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1
Content available Nowe spojrzenie na krystalochemię nukleotydów
EN
Nucleotides play a fundamental role in the functioning of all living systems. They constitute the building blocks of nucleic acids (DNA and RNA), regulate metabolic pathways, energy transfer, and signal transduction, and serve as essential components of many antiviral and anticancer drugs as well as food additives. Structural investigations in both the solid state and in solution have provided significant insights into the characteristic features of nucleotides. However, certain crystalline systems – including potassium salts, cyclic nucleotides, and anhydrous forms – remain poorly characterized. This study presents examples of structural research of nucleotides in these less-explored areas, demonstrating the application of post-crystallization dehydration as a method for obtaining crystals with novel architectures, conformations, and structural motifs, such as unique intermolecular interactions and metal-ion coordination patterns, which cannot be achieved through typical solution crystallization.
2
EN
The publication presents the structure, chemical properties, and potential applications of 4-hydroxypyridine-2,6-dicarboxylic acid named as chelidamic acid. This organic heterocyclic compound belongs to a class of materials that is becoming increasingly significant in the fields of coordination chemistry, pharmacology, and energy storage technologies. The presence of a hydroxyl group and two carboxylic groups enables this acid to undergo stepwise deprotonation and participate in numerous coordination reactions as a multidentate ligand. The paper provides a detailed presentation of the acid’s protonation behavior and tautomerism, as well as crystallographic data on its various forms. A part of the publication is devoted to the practical applications of chelidamic acid. Its effectiveness as a component of composite electrodes in lithium-ion batteries has been demonstrated. The paper also discusses its role as a ligand in sensors for detecting heavy metals (e.g., Cd2+), as a complexing agent in ion chromatography, and as a component in functional catalytic materials (e.g., in copper-free Sonogashira reactions). In discussing coordination compounds with metal ions, the authors highlight the diversity of coordination modes that chelidamic acid can adopt. These include tridentate and bridging modes in compounds containing d-block, lanthanide, p-block and s-block metal ions. Special attention is given to the presence of tautomeric forms (enol and keto) in crystalline structures and how these forms influence the geometry and types of interactions in metal-organic compounds. This comprehensive study combines structural and application-related aspects to identify chelidamic acid as a compound with significant potential for use in modern functional materials, energy storage systems, and selective chemical sensors.
EN
Acridines constitute an interesting class of compounds with significant pharmaceutical relevance. They have been used in the treatment of various diseases, including bacterial and viral infections, cancer, and neurological disorders. This article discusses the structures and properties of the most pharmaceutically important aminoacridines, along with a review of their crystal structures deposited in the Cambridge Structural Database (CSD). The review may support the design of new multicomponent crystal systems with pharmaceutical potential derived from this group of compounds.
PL
Wyznaczono odniesioną do warunków pożaru nośność specyfikowaną ze względu na wyboczenie giętne i identyfikowaną dla odpowiadających sobie słupów o identycznej geometrii i sposobie podparcia, wykonanych z różnych gatunków stali nierdzewnych, o zróżnicowanej strukturze materiału. W celach porównawczych uzyskane wyniki odniesiono do analogicznej nośności tych samych słupów, projektowanych tym razem z wybranych gatunków niestopowych stali konstrukcyjnych, kojarzonych z rozpatrywanymi wcześniej stalami nierdzewnymi z uwagi na zbliżoną wytrzymałość. Pokazano, że struktura stali nierdzewnej determinuje jej odporność ogniową. Na ogół jednak jest to odporność znacząco większa niż ta, która charakteryzuje typowe konstrukcyjne stale niestopowe.
EN
The load-bearing capacity specified for flexural buckling and related to fire conditions was precisely determined. It was identified for corresponding columns with identical geometry and support method, made of stainless steels of various types, with differentiated crystal structures. For comparative purposes, the obtained results were referred to the analogous load-bearing capacity of the same columns, designed this time from non-alloy structural steels of selected types, associated with the previously considered stainless steels due to their similar strength. It was shown that the internal structure of a stainless steel determines its fire resistance. In general, however, this resistance is significantly higher in relation to that which characterizes the typical non-alloy structural steels.
PL
Celem niniejszego artykułu był opis możliwości badań materiałów krystalicznych i amorficznych oraz metod wytwarzania przy zastosowaniu aparatury znajdującej się na wyposażeniu Katedry Fizyki. Występujące różnice, a także podobieństwa przedstawiono na podstawie metod wytwarzania materiałów, a także przeprowadzonych badań z użyciem dyfraktometru rentgenowskiego (XRD) i magnetometru wibracyjnego (VSM).
EN
The aim of this article was to describe the possibilities of testing crystalline and amorphous materials, as well as production methods, using the equipment at the Department of Physics. Differences, as well as similarities, are presented on the basis of the materials' manufacturing methods and the tests carried out using an X-ray diffractometer (XRD) and a vibrating magnetometer (VSM).
EN
This study synthesized nano-sized TiO2 using scrap from the TiN thin film manufacturing process by a hydrothermal reaction. By controlling the reaction temperature and concentration, the crystal structure and particle size were controlled. The solution from the TiN scrap was strongly acidic with a pH below 0. The mixed TiO2 of rutile and anatase crystal structures was produced at a concentration of 0.08 mole. The TiO2 particle size ranged from 4 nm to 8 nm, increased from 7 nm to 140 nm after heat treatment. At temperatures above 800°C, the crystal structure of the mixed TiO2 transformed into pure rutile.
EN
The elaboration contains the history of the development of coordination chemistry at the Maria Curie-Skłodowska University in Lublin. The Department of General and Coordination Chemistry and Crystallography at the Institute of Chemical Sciences, Faculty of Chemistry, Maria Curie-Skodowska University conducts research on metal complexes. Coordination chemistry in Lublin is inextricably associated with Professor Wanda Brzyska, who in the mid-1950s began her scientific career at the Department of Inorganic Chemistry headed by Professor Włodzimierz Hubicki. Professor Brzyska moved away from teamics related to the separation processes of rare earth elements, focusing mainly on the synthesis and characterization of coordination compounds in the solid phase, based on rare earth elements and carboxylic acids. The study presents the development of research topics over the years in the area of coordination chemistry, the evolution of methods, and the research equipment used.
EN
Purpose: The purpose of this work is to study the effect of sintering modes, especially the sintering temperature, on the crystal lattice parameters and the morphology of the ZrO2–nY2O3 (n = 3–8 mol%) ceramic microstructure components in relation to corresponding fracture micromechanisms. Design/methodology/approach: The series of ZrO2–nY2O3 (n = 3–8 mol%) ceramics were sintered in an argon atmosphere at temperatures 1450°C, 1500°C, 1550°C, and 1600°C. The cross-sectional surfaces of samples were prepared for microstructure analysis using a grinding and polishing Struers Tegramin machine. Young’s ceramics modulus values were determined using an ultrasonic flaw detector Panametrics EPOCH III 2300. The samples’ density and porosity were determined by the Archimedes’ method. Scanning electron microscopes Hitachi SU3900 and Carl Zeiss EVO-40XVP were used to analyse the microstructure and fracture surface morphology of samples. For estimating chemical compositions in an energy-dispersive X-ray spectroscopy mode, an INCA ENERGY 350 spectrometer was utilized. Microhardness measurement was performed on a NOVOTEST TC-MKB1 microhardness tester. The fracture toughness of the material was estimated using a single-edge notch beam (SENB) test and the Vickers indentation test. Both the flexural strength and SENB tests were performed under three-point bending using a UIT STM 050 test machine. All mechanical tests were carried out in air at a temperature of 20°C. Findings: Optimal sintering modes for a variety of YSZ ceramic compositions are found, taking into account the combined effect of the sintering temperature and a percentage of Y2O3, which resulted in a specified balance of cubic, tetragonal, and monoclinic zirconia phases, an optimal microstructure features, and the implementation of high-energy fracture micromechanisms responsible for high strength and fracture toughness of YSZ ceramics. Research limitations/implications: To study the behaviour of YSZ ceramics in the operating atmosphere, their microhardness, flexural strength, and fracture toughness should be evaluated under the operating temperature and pressure conditions. Practical implications: Based on the research performed, it is possible to design the microstructure of YSZ ceramic with the necessary physical and mechanical properties to provide high reliability of ceramic products in various industry branches. Originality/value: The balance of cubic, tetragonal, and monoclinic zirconia phases, as well as the crystal lattice parameters change, was determined for YSZ ceramics stabilized with the various amounts of yttria, and it was linked to their mechanical behaviour; the Vickers indentation method and SENB method were used to estimate crack growth resistance of YSZ ceramics, and an appropriate fracture micromechanism was found.
EN
The new three-dimensional coordination polymer termed {[Na2SDC(H2O)]} n (SDC2-= C16H10O42-) has been synthesized using workstation Easymax 102 while controlling the conditions and monitoring in-situ reagents. The metal complex was obtained in the reaction of sodium hydroxide with a suspension of 4,4’-stilbenedicarboxylic acid in aqueous medium. The compound was characterized by elemental analysis, single crystal, and powder X-ray diffraction methods, ATR-FTIR spectroscopy, SEM and optical microscopy, TG-DSC and TG-FTIR thermal analysis in air and nitrogen atmosphere. In the crystal structure of {[Na2SDC(H2O)]} n appears penta- and hexacoordinated sodium atoms joined by octa- and decadentate SDC2- linkers. Aqua ligand acts as bridge between Na1 and Na2 atoms. The as-synthesized sodium complex is thermally stable up to 86°C whereas its dehydrated form has extreme stability up to 491°C. Removal of water molecule leads to the crystal-to-crystal transformation yielded changes in coordination modes of COO groups. Reversibility of the hydration process in the studied complex was also examined.
EN
Modification of bentonite by the Al/Fe metal oxide pillarization process was carried out with metal oxides. The bentonite pillars were successfully characterized using an X-Ray Diffraction (XRD) spectrophotometer. The results of XRD characterization showed the peak diffraction angle (2θ) in metal-pillared bentonite was 26.84° at 698.98 cps. Meanwhile, in thermally and chemically activated bentonite, the peak angles were marked at 20.64° and 26.7°. There is a shift in the peak angle after activation and pillarization. XRD patterns showed dioctahedral smectite and quartz accessory minerals.
EN
Four macroscopically visible B–E (rim) zones of the natural grossular-andradite garnet with Grs58-64subAdr36-42>Sps2composition were crystallographically studied. The applied procedure includes the Rietveld refinements of the crystal structures in a series of six space groups, which were followed by the comparative analysis of the R-values, site occupancy factors, and the bond lengths and angles. It was established that it crystallized in the rhombohedral R-3c space group. Various polyhedral distortions and structural order-disorder variations between the studied zones were also observed, determined and discussed. Therefore, rhombohedral symmetry of the studied grandite could be treated as primary and residual strain as the second cause for its slight optical anisotropy.
12
Content available Kwas hypodifosforowy i jego sole nieorganiczne
EN
Hypodiphosphoric acid is the lower oxoacid of phosphorus of H4P2O6 composition. It contains the direct P—P bond, in contrast to its closest analog - pyrophosphoric acid, H4P2O7. In comparison to other phosphates the knowledge on hypodiphosphoric acid and its inorganic salts is quite limited. Since its discovery almost 150 years ago, establishment of the proper molecular and structural formula of the acid has initiated intensive research and dispute in the literature, which was decisively ended in 1964, when the first complete X-ray crystal structure determination of diammonium hypodiphosphate was reported. Since then structural studies have led to the discovery of ferroelectric properties in the above-mentioned diammonium salt and dehydration-induced staggerer-eclipsed transformation of hypodiphosphate in tetrabutylammonium salt, experimental electron density distribution determination in cubic tetralithium hexahydrate and last but not least crystal structure elucidation of hypodiphosphate analogs of adenosine diphosphate. In this mini-review the information on synthesis techniques, chemical and physical properties, applications of hypodiphosphates along with crystallochemical description of reported up-to-date crystal structures are presented.
EN
Quartz and feldspar are usually exist in symbiosis in nature, and they are difficult to be separated effectively by conventional physical methods owing to their similarities in crystal structures and surface characteristics. Flotation is the most resultful method, and especially, flotation with hydrofluoric acid (HF) is the most efficient way. Because HF may cause serious environmental and health problems, the effective and environmentally friendly separation of quartz and feldspar remains a formidable challenge. The crystal structure, surface broken bonds, surface energy, and solid–liquid interface properties of quartz and feldspar are investigated in this paper. In particular, some types of mixed cationic/anion collectors and their interaction mechanism on the quartz and feldspar surfaces with acidic, alkaline, and neutral media in the absence of fluorine are discussed, and the grade and scheme of quartz and feldspar for the practical application are illustrated. This review proposes concrete research approaches and provides perspectives for the advanced processing of quartz and feldspar in an environmentally friendly and economical way.
EN
The purpose of this work was to determine whether the structures of ordered part of novel poly(3,4-ethylenedioxythiophene) PEDOT : OTf (doped with trifluoromethanesulfonate anions) and PEDOT : HSulf (doped with hydrogensulfate anions) systems could really be simply the layered structure of PEDOT : Tos (doped with tosylate anions) with the counter ion changed to the appropriate one. Insight into this problem could be provided by molecular dynamics simulations but also by swarm intelligence optimization, developed earlier for the purpose of investigating the other structures.
PL
Zbadano zdolność struktury uporządkowanej części nowych układów domieszkowanych poli(3,4-etylenodioksytiofenu) (PEDOT) [PEDOT : OTf (domieszkowane anionami trifluorometanosulfonianowymi) i PEDOT : HSulf (domieszkowane anionami wodorosiarczanowymi)] do powielania znanej z literatury warstwowej struktury PEDOT : Tos (domieszkowane anionami tosylanowymi) z jonem domieszki zmienionym na odpowiedni. Poszukiwania nowych struktur wspomagano symulacjami dynamiki molekularnej, a także z zastosowaniem optymalizacji opartej na algorytmach inteligencji stadnej.
EN
Single crystals of L-Valinium Picrate (LVP), 0.1 mol% Ni2+ doped L-Valinium Picrate, and 0.2 mol% Ni 2+ doped L-Valinium Picrate were grown by low temperature solution growth method, especially by solvent evaporation technique at ambient temperature. Function groups and modes of vibration were identified by FT-IR studies. The grown crystals belong to monoclinic system which has been revealed by powder XRD. The estimated band gaps were found to be 3.86 eV for LVP, 3.72 eV for 0.1 mol% Ni2+ doped LVP, and 3.70 eV for 0.2 mol% Ni2+ doped LVP crystals, respectively. The PL excitation wavelength of the grown materials is 370 nm. All the elements (C, N, O, Ni, and Cl) as per molecular formula were present in the EDAX spectrum of the grown materials. The 0.2 mol% Ni2+ ion doped LVP materials had higher thermal stability (208 °C) than LVP and 0.1 mol% Ni2+ doped LVP.
EN
Goal of the present research was to apply a solid state reaction route to fabricate bismuth layer-structured multiferroic ceramics described with the formula Bi5FeTi3O15 and reveal the influence of processing conditions on its crystal structure and phase composition. Simple oxide powders Bi2O3, TiO2 and Fe2O3 were used to fabricate Aurivillius-type bismuth layer-structured ferroelectrics. Pressureless sintering in ambient air was employed and the sintering temperature was TS = 900°C, TS = 1000°C and TS = 1040°C. The phase composition as well as crystal structure of ceramics sintered at various processing conditions was examined with powder X-ray diffraction method at room temperature. The Rietveld refinement method was applied for analysis of X-ray diffraction data. It was found that ceramics adopted orthorhombic structure Cmc21. The unit cell parameters of bismuth layer-structured multiferroic ceramics increased slightly with an increase in sintering temperature.
EN
In the present study, the dopant effect of Zn on the crystal structure, thermal properties and morphology of magnesium aluminate (MgAl2O4) spinel (MAS) structure was investigated. A pure and two Zn-containing MASs (e.g. MgAl1.93Zn0.07O and MgAl1.86Zn0.14O) were synthesized for this purpose via a wet chemical method, and the as-prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, differential thermal analysis (DTA), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy techniques. It was found that the crystal structure, thermal properties and morphology of the MAS system change with the increase in the amount of Zn. MgO phase formation was observed. The values of the lattice parameter, unit cell volume and crystallite size increased, and the crystallinity percentage decreased. The morphology was also affected by adding of Zn.
EN
Nonlinear optical single crystals of L-histidine nitrate (LHN) as well as 0.05 mol % Y2+ doped LHN and 0.10 mol % Y2+ doped LHN were successfully grown by slow evaporation technique at room temperature. The lower cutoff wavelength and transmittance were 339 nm, 343 nm, 347 nm and 84 %, 86 % and 87 % for LHN, 0.05 mol % and 0.10 mol % yttrium doped LHN, respectively. Powder XRD studies revealed that the grown materials belong to an orthorhombic system with the space group P212121. FT-IR peak at 534 cm−1 due to yttrium coordinated with oxygen was observed. The EDAX analysis confirmed the presence of such elements as C, N, O and Y in the grown materials. High intensity PL emission peak was obtained at 420 nm.
EN
Nanostructured CdO thin films have been prepared on glass substrates by spray pyrolysis technique using perfume atomizer from fresh and aged (1, 2, 3 and 4 days) precursor solutions. XRD studies confirm that all the films exhibit cubic crystal structure with a (1 1 1) preferential orientation. The preferential orientation factor f(1 1 1) increases with an increase in aging the period of precursor solution. The 2θ value of the (1 1 1) plane shifts towards lower Bragg angles with aging inferring an expansion in the lattice volume of the aged films. Increased crystallite size is observed for the 3-days aged film for which minimum strain and dislocation density values are obtained. Optical transparency increases with an increase in aging period of the precursor solution and the optical band gap exhibits a red shift from 2.48 eV to 2.32 eV. Minimum resistivity of 0.78 × 10−2 Ω·cm is observed for the CdO film prepared from 3-days aged solution. The obtained results infer that the CdO film prepared from 3-days aged solution exhibits better physical properties than the others.
EN
We present the results of the stabilization of the γ-U phase with a cubic structure in U-T alloys by means of combined ultrafast cooling (with a cooling rate 106 K/s) and doping with alloying elements in the VI and VIII group (T = Mo, Pt, Nb, Ru, Ti). The X-ray diffraction data have confirmed the cubic structure presented in all U-T alloys with the alloying element content T≥15 at.% (atomic percentage concentration). Some results of the microstructure analysis, phase distribution and orientation of selected samples by using electron backscatter diffraction are also shown.
PL
Zaprezentowaliśmy wyniki stabilizacji fazy γ-U ze strukturą kubiczną w związkach U-T za pomocą techniki ultraszybkiego chłodzenia (z szybkością chłodzenia 106 K/s) oraz domieszkowania pierwiastkami z grup VI i VIII (T= Mo, Pt, Nb, Ru, Ti). Dane dyfrakcji rentgenowskiej potwierdziły obecność kubicznej struktury we wszystkich związkach U-T posiadających zwartość pierwiastków domieszkujących T≥15 at.% (procent atomowy). Wyniki analizy mikrostruktury, rozkładu fazowego i orientacji wybranych próbek zostały również pokazane, używając dyfrakcji wstecznego rozpraszania elektronów.
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