Synthesis, in vitro and docking studies of 2-substituted 5,6,7,8-tetrahydrobenzo[4,5]thieno[2,3-d]pyrimidine-4(3H)-one derivatives as agents for the treatment of Alzheimer's disease Chimica Techno Acta ARTICLE published by Ural Federal University 2022, vol. 9(2), No. 20229205 eISSN 2411-1414; chimicatechnoacta.ru DOI: 10.15826/chimtech.2022.9.2.05 1 of 5 Synthesis and luminescent properties of new double Ln2Zr(WO4)5 (Ln = Tb, Dy) tungstates Bair Bazarov a,b* , Sesegma G. Dorzhieva a , Roman Yu. Shendrik c,d , Yunna L. Tushinova a,b , Tsirendyzhit T. Bazarova a , Dmitriy O. Sofich c , Olga D. Chimitova a , Jibzema G. Bazarova a a: Baikal Institute of Nature Management SB RAS, Ulan-Ude 670047, Russia b: Department of Inorganic and Organic Chemistry, Buryat State University, Ulan-Ude 670000, Russia c: A.P. Vinogradov Institute of Geochemistry SB RAS, Irkutsk 664033, Russia d: Irkutsk State University, Irkutsk 664033, Russia * Corresponding author: info@binm.ru; bazbg@rambler.ru This paper belongs to a Regular Issue. © 2021, the Authors. This article is published open access under the terms and conditions of the Creative Commons Attribution (CC BY) license (http://creativecommons.org/licenses/by/4.0/). Abstract New polycrystalline powder samples of double Ln2Zr(WO4)5 (Ln = Dy, Tb) tungstates were synthesized using high-temperature solid-phase and sol-gel methods. The conditions of the sol-gel syn- thesis of tungstates were optimized. The obtained phases were char- acterized by the X-ray powder diffraction on the basis of the crystal- lographic data of similar Ln–Zr molybdates. It is found that Ln2Zr(WO4)5 (Ln = Dy, Tb) double tungstates crystallize in the ortho- rhombic crystal system, space group Cmc21 (Z = 4). The intensive luminescence in the green spectral region for Tb2Zr(WO4)5 and yel- low spectral region for Dy2Zr(WO4)5 was shown. Keywords solid-phase synthesis sol-gel technique framework structure luminescence tungstates lanthanides Received: 08.11.21 Revised: 19.04.22 Accepted: 26.04.22 Available online: 03.05.22 1. Introduction The search and synthesis of new compounds are associat- ed with the study of multicomponent systems. In terms of the formation of promising compounds, molybdate and tungstate systems are of great interest [1–19]. Complex oxide compounds containing REE and elements of the IV B subgroup (Ti, Zr, Hf) are the objects of intensive research in connection with the search of new materials used as solid-state electrolytes, phosphors and matrices for immo- bilizing radioactive waste. Previously, we studied interac- tions in the ternary oxide systems in the subsolidus region by the intersecting cuts method and established the for- mation of three types of compounds with following formu- las: Ln2Zr3(MoO4)9 (1:3) (Ln = La–Tb), Ln2Zr2(MoO4)7 (1:2) (Ln = Sm–Dy), Ln2Zr(MoO4)5 (1:1) (Ln = Tb–Lu) [20–22]. The crystal structures for the double molybdate represent- atives were also studied [23]. This work was devoted to synthesis and luminescent characteristics of double tung- states Ln2Zr(WO4)5 (Ln = Tb, Dy) obtained by a solid- phase synthesis and sol-gel methods. It was established that the tungstate phases are isostructural to the molyb- denum analogues. 2. Experimental New Ln2Zr(WO4)5 (Ln = Tb, Dy) tungstates were obtained by the solid-phase reaction and sol-gel technique. For sol- id-phase synthesis, Ln2O3 (99.9% purity), ZrO2 obtained by calcining ZrO(NO3)22H2O (analytical grade), WO3 (ana- lytical grade) were used as starting reagents. The initial oxides, preliminary calcined at T=200 °C, were thoroughly mixed in appropriate ratios. The samples were annealed in porcelain crucibles in air in a muffle furnace. The initial annealing temperature was 450 °C. The final synthesis temperature was varied in the range of 750–800 °C with 50 h dwell time. In the course of synthesis, the samples were repeatedly ground in an agate mortar in ethanol. The phases were identified by X-ray phase analysis using a D8 Advance Bruker diffractometer. Also, double tungstates Ln2Zr(WO4)5 (Ln = Tb, Dy) were synthesized by the Pechini method, where ethylene glycol is completely replaced by water, there by reducing the amount of organic compounds. The second difference is the formation of an amorphous gel-like substance in- stead of a polymer. As a complexing agent, as in the Pechini method, an aqueous solution of citric acid (C6H8O7H2O) was used. http://chimicatechnoacta.ru/ https://doi.org/10.15826/chimtech.2022.9.2.05 https://orcid.org/0000-0003-1712-6964 http://orcid.org/0000-0003-2071-1152 https://orcid.org/0000-0001-6810-8649 https://orcid.org/0000-0003-1032-8854 https://orcid.org/0000-0001-9697-6320 https://orcid.org/0000-0002-2836-3597 http://orcid.org/0000-0002-9381-8922 https://orcid.org/0000-0002-1231-0116 mailto:info@binm.ru mailto:bazbg@rambler.ru http://creativecommons.org/licenses/by/4.0/ https://crossmark.crossref.org/dialog/?doi=https://doi.org/10.15826/chimtech.2022.9.2.05&domain=pdf&date_stamp=2022-5-3 Chimica Techno Acta 2022, vol. 9(2), No. 20229205 ARTICLE 2 of 5 The excitation and emission spectra in the UV-IR range were measured using a MDR-2 laboratory monochromator and a SDL-1 dual monochromator. The absorption spectra were obtained using a Perkin-Elmer Lambda 950 UV/VIS/NIR spectrophotometer, operating in the range of 180–3000 nm with a maximum resolution of 0.2 nm. To measure the absorption spectra of powder samples to the device, a prefix was connected to the integrating sphere with a diameter of 150 mm. Powder was poured into a quartz ampoule and was fixed in the holder of the inte- grating sphere. The absorption of the test glass was sub- tracted from the absorption spectra. 3. Results and Discussion Ln2Zr(WO4)5 (Ln = Tb, Dy) double tungstates were ob- tained by ceramic and sol-gel methods. The conditions of the sol-gel technique for obtaining of Ln2Zr(WO4)5 (Ln = Tb, Dy) were optimized. The synthesis scheme is shown in Figure 1. Figure 1 Block diagram of the sol-gel technique for obtaining of Ln2Zr(WO4)5 (Ln = Tb, Dy) tungstates. According to the X-ray powder diffraction data, all compounds synthesized by two methods are isostructural. Crystallographic parameters of double tungstates was de- termined using the TOPAZ 4.2 program according to data of isostructural high-temperature phase of Er2Zr(MoO4)5 molybdate [24]. The results of refinement are shown in Table 1. Ln2Zr(WO4)5 (Ln = Tb, Dy) are crystallized in or- thorhombic crystal system, space group Cmc21 (Z = 4). The shape and intensity of the spectral lines indicate low symmetry of rare-earth ions coordination, which is in good agreement with the crystallographic data of molyb- dates. As an example, Figure 2 shows an X-ray diffraction pattern for Tb2Zr(WO4)5 obtained by the solid state reac- tion. Table 1 The refinement parameters for Ln2Zr(WO4)5 (Ln = Tb, Dy). The crystal structure of the studied tungstates can be represented by a three-dimensional mixed framework consisting of three polyhedra: WO4 tetrahedra, Ln(2)/ZrO6 octahedra and eight vertex polyhedra Ln(1)O8 connected to each other through common oxygen atoms (Figure 3). Ln and Zr atoms are distributed with equal probability over equivalent crystallographic positions. 2Th Degrees 100908070605040302010 C o u n ts 12 500 12 000 11 500 11 000 10 500 10 000 9 500 9 000 8 500 8 000 7 500 7 000 6 500 6 000 5 500 5 000 4 500 4 000 3 500 3 000 2 500 2 000 1 500 1 000 500 0 -500 -1 000 Structure 100.00 % Figure 2 Measured and calculated powder diffraction patterns for Tb2Zr(WO4)5 together with the difference curve (Cu Kα1 radiation). Empirical formula Tb2Zr(WO4)5 Dy2Zr(WO4)5 Formula weight, g/mol 1648.31 1655.46 Crystal system Orthorhombic Space group Cmc21 Cell parameters, Å a = 21.078(1) b = 9.6844(4) c = 9.8164(6) a = 21.177(1) b = 9.6737(7) c = 9.8176(8) Cell volume, Å3 2003.8(1) 2011.3(2) Z 4 Calc. density, g/sm3 4.061 4.047 Rwp, % 2.88 6.75 Rp, % 2.24 5.34 GOF 1.80 1.21 Chimica Techno Acta 2022, vol. 9(2), No. 20229205 ARTICLE 3 of 5 Figure 3 The structural model of Ln2Zr(WO4)5 (Ln = Tb, Dy), viewed along the b axis. Light-lilac tetrahedra are formed by W atoms, dark-grey octahedra by Ln(2)/Zr atoms and turquoise pol- yhedra by Ln(1)atoms. In the excitation spectra of the investigated tungstates Tb2Zr(WO4)5, two types of bands are observed – narrow, corresponding to transitions inside 4f shells of REE (rare earth elements) and broad bands associated with charge transfer bands in complexes WO42– on REE. The lumines- cence and excitation spectra of Tb2Zr(WO4)5 in the band with an energy of 26500 cm–1 (λ = 377 nm) are shown in Figure 4. The position of the bands associated with transi- tions inside the 4f shell remains almost unchanged in the molybdate and the tungstate. The vertical lines in Figure 4 represent the energies of corresponding terms according to Carnall [25]. Figure 4 Excitation (1) and luminescence (2) spectra of Tb2Zr(WO4)5 tungstate. Since Tb2Zr(WO4)5 is isostructural to the corresponding molybdate analogue Tb2Zr(MoO4)5 [26], all their spectra (luminescence, excitation) are similar. The luminescence spectra are characterized by the band with a highest inten- sity and maximum in the region of 18500 cm–1 (λ = 540 nm) associated with the 5D4–7F5 magnetic dipole transi- tion. The luminescence band with a maximum at 20500 cm–1 (λ = 488 nm) refers to the electric dipole transition 5D4–7F6 in a Tb3+ ion and depends on the symmetry of the crystal field; it is more intense than the other bands (ex- cept for 5D4–7F5) and splits into three types, which indi- cates a spatial distortion of the 8-vertex TbO8 polyhedra with a decrease in symmetry. The absorption spectra of Dy2Zr(WO4)5 (Figure 5) ex- hibit a number of bands corresponding to transitions from the ground term of the 4F15/2 and 4f- state to higher energy terms. The position of the bands associated with transi- tions inside the 4f shell remains almost unchanged in the molybdate and in the tungstate. Upon excitation by a laser with a wavelength of 404.5 nm, three emission bands with energies of 15100 cm–1, 17400 cm–1, and 20600 cm–1 are observed (Figure 6, curve 2), associated with transitions inside the Dy3+ ions. The most intense is the band with a maximum at 17400 cm–1, associated with the transition from the 4F9/2 term to the 6H13/2 term (yellow region of the spectrum), the luminescence band at 20600 cm–1 is associated with transitions from the 4F9/2 to 6H15/2 term (blue spectral re- gion), and the 15100 cm–1 band is associated with the 4F9/2–6H11/2 transition (red spectral region). Figure 5 Absorption spectrum of Dy2Zr(WO4)5. Figure 6 Excitation (1) and emission (2) spectra of Dy2Zr(WO4)5. Chimica Techno Acta 2022, vol. 9(2), No. 20229205 ARTICLE 4 of 5 The 4F9/2–6H15/2 transition is magnetic-dipole and its in- tensity weakly depends on the crystal environment. The 4F9/2–6H13/2 transition is of the electric-dipole type. Due to low symmetry, the 4F9/2–6H13/2 transition becomes partial- ly allowed and its intensity is higher or comparable to the intensity of the 4F9/2–6H15/2 transition in crystals without an inversion center. If a rare-earth ion occupies a position with an inversion center and its environment is sufficient- ly symmetric, then the transition intensity is significantly lower than 4F9/2–6H15/2. Thus, we can conclude that the environment of the rare-earth ion has rather low sym- metry, which is confirmed by the structural analysis data. In the excitation spectrum of yellow luminescence (Figure 6, curve 1), there is a number of bands associated with the transition from the 4H15/2 term to higher energy terms with subsequent relaxation and luminescence from the 4F9/2 level. The most intense excitation bands corre- spond to transitions to the 4F3/2, 4L19/2 terms; upon excita- tion to a group of levels with lower energies: 6P5/2, 4M19/2, 5F7/2, 4I13/2, luminescence with a lower intensity is observed. 4. Conclusions New Ln2Zr(WO4)5 (Ln = Tb, Dy) double tungstates were obtained by ceramic and sol-gel techniques. The conditions of the sol-gel synthesis of tungstates were optimized. Their crystallographic and luminescent properties were determined. It was established that Ln2Zr(WO4)5 (Ln= Dy, Tb) double tungstates are crystallized in orthorhombic crystal system, space group Cmc21 (Z = 4). The luminescence properties of Tb3+, Dy3+ ions in tung- state matrices were investigated. The observed spectral lines and bands of luminescence and excitation were iden- tified. The structural features of the considered double tung- states suggest the possibility of their use as matrices for ob- taining effective laser materials and promising phosphors. Supplementary materials No supplementary materials are available. Funding This research was carried out within the state assignment of Baikal Institute of Nature Management SB RAS No. 0273-2021-0008. Acknowledgment The Equipment of the Centre for Collective Use of Baikal Institute of Nature Management SB RAS. Author contributions Conceptualization: J.G.B., B.G.B. Data curation: B.G.B., J.G.B., S.G.D., R.Yu.Sh. Formal Analysis: S.G.D., D.O.S., Yu.L.T., Ts.T.B., O.D.Ch. Funding acquisition: J.G.B. Investigation: S.G.D., D.O.S., R.Yu.Sh. Methodology: S.G.D., D.O.S., R.Yu.Sh. Project administration: B.G.B., J.G.B. Resources: B.G.B., J.G. B., R.Yu.Sh. Software: S.G.D., D.O.S., R.Yu.Sh. Supervision: B.G. B., J.G.B. Validation: S.G. D., D.O. S., R.Yu.Sh. Visualization: S.G.D., D.O.S., R.Yu.Sh. Writing – original draft: B.G.B., J.G.B. Writing – review & editing: S.G.D., D.O.S. Conflict of interest The authors declare no conflict of interest. Additional information Author ID’s: B.G. 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