20 research outputs found

    Magnetic and structural studies into the effect of solvent exchange process in metal-organic framework MOF-76(Gd)

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    Effect of solvent exchange/absence on magnetic and structural properties of microporous metal-organic framework MOF-76(Gd) has been performed. Three compounds have been prepared and characterized: as synthesized MOF-76(Gd)-DMF, which containing DMF (N,N'-dimethylformamide) and H₂O molecules in the cavity system, activated complex without solvents, MOF-76(Gd) and water exchanged sample MOF-76(Gd)-H₂O. The structural study showed that compounds undergo structural changes after activation/exchange processes. Changes were mainly observed in the magnetic properties and distances between Gd...Gd ions: 4.718 Å for MOF-76(Gd)-DMF, 4.326 Å for MOF-76(Gd)-H₂O and 4.296 Å for MOF-76(Gd). The magnetic properties of the samples were studied by magnetic susceptibility χ_{M}(T) and magnetization M(H). The low positive value of the Weiss constant, Θ = 1.54 K in compound MOF-76(Gd)-DMF shows on a very weak ferromagnetic interaction. On the contrary, the negative values of Θ in complexes MOF-76(Gd) (-5.58 K) and MOF-76(Gd)-H₂O (-6.23 K) confirm the existence of antiferromagnetic exchange interaction between Gd(III) ions

    Structure and Magnetic Properties of Three-Dimensional Gadolinium-Based Hybrid Framework

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    In the present work we have focused on the preparation and magnetic study of coordination polymer formed by Gd(III) cations as nodes and formate (HCOO¯; FOR) anions as charge compensating linkers. The prepared complex with formula [Gd(μ3FOR)3]n{[Gd(μ_{3}-FOR)_{3}]}_{n} was characterized by single-crystal X-ray diffraction, and high-energy powder X-ray diffraction. The structural study showed that complex is formed by 3D polymeric network with the shortest Gd-Gd, distances of 3.998 Å. The magnetic properties of the complex were studied by magnetic susceptibility χM(T)χ_{M}(T) and magnetization M(H) measurements. The results show on the weak antiferromagnetic coupling at low temperatures represented by the Weiss constant θ=-0.468 K. The value of effective magnetic moment μeff=7.57μBμ_{eff}=7.57μ_{B}, which was estimated from the experimental data is close to the theoretical value for systems with S=7/2. Correlation between crystal structure of complexes and magnetic properties is presented

    Effect of Annealing Time on Structure of Fe72.5Cu1Nb2Mo2Si15.5B7\mathrm{Fe_{72.5}Cu_{1}Nb_{2}Mo_{2}Si_{15.5}B_{7}} Alloy

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    The process of a primary crystallization of the Fe72.5Cu1Nb2Mo2Si15.5B7Fe_{72.5}Cu_{1}Nb_{2}Mo_{2}Si_{15.5}B_{7} alloys was investigated by differential thermal analysis (DTA), x-ray diffraction (XRD) and transmission electron microscopy (TEM). Amorphous ribbons were isothermally annealed for 0.5, 2, 6, 30 and 150 minutes at 520 °C. Both, the XRD and TEM study showed that the level of devitrification of the sample increases with the annealing time. The above mentioned techniques confirmed the presence of the nanocrystalline grains of the Fe3SiFe_{3}Si phase and enable us to study the evolution of the identified phase

    Toxic metal complexes of macrocyclic cyclen molecule – synthesis, structure and complexing properties

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    Toxic metal (Cd2+, Hg2+, Pb2+, and Ag+) complexes with the tetradentate macrocyclic ligand - cyclen (1,4,7,10-tetraazacyclododecane, [12]aneN4, L) were prepared and studied in the solid state by IR, X-ray diffraction, elemental and thermal analysis. Diffraction results have yielded three molecular structures, [Cd([12]ane-κ4N1,4,7,10)(NO3)2)] (1), [Hg([12]ane-κ4N1,4,7,10)(NO3-κ2O,O`)]NO3 (2), [Pb2([12]ane-κ4N1,4,7,10)2][Pb(NO3)6] (3) and one polymeric structure {[Ag2([12]ane-κ3N1,4,7)(μ2-[12]aneN10)](NO3)2∙2H2O)}n (4) featuring a unique coordination mode not observed before with cyclen as a ligand. The monodentate (1) and chelate (with small bite angle 50.3(3)°, (2) coordination modes of nitrate ligands were confirmed. Stereochemically active 6s2 lone pair was suggested in 3 and DFT results confirmed no significant metal–metal covalent bond. The stability constants of the complexes with Cd2+ and Pb2+ ions were determined by potentiometric methods in aqueous solutions. Additionally, the structures of complexes in solution were observed by 1H NMR. Both methods confirm similar cyclen complexing properties toward Zn2+ biometal and Cd2+, Pb2+ toxic metals

    Ag(I) and Zn(II) isonicotinate complexes: Design, characterization, antimicrobial effect and CT–DNA binding studies

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    <div><p></p><p>Trinuclear Ag(I) (<b>1</b>) and dinuclear and mononuclear Zn(II) isonicotinate (<b>2</b> and <b>3</b>) complexes were prepared and characterized by X–ray crystallography, elemental analysis, IR spectroscopy and thermal analysis. Single crystal analysis of the Ag(I) complex reveals two different monodentate carboxylate coordination modes, protonated and deprotonated, respectively. IR spectra showed correlations between isonicotinate coordination modes and <i>Δ</i>(<i>ν</i><sub>as</sub>–<i>ν</i><sub>s</sub>)<sub>IR</sub> values. In addition, the hydrogen bonds significantly influence a position of carboxylate absorption bands. Moreover, IC<sub>50</sub> and MIC data for bacteria, yeasts and filamentous fungi were determined and the binding of Ag(I) and Zn(II) complexes to calf thymus DNA was investigated using electronic absorption, fluorescence and CD measurements. Biological tests showed that the Ag(I) complex is more active than commercially used Ag(I) sulfadiazine against <i>E. Coli</i>. The fluorescence spectral results indicate that the complexes can bind to DNA through an intercalative mode. The Stern–Volmer quenching constants for investigated complexes obtained from the linear quenching plot are in the range of 1.67 × 10<sup>4</sup> to 3.42 × 10<sup>4</sup> M<sup>–1</sup>.</p></div
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