CCDC 2057269: Experimental Crystal Structure Determination. Crystallographic data for "Charge assisted assembly of zwitterionic pyridone hydrates"

UREZEZ : 4-methyl-6-oxo-5-(pyridin-1-ium-1-yl)-1,6-dihydropyridin-2-olate dihydrate Space Group: P 1 (2), Cell: a 7.2258(14)Å b 8.0470(16)Å c 11.287(2)Å, α 70.71(3)° β 74.88(3)° γ 79.85(3)°Crystallographic data (CCDC 2057269) for the article: Mašulović, A. D., Lađarević, J. M., Radovanović, L. D., Vitnik, Ž. J., Vitnik, V. D., Rogan, J. R.,& Mijin, D. Ž. (2021). Charge assisted assembly of zwitterionic pyridone hydrates. Journal of Molecular Structure, Elsevier., 1237, 130419. [https://doi.org/10.1016/j.molstruc.2021.130419]The published version of the article: [https://cer.ihtm.bg.ac.rs/handle/123456789/4506]The peer-reviewed version of the article: [https://cer.ihtm.bg.ac.rs/handle/123456789/4507]Supporting information: [https://cer.ihtm.bg.ac.rs/handle/123456789/4508]Related crystallographic data (CCDC 2057270): [https://cer.ihtm.bg.ac.rs/handle/123456789/4510

Complexes of d-block elements with aromatic o,o- and n,n-donor ligands: synthesis, structure, properties and applications

Reakcijom izmene liganada različitim metodama sinteze dobijeno je 22 ternarna kompleksa elemenata d-bloka [Mn(II), Co(II), Ni(II), Cu(II) i Zn(II)] sa anjonima aromatičnih polikarboksilnih kiselina (ftalne, izoftalne, tereftalne i piromelitne) kao O,O-donorskim ligandima i aromatičnim N,N-donorskim ligandima kao što su 2,2'-dipiridilamin i 2,2'-bipirimidin. Trinaest kompleksa sintetisano je u monokristalnom obliku, dok su ostala jedinjenja mikrokristalna. Prema vrsti centralnog atoma, u obliku monokristala dobijeno je pet Mn(II)-, dva Co(II)-, jedan Ni(II)-, dva Cu(II)-, dva Zn(II)-kompleksa, kao i bimetalni Mn(II)–Cu(II)-kompleks...A series of 22 d-block element complexes [Mn(II), Co(II), Ni(II), Cu(II) and Zn(II)] containing anions of aromatic polycarboxylate acids (phthalic, isophthalic, terephthalic and pyromellic) as O,O-donor ligands and aromatic N,N-donor ligands such as 2,2'-dipyridylamine and 2,2'-bipyrimidine, has been obtained by ligand exchange reaction using different synthetic methods. Thirteen complexes were obtained as single crystals, while the others were microcrystalline powders. According to the type of central atom, five Mn(II), two Co(II), one Ni(II), two Cu(II), two Zn(II) complexes, and bimetallic Mn(II)–Cu(II) complex were synthesized in form of single crystals. The structures of these compounds were determined by single-crystal X-ray analysis. Structural properties of complexes were discussed in detail and compared..

CCDC 2057270: Experimental Crystal Structure Determination. Crystallographic data for "Charge assisted assembly of zwitterionic pyridone hydrates"

UREZID : 3-(3,5-dimethylpyridin-1-ium-1-yl)-4-methyl-6-oxo-1,6-dihydropyridin-2-olate tetrahydrate Space Group: P 1 (2), Cell: a 7.4411(15)Å b 10.581(2)Å c 11.235(2)Å, α 108.96(3)° β 96.14(3)° γ 107.41(3)°Crystallographic data (CCDC 2057270) for the article: Mašulović, A. D., Lađarević, J. M., Radovanović, L. D., Vitnik, Ž. J., Vitnik, V. D., Rogan, J. R.,& Mijin, D. Ž. (2021). Charge assisted assembly of zwitterionic pyridone hydrates. Journal of Molecular Structure, Elsevier., 1237, 130419. [https://doi.org/10.1016/j.molstruc.2021.130419]The published version of the article: [https://cer.ihtm.bg.ac.rs/handle/123456789/4506]The peer-reviewed version of the article: [https://cer.ihtm.bg.ac.rs/handle/123456789/4507]Supporting information: [https://cer.ihtm.bg.ac.rs/handle/123456789/4508]Related crystallographic data (CCDC 2057269): [https://cer.ihtm.bg.ac.rs/handle/123456789/4509

Towards understanding intermolecular interactions in hydantoin derivatives: the case of cycloalkane-5-spirohydantoins tethered with a halogenated benzyl moiety

A series of cycloalkane-5-spirohydantoins bearing a halogeno substituted benzyl group (X = Cl and Br) in position 3 has been synthesized and their structures (1-6) have been determined by a single crystal X-ray diffraction method. These compounds have multiple functional groups, which allow greater competition and/ or cooperation among the different intermolecular interactions in the formation of their crystal structures. The molecules are linked together by paired N-H... O hydrogen bonds in R22(8) rings, while the CH. O interactions lead to their further association into double chains. The contribution of the cycloalkyl ring depends on its conformational flexibility and the multiple C-H donor implications. In the case of compounds 1-4 bearing the cyclopentyl or the cyclohexyl ring, halogen bonding (X...O) interactions give rise to a supramolecular pseudo-hexagonal network. In addition, the C-H... X interactions with a higher degree of multifurcation at the halogen acceptor have an important role in the formation of the crystal structure. Regarding compounds 5 and 6 with the cycloheptane ring, the X. O interaction is absent, and along with the C-H. X interactions, these compounds realize an alternative crystal structure with an emphasis on the X. p interactions. The lattice energies of all these crystal structures, as well as the intermolecular pair energies, have been calculated using PIXEL and further partitioned into coulombic, dispersive, polarization and repulsive factors. The crystal structures have also been subjected to Hirshfeld surface analysis which reveals that approximately 75% of the close contacts correspond to relatively weak interactions. The application of both concepts has provided a new insight into the relationship between the molecular interactions and crystal structures of the hydantoin derivatives.This is the peer-reviewed version of the following article: Crystengcomm, 2017, 19, 3, 469-483 [https://dx.doi.org/10.1039/C6CE02210C][http://cer.ihtm.bg.ac.rs/handle/123456789/2204

Complexes of d-block elements with aromatic o,o- and n,n-donor ligands: synthesis, structure, properties and applications

Reakcijom izmene liganada različitim metodama sinteze dobijeno je 22 ternarna kompleksa elemenata d-bloka [Mn(II), Co(II), Ni(II), Cu(II) i Zn(II)] sa anjonima aromatičnih polikarboksilnih kiselina (ftalne, izoftalne, tereftalne i piromelitne) kao O,O-donorskim ligandima i aromatičnim N,N-donorskim ligandima kao što su 2,2'-dipiridilamin i 2,2'-bipirimidin. Trinaest kompleksa sintetisano je u monokristalnom obliku, dok su ostala jedinjenja mikrokristalna. Prema vrsti centralnog atoma, u obliku monokristala dobijeno je pet Mn(II)-, dva Co(II)-, jedan Ni(II)-, dva Cu(II)-, dva Zn(II)-kompleksa, kao i bimetalni Mn(II)–Cu(II)-kompleks...A series of 22 d-block element complexes [Mn(II), Co(II), Ni(II), Cu(II) and Zn(II)] containing anions of aromatic polycarboxylate acids (phthalic, isophthalic, terephthalic and pyromellic) as O,O-donor ligands and aromatic N,N-donor ligands such as 2,2'-dipyridylamine and 2,2'-bipyrimidine, has been obtained by ligand exchange reaction using different synthetic methods. Thirteen complexes were obtained as single crystals, while the others were microcrystalline powders. According to the type of central atom, five Mn(II), two Co(II), one Ni(II), two Cu(II), two Zn(II) complexes, and bimetallic Mn(II)–Cu(II) complex were synthesized in form of single crystals. The structures of these compounds were determined by single-crystal X-ray analysis. Structural properties of complexes were discussed in detail and compared..

Zinc oxide nanoparticles prepared by thermal decomposition of zinc benzenepolycarboxylato precursors: Photoluminescent, photocatalytic and antimicrobial properties

Zinc oxide (ZnO) nanoparticles were obtained by thermal decomposition of one-dimensional zinc-benzenepolycarboxylato complexes as single-sourceprecursors at 450 degrees C in an air atmosphere. The mechanism and kinetics of thermal degradation of zinc-benzenepolycarboxylato complexes were analyzed under non-isothermal conditions in an air atmosphere. The results of X-ray powder diffraction and field emission scanning electron microscopy revealed hexagonal wurtzite structure of ZnO with an average crystallite size in the range of 39-47 nm and similar morphology. The band gap and the specific surface area of ZnO nanoparticles were determined using UV-Vis diffuse reflectance spectroscopy and the Brunauer, Emmett and Teller method, respectively. The photoluminescent, photocatalytic and antimicrobial properties of the ZnO nanoparticles were also examined. The best photocatalytic activity in the degradation of C. I. Reactive Orange 16 dye was observed for the ZnO powder where the crystallites form the smallest agglomerates. All ZnO nanoparticles showed excellent inhibitory effect against Gram-positive bacterium Staphylococcus aureus and Gram-negative bacterium Escherichia coli

Corrosion resistance of welded joints of X5CrNi18-10 stainless steel

This paper considers the influence of nitrogen in the shielding gas during TIG welding as well as the influence of a welding current level on the resistance to pitting corrosion and intergranular corrosion in welded joints of X5CrNi18-10 stainless steel. Testing of pitting corrosion was carried out using the potentiodynamic method, while intergranular corrosion was tested with the Double-Loop Electrochemical Potentiokinetic Reactivation method. Pitting corrosion resistance of welded joints (the weld metal and the heat affected zone) is higher in the presence of nitrogen in the shielding gas, while integranular corrosion resistance remains unchanged. Pitting corrosion resistance of the heat affected zone in the welded joint formed in nitrogen-free shielding gas is lower than in the base metal, while the weld metal has similar pitting corrosion resistance as the base metal. With an increase in a welding current level, pitting corrosion resistance and resistance to intergranular corrosion of welded joints decrease. The passivation current density is shown to be a good indicator of pitting corrosion resistance of welded joints. Hardness values of the weld metal and the heat affected zone are slightly lower than the base metal hardness value

The influence of the structure on the antiproliferative activity of the cycloalkanespiro-5-hydantoin derivatives

U okviru proučavanja uticaja strukture na biološku aktivnost derivata cikloalkanspiro-5-hidantoina, u radu je testirana citotoksičnost novih serija jedinjenja: 3-(4-supstituisanih benzil)-1,3- -diazaspiro[4.5]dekan-2,4-diona i 3-(4-supstituisanih benzil)-1,3-diazaspiro[4.6] undekan-2,4- diona. Citotoksična aktivnost određena je MTT testom prema ćelijskoj liniji humanog karcinoma dojke (MDA-MB-231). Strukturne karakteristike jedinjenja su određene rendgenskom strukturnom analizom kao i odgovarajućim spektroskopskim metodama. Testirana jedinjenja su pokazala statistički značajnu antiproliferativnu aktivnost prema ćelijskoj liniji MDA-MB-231 u proučavanom opsegu koncentracija. Naročito su se istakli derivati koji u okviru svoje strukture sadrže kao supstituente atome halogena i nitro-grupu. Rezultati su upoređeni sa prethodno određenom antiproliferativnom aktivnošću za 3-(4-supstituisane benzil)-5,5-difenilhidantoine. Diskutovan je uticaj strukture na antiproliferativnu aktivnost proučavanih jedinjenja.In order to investigate the influence of the structure on the antiproliferative activity of the cycloalkanespiro-5-hydantoine derivatives, the cytotoxity of the new series of compounds: 3-(4- substituted benzyl)-1,3-diazaspiro[4.5]decane-2,4-dione and 3-(4-substituted benzyl)-1,3- -diazaspiro[4.6]undecane-2,4-dione has been tested. Cytotoxic activity was determined by the MTT assay againist the cell line of human breast cancer (MDA-MB-231). The structural characteristics of the compounds are determined by X-ray structural analysis, as well as by appropriate spectroscopic methods. The tested compounds showed statistically significant antiproliferative activity to the MDA-MB-231 cell line in the studied concentration range. Among the most active are derivatives containing as substituents halogen atoms and a nitro group. The results were compared with a predetermined antiproliferative activity for 3-(4-substituted benzil)-5,5- -diphenylhydantoines. The influence of structure on the antiproliferative activity of the studied compounds is also discussed

Supramolecular architectures of selected xanthenedione derivatives

The wide range of pharmacological activities (e.g. antiviral, antifungal, antibacterical, antiinflamatory, leishmanicidal and antidepresant) has already been attributed to the xanthenediones, a group of synthetic heterocyclic compounds possessing a pyran nucleus fused on either side with cyclohex-2-enone rings [1]. In this work, two 3,3,6,6- tetramethyl-9-substituted-3,4,5,6,7,9-hexahydro-1H-xanthene-1,8(2H)-diones (Figure 1) were synthesized and their crystal stuctures were determined by single crystal X-ray diffraction. The main structural feature in compound 1 is a supramolecular chain along the a-axis formed by O4–H4···O2 hydrogen bond and C13–H13···O4 and Br1···Br2 interactions between the adjacent asymmetric units, while the formation of supramolecular network is further achieved by C–H···π interactions between the adjacent chains. The main motif in 2 is a dimer formed via O4–H4···O2 hydrogen bond and Cl1···π interactions. The neighbouring dimers are connected through strong C7– H7A···π interactions, thus resulting in formation of a zigzag chain parallel to the c-axis. Weak C–H···π interactions link the adjacent chains into a supramolecular layer. This work may provide a basis for design of new biologically active xanthenediones both at the molecular and supramolecular level

Decomposition mechanism and kinetics of zinc–isophthalate complex with 2,2’-dipyridylamine as a precursor for obtaining nanosized zinc oxide

Studies related to the synthesis of nanosized ZnO as the antibacterial agent have become an interdisciplinary area gathering chemists, physicists, biologists, and medics. The broad scope of materials based on ZnO resulted in the development of various techniques for its preparation. Considering the dependence of particle shape and size onto physical and chemical properties of ZnO, the synthesis procedure is of major importance. In this work, an unconventional methodology of synthesis is proposed for obtaining nanosized ZnO. Polymeric zinc complex containing 2,2’-dipyridylamine (dipya) and dianion of 1,3-benzenedicarboxylic acid (ipht), [Zn(dipya)(ipht)]n, was used as precursor. Besides the crystal structure of [Zn(dipya)(ipht)]n which was already published [1], the luminescent properties are presented in this work. Also, the amazing antibacterial activity of this precursor prompted us to investigate the relationship between the crystal structure and thermal properties, especially if we bear in mind the lack of similar studies in the literature. Therefore, the mechanism and kinetics of its degradation was investigated under nonisothermal conditions in nitrogen and air atmospheres. Degradation enthalpies, thermodynamic activation parameters, pre-exponential factor, A, and the apparent activation energy, Ea, were determined for each step using Kissinger’s and Ozawa’s equations. The complexity of degradation steps has been analyzed using isoconversional methods. TG/DCS data were collected at four different heating rates: 10, 15, 20 and 25 ºC min –1 , while the formation of nanosized ZnO was confirmed using XRPD and FESEM techniques. The influence of precursor on the crystallite size and morphology of the resulting ZnO along with its antibacterial activity was examined. The obtained results will be discussed and compared