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

Manganese-pyromellitate complex as a precursor for preparation of spinel Mn3O4

In recent years, thermal decomposition studies of transition metal complexes with benzenepolycarboxylate ligands have become an area of a great importance due to the possibility of obtaining useful metal oxides with desirable electrical, magnetic and catalytic properties [1]. As a contrast to conventional methods for the preparation of metal oxides, such as hydrothermal or sol– gel treatment, thermolysis is faster, more efficient and environmentally friendly. Mn(II)–dipya (dipya = 2,2’-dipyridylamine) complex with tetraanion of 1,2,4,5-benzenetetracarboxylic (pyromellitic, H4pyr) acid, [Mn2(dipya)2(pyr)(H2O)2], has been prepared and characterized by elemental, spectral and microscopy analyses. Direct thermolysis of the complex up to 1200 °C in an air atmosphere yielded spinel Mn3O4 oxide material. The obtained Mn3O4 has been characterized for its structural, spectroscopic, morphological and optical properties. The possibilities of using this oxide as photocatalyst or co-photocatalyst for removing textile organic dyes, as well as inorganic pigmentary material, were also investigated and discussed

Raw kaolinitic–illitic clays as high‑mechanical‑performance hydraulically pressed refractories

The usage possibility of 19 composites of raw refractory clays from Serbia containing approximately 53.29% of SiO2 and 26.73% of Al2O3 is presented. The sum of fluxing oxides was 57.74%, while these materials contained 32% of quartz, 29% of kaolinite and 26% of illite–mica. Dilatometry tests revealed a sudden shrinkage with the peak at approximately 1115 °C, owing to the formation of mullite. The refractoriness was in the range of 1581–1718 °C, which classifies the composites from low- to high-duty refractories. Based on correlation analysis, the refractoriness mostly depended on the content of alumina. The lightness of the fired test pieces was lower after firing when compared to the dry samples, and it decreased with the firing temperature from reddish to grayish. The study presents a novel attempt to define all the necessary properties of raw refractory clays and products fired at the 1100–1300 °C range on a laboratory level. Most of these clays can be used as natural refractory materials for ceramic and glass furnace lining. The organic matter in some of the samples influences negatively the fast-firing process

Structure and properties of ZnO/ZnMn2O4 composite obtained by thermal decomposition of terephthalate precursor

A biphasic [Mn(dipya)(H2O)4](tpht)/{[Zn(dipya)(tpht)]·H2O}n complex material, I, (dipya = 2,2’-dipyridylamine, tpht2– = dianion of terephthalatic acid) was synthesized by ligand exchange reaction and characterized by XRPD and FTIR spectroscopy. A ZnO/ZnMn2O4 composite, II, has been prepared via thermal decomposition of precursor I in an air atmosphere at 450 °C. XRPD, FTIR and FESEM analyses of II revealed the simultaneous presence of spherical nanoparticles of wurtzite ZnO and elongated nanoparticles of spinel ZnMn2O4. The specific surface area of II was determined by the BET method, whereas the volume and average size of the mesopores were calculated in accordance with the BJH method. The measurements of the mean size, polydispersity index and zeta potential showed colloidal instability of II. Two band gap values of 2.4 and 3.3 eV were determined using UV–Vis diffuse reflectance spectroscopy, while the measurements of photoluminescence revealed that II is active in the blue region of the visible spectrum. Testing of composite II as a pigmentary material showed that it can be used for the colouring of a ceramic glaze

Structure and properties of ZnO/ZnMn2O4 composite obtained by thermal decomposition of terephthalate precursor: Scientific paper

A biphasic [Mn(dipya)(H2O)4](tpht)/{[Zn(dipya)(tpht)]·H2O}n com­plex material, I (dipya = 2,2’-dipyridylamine, tpht2– = dianion of terephthalatic acid) was synthesized by ligand exchange reaction and characterized by XRPD and FTIR spectroscopy. A ZnO/ZnMn2O4 composite, II, has been prepared via thermal decomposition of I in an air atmosphere at 450 °C. XRPD, FTIR and FESEM analyses of II revealed the simultaneous presence of spherical nano­particles of wurtzite ZnO and elongated nanoparticles of spinel ZnMn2O4. The specific surface area of II was determined by the BET method, whereas the volume and average size of the mesopores were calculated in accordance with the BJH method. The measurements of the mean size, polydispersity index and zeta potential showed colloidal instability of II. Two band gap values of 2.4 and 3.3 eV were determined using UV–Vis diffuse reflectance spectroscopy, while the measurements of photoluminescence revealed that II is active in the blue region of the visible spectrum. Testing of composite II as a pigmentary material showed that it can be used for the colouring of a ceramic glaze

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

Role of structural motifs in formation of the supramolecular architecture of 3-(4-tert-butylbenzoyl)-1,3-diazaspiro[4.5]Decane-2,4-dione

Proučavano jedinjenje (slika 1) sintetisano je polazeći od cikloheksanona Bučerer- Bergsovom reakcijom i naknadnim acilovanjem dobijenog spirohidantoina. Izgradnja kristalne strukture ovog jedinjenja proučavana je sa aspekta doprinosa jednostavnih dimernih motiva koji se uspostavljaju preko različitih intermolekulskih interakcija.Intermolekulske interakcije dodatno su proučavane pomoću Hiršfeldovih površina i 2D grafičkih prikaza otisaka interakcija. Kristalna struktura, naime, zadržava motiv koji se često sreće kod derivata hidantoina, u kome su dva inverzano orijentisana molekula povezana parom N–H···O vodoničnih veza. Ovaj motiv formira dva tipa dvostrukih lanaca, koji dalje grade sloj (slika 2). Osim toga, slabe C–H⋯O interakcije zajedno sa disperzionim interakcijama (π-π i hidrofobne interakcije) identifikovane su u ovoj kristalnoj strukturi. Kristalografski podaci: C19H24N2O3, Mr = 328,4, trikliničan sistem, prostorna grupa P–1, a = 6,2810(2), b = 12,0586(4), c = 12,1852(5) Å,α = 77,624(3), β = 81,039(3), γ = 79,111(3) °, V = 878.81(6) Å3, Z = 2, F(000) = 352, ρx = 1,380 g cm–3,µ(MoKα) = 0,084 mm–1. Utačnjavanje sa F2 (220 parametara) dalo je R1 = 0,0520, wR2 = 0,1199, S = 1,033 za sve podatke i R1 = 0,0443 za 3232 uočenih refleksija sa I ≥ 2σ(I).The title compound (Figure 1) was prepared from cyclohexanone in the Bucherer-Bergs reaction, followed by acylation of the obtained spirohydantoin. Formation of the crystal structure of this compound was analysed in terms of a number of simple dimeric motifs which are associated with different intermolecular interactions. The crystal structure retains the motif commonly found in hydantoin derivatives, where two molecules related by inversion are linked by a pair of N–H O hydrogen bonds. This motif is involved in two types of double chains, whichfurther form a layer (Figure 2). Intermolecular interactions were also investigated using Hirshfeld surface analysis and 2D fingerprint analysis. Weak C–H⋯O interactions together with thedispersion interactions (π-π and hydrophobic) as the source of attraction are identified in this crystal structure.Crystal data: C19H24N2O3, Mr = 328.4, triclinic system, space group P–1, a = 6.2810(2), b = 12.0586(4), c = 12.1852(5) Å, a = 77.624(3), β = 81.039(3), γ = 79.111(3) °, V = 878.81(6) Å3, Z = 2, F(000) = 352,ρx = 1.380 g cm–3, µ(MoKa) == 0.084 mm–1. The refinement on F2 (220 parameters) yielded R1 = 0.0520, wR2 = 0.1199,S = 1.033 for all data, and R1 = 0.0443 for 3232 observed reflections with I ≥ 2σ(I)