5-fluoro-2-oxo-1H-indol-3-ylidene)methyl]-2,4-dimethyl-1H-pyrrole-3-carboxamide, for short Cu(Sun)Cl3, was determined by X-ray diffraction. It crystallizes in the triclinic space group P-1 with a = 7.9061(5) Å, b = 12.412(1) Å, c = 13.7005(8) Å, α = 105.021(6)°, β = 106.744(5)°, γ = 91.749(5)°, and Z = 2 molecules per unit cell. Also, we have found π-π interactions and classic and non-classic H-bonds in the crystal structure by using Hirshfeld surface analysis. In the speciation studies, the complex has dissociated in protonated sunitinib and chlorocomplex of copper(II), according to 1HNMR, EPR, UV-vis and conductimetric analysis. Molecular docking of the complex in both, ATP binding site and allosteric site of VEGFR2 have shown no improvement in comparison to the free ligand. Besides, cytotoxicity assay on HepG2 cell line shows similar activity for complex and ligand in the range between 1–25 μM supporting the data obtained from studies in solution.

Provenance of loess from the Spanish central region: chemometric interpretation

2010 ◽  
Vol 148 (3) ◽  
pp. 481-491 ◽  
Author(s):  
R. GARCÍA ◽  
M. D. PETIT-DOMÍNGUEZ ◽  
M. I. RUCANDIO ◽  
J. A. GONZÁLEZ
Keyword(s):  
Chemical Composition ◽  
Central Region ◽  
Mineralogical Composition ◽  
Absorption Spectrometry ◽  
Bulk Sample ◽  
Heavy Minerals ◽  
X Ray Diffraction ◽  
Average Composition ◽  
Flame Atomic Absorption

AbstractIn this work our purposes are (1) geochemical characterization of loess (‘primary loess’ or ‘true loess’ and ‘secondary loess’ or ‘loess-like deposits’) located in the centre of the Iberian Peninsula, (2) systematic study of element behaviour during pedogenesis and (3) evaluation of the suitability of using the geochemistry of loess to establish the average composition of these discontinuous aeolian sedimentary covers in central Spain. Several analyses were carried out on the bulk sample and on the sandy and clay fractions (mineralogical composition by X-ray diffraction, mineralogical studies of heavy minerals by petrographical microscopy and chemical composition by flame atomic absorption spectrometry). Loess from the Spanish central region has a local origin. The presence of gypsum in the ‘loess-like’ deposits reaches values two times higher than in ‘true loess’, and ‘true loess’ has a higher concentration of quartz, calcite and kaolinite. Regarding chemical composition, similar concentrations of Ca, K, Mg and Na were found, although it is important to note the higher concentration of Na in some of the samples.

Levels of selected metals in coriander (Coriandrum sativum L.) leaves cultivated in four different areas of Ethiopia

2019 ◽  
Author(s):  
Chem Int
Keyword(s):  
Pearson Correlation ◽  
Absorption Spectrometry ◽  
Coriandrum Sativum ◽  
Good Source ◽  
Digestion Method ◽  
Flame Atomic Absorption ◽  
Significant Difference ◽  
Metal Levels ◽  
Good Percentage ◽  
Coriander Leaves

Coriander (Coriandrum sativum L.) is one of the herbs which is used for medicinal and food purposes. In the present study the levels of selected metals in coriander leaves were determined in the samples collected from four different farmlands (Sebeta, Mekanisa, Holeta and Gefersa) in Ethiopia where its cultivation is common. The levels of metals were determined after digestion of samples with the mixture of 4 mL of HNO3 and 4 mL of HClO4 at 300 oC for 3:00 hours by flame atomic absorption spectrometry. The optimized wet digestion method for coriander leaves analysis was validated through the recovery experiment and a good percentage recovery was obtained (93.2-101%). The levels of metals were found in the range Ca, 2319–3503 mg/kg; Zn, 33.4–54.8 mg/kg and Cr, 5.55-9.86 mg/kg while the trace metals Cu, Ni, Cd and Pb were too low to be detected. The results indicated that Ethiopian coriander is a good source of essential metals and free from the toxic metals Pb and Cd. A statistical analysis of variance (ANOVA) at 95% confidence level indicated that there is significant difference (p < 0.05) in the levels of all detected metals between the four sample means. The Pearson correlation was used to predict the dependence of metal levels on one another. The levels of the metals determined in this study compared well with those reported for coriander leaves from some other parts of the world.

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