Trigonal Unit Cell Research Articles

Lizardite “kolskite” from the Lesnaya Varaka alkaline ultrabasic massif (Kola peninsula): new data

Background. A rare morphological variety of magnesian serpentine, described in 1939 in the veins of the Lesnaya Varaka alkaline ultrabasic massif (Kola Peninsula) under the name “kolskite” is studied. For a long time, this variety has been considered an antigorite.Aim. Identification of the polymorphic modification of “worm-like” serpentine; determination of its crystal chemical features and possible genesis.Materials and methods. Samples were studied using electron probe analysis and scanning electron microscopy by a Jeol JSM-IT500 scanning electron microscope equipped with an INCA X-Max energy dispersion spectrometer; powder X-ray diffraction; infrared spectroscopy using a FSM-1201 IR Fourier spectrometer; and Raman spectroscopy using a EnSpectr R532 spectrometer.Results. Serpentine “kolskite” is represented by lizardite with the empirical formula (Mg2.79Al0.04Fe3+0.01)∑2.84[Si2.06O5](OH)4. The calculated parameters of the trigonal unit cell are as follows: a = 5.32(1) Å, c = 7.88(2) Å, V = 193.0(1) Å3. An increase in parameter c compared to that of apoolivine lizardite typical of ultrabasic objects indicates an expansion of the interlayer distance and is associated with serpentine hydration.Conclusion. The formation of “worm-like” lizardite aggregates could occur either by replacing vermiculite under the action of low-temperature alkaline hydrothermal solutions, or as a result of hypergenic alteration in the earlier apoolivine serpentine.

Zipserite, a new bismuth chalcogenide Bi5(S,Se)4 from Nagybörzsöny in Hungary with a R$\bar{3}$m(00γ)00 modulated structure

AbstractZipserite is a new mineral species discovered in a sample collected from the old mine dumps of the abandoned epithermal deposit Nagybörzsöny in Hungary. Zipserite occurs as anhedral to subhedral, lath-like grains, up to 500 μm in size, in hydrothermally strongly altered rocks. It is found at a contact between bismuth and bismuthinite, also associated with rare ikunolite and joséite-A. Zipserite is silvery white with a metallic lustre. Mohs hardness is ca. 2–3 and the calculated density is 7.815 g.cm–3. In reflected light, zipserite is grey–white, with colour and reflectance essentially matching those of bismuthinite. Bireflectance is weak, internal reflections not present. Anisotropy is moderately strong, with dark blue and grey colours of anisotropy. Reflectance values for the four Commission on Ore Mineralogy wavelengths of zipserite in air [Rmax, Rmin (%) (λ in nm)] are: 48.4, 46.4 (470); 47.8, 45.9 (546); 47.8, 45.8 (589); and 47.5, 45.6 (650). The empirical formula, based on electron-microprobe analyses, is (Bi4.74Pb0.31)Σ5.05(S3.38Se0.56Te0.02)Σ3.96, that can be simplified as Bi5(S,Se)4. The ideal end-member formula of zipserite is Bi5S4, which requires Bi 89.07 and S 10.93, total 100 wt.%. Zipserite possesses a fascinating crystal structure. The average structure is trigonal, with space group P$\bar{3}$m, a = 4.162(1) Å, c = 16.397(1) Å, V = 245.94(4) Å3 and Z = 2. The structure is built by the alternation of a double bismuth layer Bi2 and the Bi3S4 block which is a three octahedra thick layer. Its general formula can be expressed as Bi2 + Bi3S4, which corresponds directly to the observed stacking. At 98 K, the structure can be described using the superspace formalism with an R-centred trigonal unit cell a = 4.209(2) Å, c0 = 5.616(6) Å, a modulation vector q ≈ 4/3 c* and the superspace group R$\bar{3}$m(00γ)00. Zipserite is not only a new mineral but also the first named member of a new sub-group of compounds within the broader family of bismuth chalcogenides, characterised by complex stacking of structural units (Bi2 layers and Bi3S4 blocks). Some of these phases are being investigated as promising thermoelectric materials and synthetic analogues of zipserite could also be inspected for similar physical properties.

Ba1.09Pb0.91Be2(BO3)2F2: The First Pb-Containing Beryllium Borate Fluoride with Trigonal Prismatic PbO6 and 2D [Be3B3O6F3]∞ Layers.

Ba1.09Pb0.91Be2(BO3)2F2 (BPBBF), a previously unreported lead-containing beryllium borate fluoride, has been successfully grown through a high-temperature flux method. Its structure is solved by single-crystal X-ray diffraction (SC-XRD), and it is optically characterized via infrared, Raman, UV-vis-IR transmission, and polarizing spectra as well. SC-XRD data suggests that it can be indexed by a trigonal unit cell (space group P3m1) with lattice parameters a = 4.7478(6) Å, c = 8.3856(12) Å, Z = 1, and V = 163.70(5) Å. This material could be considered as a derivative of the Sr2Be2B2O7 (SBBO) structural motif. It consists of 2D [Be3B3O6F3]∞ layers in the crystallographic ab plane, with divalent Ba2+ or Pb2+ cations serving as spacers among the adjacent layers. Ba and Pb were found to adopt a disordered arrangement in the trigonal prismatic coordination within the BPBBF structural lattice, which is evidenced by both structural refinements against SC-XRD data and energy dispersive spectroscopy. The UV absorption edge (279.1 nm) and birefringence (Δn = 0.054@ 546.1 nm) of BPBBF are confirmed by UV-vis-IR transmission and polarizing spectra, respectively. The discovery of this previous unreported SBBO-type material, BPBBF, along with other reported analogues such as BaMBe2(BO3)2F2 (M = Ca, Mg, and Cd), provide a prodigious example for tuning the bandgap, birefringence, and short UV absorption edge via simple chemical substitution.

Hydrogen Absorption Reactions of Hydrogen Storage Alloy LaNi5 under High Pressure.

Hydrogen can be stored in the interstitial sites of the lattices of intermetallic compounds. To date, intermetallic compound LaNi5 or related LaNi5-based alloys are known to be practical hydrogen storage materials owing to their higher volumetric hydrogen densities, making them a compact hydrogen storage method and allowing stable reversible hydrogen absorption and desorption reactions to take place at room temperature below 1.0 MPa. By contrast, gravimetric hydrogen density is required for key improvements (e.g., gravimetric hydrogen density of LaNi5: 1.38 mass%). Although hydrogen storage materials have typically been evaluated for their hydrogen storage properties below 10 MPa, reactions between hydrogen and materials can be facilitated above 1 GPa because the chemical potential of hydrogen dramatically increases at a higher pressure. This indicates that high-pressure experiments above 1 GPa could clarify the latent hydrogen absorption reactions below 10 MPa and potentially explore new hydride phases. In this study, we investigated the hydrogen absorption reaction of LaNi5 above 1 GPa at room temperature to understand their potential hydrogen storage capacities. The high-pressure experiments on LaNi5 with and without an internal hydrogen source (BH3NH3) were performed using a multi-anvil-type high-pressure apparatus, and the reactions were observed using in situ synchrotron radiation X-ray diffraction with an energy dispersive method. The results showed that 2.07 mass% hydrogen was absorbed by LaNi5 at 6 GPa. Considering the unit cell volume expansion, the estimated hydrogen storage capacity could be 1.5 times higher than that obtained from hydrogen absorption reaction below 1.0 MPa at 303 K. Thus, 33% of the available interstitial sites in LaNi5 remained unoccupied by hydrogen atoms under conventional conditions. Although the hydrogen-absorbed LaNi5Hx (x < 9) was maintained below 573 K at 10 GPa, LaNi5Hx began decomposing into NiH, and the formation of a new phase was observed at 873 K and 10 GPa. The new phase was indexed to a hexagonal or trigonal unit cell with a ≈ 4.44 Å and c ≈ 8.44 Å. Further, the newly-formed phase was speculated to be a new hydride phase because the Bragg peak positions and unit cell parameters were inconsistent with those reported for the La-Ni intermetallic compounds and La-Ni hydride phases.

New Data on the Isomorphism in Eudialyte-Group Minerals. XII: Refined Structure of the Hydrated Mineral from the Inagli Massif

A hydrated eudialyte-group mineral from the Inagli alkaline massif (Kola Peninsula) has been investigated by electron-probe and X-ray diffraction analyses. The parameters of the trigonal unit cell are as follows: a = 14.1558(3) Å, c = 30.998(1) Å, V = 5378.6(3) Å3, sp. gr. R3; the calculated density is 2.661 g/cm3. The crystal structure is refined to the final reliability factor of R = 3.8% within the anisotropic approximation of atomic displacements using 1230 reflections with F 3σ(F). The simplified formula of the mineral (Z = 3) is (H3O)7Na7.5(K,Sr,Ba,Ce)1.5Zr3Ca6[Si24O68(OH)3(O,OH)]Si1.5Cl1(OH)2H2O1.5. The problems of symmetry of calcium-rich hydrated eudialyte-group minerals are discussed.

On the Isomorphism of Sodium at the M(2) Site in Eudialyte-Group Minerals: The Crystal Structure of Mn-Deficient Manganoeudialyte and the Problem of the Existence of the M(2)Na-Dominant Analogue of Eudialyte

Sodium plays an important role in the crystal structures of eudialyte-group minerals given that it can occupy different crystallographic sites. Predominantly, it distributes between the N(1–5) sites situated in the large cavities of the heteropolyhedral framework. Rarely, Na occupies split sites of the M(2) microregion where it can predominate over other elements (predominantly Mn, Fe2+, and Fe3+). The crystal structure of the Mn-deficient manganoeudialyte from the Lovozero alkaline complex (Kola Peninsula, Russia) has been refined. The trigonal unit–cell parameters are: a = 14.1848(2) Å, c = 30.4726(3) Å, V = 5309.90(11) Å3. The sample is a rare example of a high-sodium and high-calcium representative of the eudialyte group with Fe + Mn &lt; 2 apfu. The idealized formula is Na14Ca6[(Mn,Fe)2Na]Zr3Si2[Si24O72]O(OH)·2H2O with bivalent components, Mn2+ and Fe2+, dominating at the M(2) site. The regularities of isomorphism involving M(2)Na in EGMs and the problem of the existence of the M(2)Na-dominant analogue of eudialyte are discussed. The new data obtained in this work confirm the previous conclusion that the complete isomorphism between Ca-deficient and Ca-rich members of the eudialyte group cannot be realized in frames of a single-space group (R3m, R-3m or R3). Thus, the existence of the M(2)Na analogue of eudialyte remains questionable.

Distinctive occurrences of green-yellow luminescence from orthogermanate-type Ba9Y2(GeO4)6:Ce3+, Na+ phosphors under blue excitation and white-light performance with light-emitting diodes

In this study, barium yttrium orthogermanate luminescent host was prepared by a solid-state method using LiCl flux and combined with Ce3+-doped phosphor-converted light-emitting diodes (pc-LEDs) under blue excitation. The structure of Ba9Y2(GeO4)6 (Ba9Y2Ge6O24) was determined with the use of synchrotron X-ray powder diffraction. The compound crystallized in trigonal unit cell (R3¯H), which contains 12-, 9-, and 10-coordinated Ba sites with isolated tetrahedral Ge–O4 and octahedral Y–O6 polyhedrons. The X-ray diffraction patterns, photoluminescence spectra, defect characterization results, Gaussian deconvolution of fitting emission bands, ligand-field splitting parameters, d-band edge positions, distortion values, cation occupancy results, and scanning electron microscopy images of the Ce3+-doped phosphors were characterized to figure out the specific origin of the green-yellow luminescence under blue excitation. The white emission spectra, color-rendering index, correlated color temperature, Commission Internationale de l′Eclairage coordinates and internal quantum efficiency of Ba8.8Ce0.1Na0.1Y2Ge6O24 phosphors on a blue LED chip were measured. Finally, the valence states of Ge4+ ions in the Ba8.8Ce0.1Na0.1Y2Ge6O24 phosphors were determined by the extended X-ray absorption fine structure analysis at the Ge K-edge to elucidate the luminescence loss under a strong reduction atmosphere.

Guest-Mediated Hierarchical Self-Assembly of Dissymmetric Organic Cages to Form Supramolecular Ferroelectrics

Guest-Mediated Hierarchical Self-Assembly of Dissymmetric Organic Cages to Form Supramolecular Ferroelectrics

Computational Prediction of a Novel Superhard sp 3 Trigonal Carbon Allotrope with Bandgap Larger than DiamondSupported by the National Natural Science Foundation of China (Grant Nos. 11804307, U1804155, and U1604263), and the China Postdoctoral Science Foundation (Grant Nos. 2018M630830 and 2019T120631).

Searching for new carbon allotropes with superior properties has been a longstanding interest in material sciences and condensed matter physics. Here we identify a novel superhard carbon phase with an 18-atom trigonal unit cell in a full-sp 3 bonding network, termed tri-C18 carbon, by first-principles calculations. Its structural stability has been verified by total energy, phonon spectra, elastic constants, and molecular dynamics simulations. Furthermore, tri-C18 carbon has a high bulk modulus of 400 GPa and Vickers hardness of 79.0 GPa, comparable to those of diamond. Meanwhile, the simulated x-ray diffraction pattern of tri-C18 carbon matches well with the previously unexplained diffraction peaks found in chimney soot, indicating the possible presence of tri-C18 carbon. Remarkably, electronic band structure calculations reveal that tri-C18 carbon has a wide indirect bandgap of 6.32 eV, larger than that of cubic diamond, indicating its great potential in electronic or optoelectronic devices working in the deep ultraviolet region.

Magnetic, Electronic, and Mechanical Properties of Bulk ε-Fe2N Synthesized at High Pressures.

We sintered bulk trigonal ε-Fe2N (space group: P312) with the high-pressure and high-temperature method. Structural refinements by the Rietveld method result in a trigonal unit cell with parameters of a = 4.7767(1) Å and c = 4.4179(3) Å. ε-Fe2N is ferromagnetic with a Curie temperature of ∼250 K, a saturation magnetization (Ms) value of up to 1.2 μB/formula units (f.u.), and comparatively low coercive field. The Vickers hardness was measured, and the results showed that the asymptotic hardness of bulk ε-Fe2N is about 6.5 GPa with a load of 1000 g. Thermogravimetric (TG) analysis shows that ε-Fe2N is thermally stable below 670 K. ε-Fe2N exhibits good metal conductivity, and the electron transport measurements show that the resistivity of it is 172 μΩ cm at room temperature. The theoretical calculations suggest that the conducting states are mainly derive from Fe-3d states.

Trigonal double molybdates and tungstates: Ferroelastic phase transitions

The overview contains basic information about trigonal double molybdates and tungstates MR(XO4)2, representing a crystal family with layered structure. Their structure features networks of corner-linked RO6 octahedra and XO4 Â tetrahedra. Many compounds of this crystal family exhibit ferroelastic phase transitions. Their ferroelastic properties are discussed, with particular emphasis on the peculiarities of the domain structure. An overview of results of studies on ferroelastic phase transitions, obtained with various experimental methods, is provided. Models of trigonal unit cell distortion are presented for monoclinic phases of KSc(MoO4)2 and RbIn(MoO4)2 crystals.

On the CN-K coordination modes in Kn[M6-n(CN)6]·xH2O: first evidence of CN-K electron-deficient bonding.

Based on the determination of single crystal XRD structures of potassium hexacyanidometallates and on IR, and Raman data, here we propose for the first time the occurrence of an electron-deficient bonding between the N end of the CN- ligand and the K+ metal center. The crystal structures of Kn[M6-n(CN)6]·xH2O (M = Fe(ii), Ru(ii), Os(ii), Co(iii), Rh(iii), Ir(iii), Pt(iv)) reveal the presence of four types of CN-K interactions: (i) a linear CN-K bond, (ii) the N ends in a bipodal coordination involving two K atoms, (iii) the N ends in a tripodal coordination mode involving three K atoms and (iv) the N ends and the K atoms with the largest K-N distances within the subseries that can be attributed to the electrostatic interactions. The bi- and tripodal coordination modes between the N end of the CN- ligand and K+ ions are atypical and their nature is discussed in this contribution. The CN- ligand N end can behave as a two-electron donor that participates in a three-center two-electron bonding (i.e. Class II μ-L 3c-2e) for a N-bipodal coordination mode or as a two-electron donor that participates in a four-center two-electron bonding (4c-2e) for an N-tripodal coordination mode. Such a possibility is closely related to the π-back donation ability of the CN- ligand, which results in a charge density accumulation on the N end, which could be partially donated to the K atom through an σ-mechanism. For the divalent metals (Fe, Ru, Os), the solids crystallize with a monoclinic unit cell in the C2/c space group, while for the trivalent ones (Co, Rh, Ir), the crystal structure corresponds to an orthorhombic unit cell in the Pbcn space group. Potassium hexacyanidoplatinate(iv) crystallizes with a trigonal unit cell, in the P3[combining macron]1m space group, where each N end is always found coordinating two K atoms. The finding of these novel coordination modes of the CN- ligands, relying on an electron-deficient bonding behavior, paves the way for the design of functional materials based on hexacyanidometallates. The experimental results and the proposed electron-deficient bonding model herein discussed were appropriately supported by the computational calculations.

Анизотропия анионной проводимости в монокристаллах суперионного проводника CeF-=SUB=-3-=/SUB=-

The anisotropy of anionic conductivity in crystals of a superionic conductor CeF3 with the tysonite structure (sp. gr. P-3с1) has been studied for the first time. The conductivity measurements at temperatures from 300 K to 600 K were carried out along the principal a- and c-axes of trigonal unit cell of the crystal. The maximum value of electrical conductivity is observed along the c-axis. The superionic CeF3 crystals have the weak anisotropy of electrical conductivity equal to σ||c/σ||a = 2.4 and σ||c = 5.6 10–4 S/cm at 500 K. The anisotropy effect of anionic conductivity in individual fluorides with the tysonite structure is discussed in connection with the peculiarities of their atomic structure.

Conformation and Aromaticity Switching in a Curved Non-Alternant sp2 Carbon Scaffold.

A curved sp2 carbon scaffold containing fused pentagon and heptagon units (1) was synthesized by Pd‐catalyzed [5+2] annulation from a 3,9‐diboraperylene precursor and shows two reversible oxidation processes at low redox potential, accompanied by a butterfly‐like motion. Stepwise oxidation produced radical cation 1 .+ and dication 1 2+. In the crystal structure, 1 exhibits a chiral cisoid conformation and partial π‐overlap between the enantiomers. For the radical cation 1 .+, a less curved cisoid conformation is observed with a π‐dimer‐type arrangement. 1 2+ adopts a more planar structure with transoid conformation and slip‐stacked π‐overlap with closest neighbors. We also observed an intermolecular mixed‐valence complex of 1⋅(1 .+)3 that has a huge trigonal unit cell [(1)72(SbF6)54⋅(hexane)101] and hexagonal columnar stacks. In addition to the conformational change, the aromaticity of 1 changes from localized to delocalized, as demonstrated by AICD and NICS(1)zz calculations.

Conformation and Aromaticity Switching in a Curved Non‐Alternant sp2 Carbon Scaffold

AbstractA curved sp2 carbon scaffold containing fused pentagon and heptagon units (1) was synthesized by Pd‐catalyzed [5+2] annulation from a 3,9‐diboraperylene precursor and shows two reversible oxidation processes at low redox potential, accompanied by a butterfly‐like motion. Stepwise oxidation produced radical cation 1.+ and dication 12+. In the crystal structure, 1 exhibits a chiral cisoid conformation and partial π‐overlap between the enantiomers. For the radical cation 1.+, a less curved cisoid conformation is observed with a π‐dimer‐type arrangement. 12+ adopts a more planar structure with transoid conformation and slip‐stacked π‐overlap with closest neighbors. We also observed an intermolecular mixed‐valence complex of 1⋅(1.+)3 that has a huge trigonal unit cell [(1)72(SbF6)54⋅(hexane)101] and hexagonal columnar stacks. In addition to the conformational change, the aromaticity of 1 changes from localized to delocalized, as demonstrated by AICD and NICS(1)zz calculations.

The influence of Ni2+ and other ions on the trigonal structure of DNA.

We present a new structure of a DNA dodecamer obtained in the presence of Ni2+ ions. The DNA forms Ni-guanine cross-links between neighboring molecules. Our results show that an adequate dosage of Ni2+ may help to form well-defined DNA nanostructures. We also compare our structure with other dodecamers which present unique features and also crystallize in trigonal unit cells, strongly influenced by the counterions associated with DNA. In all cases, the DNA duplexes form parallel pseudo-helical columns in the crystal, similar to DNA-protamine and native DNA fibers.

Six novel carbon and silicon allotropes with their potential application in photovoltaic field

By stacking up five novel cagelike structures, three novel three-dimensional (3D) sp3 bonding networks, named hP24, hP30 and hP36, were predicted in this work for the first time. These three newly discovered structures have trigonal unit cell with the space groups of P−3m1, P−3m1 and P3m1, respectively. Using first-principle calculations, the physical properties, including structural, mechanical, electronic and optical properties of C and Si in hP24, hP30 and hP36 phases were systematically studied. All these newly discovered carbon and silicon allotropes were proven to be thermodynamically and mechanically stable. The wide indirect bandgap value in range of 3.89–4.03 eV suggests that C in hP24, hP30 and hP36 phases have the potential to be applied in high frequency and high power electronic devices. The direct bandgap value in range of 0.60–1.16 eV, the smaller electron and hole effective mass than diamond-Si, and the significantly better photon absorption characteristics than diamond-Si suggest that hP24-Si, hP30-Si and hP36-Si are likely to have better performance in photovoltaic applications than diamond-Si. hP24-Si also has the potential to be applied in infrared detectors.

Ca2+-substitution effects in Ba9-xCaxAl2Si6O24:Ce3+, Na+ phosphors

The Ca2+ ion was substituted for a Ba2+ ion in Ba9Al2Si6O24 host lattice using a solid-state reaction. The solid-solubility of Ba9-xCaxAl2Si6O24 compounds was characterized using X-ray powder diffraction (XRD) for x = 0 to x = 9 according to the Hume-Rothery rule. The obtained Ba9-xCaxAl2Si6O24 hosts between x = 2 and x = 5 were examined in order to index the peak positions as a single-phase orthosilicate, which has a trigonal unit-cell. The structure of Ba6Ca3Al2Si6O24 was characterized using synchrotron XRD. The photoluminescence excitation, emission spectra, and scanning electron microscopy (SEM) data of intense blue Ba8.8-xCaxCe0.1Na0.1Al2Si6O24 (x = 2 to x = 5) phosphors were monitored. Furthermore, a comparison of the quantum efficiency of the obtained phosphors and sodium salicylate was performed.

Mössbauer Spectral Study of the Low-Temperature Electronic and Magnetic Properties of α-FePO4 and the Mixed Valence Iron(II/III) Phosphate SrFe3(PO4)3.

The Mössbauer spectra of trigonal α-FePO4, measured between 4.2 and 300 K, exhibit hyperfine parameters characteristic of high-spin iron(III) in a pseudotetrahedral oxygen environment. Between 24.5 and 300 K, the spectra show a paramagnetic quadrupole doublet and at 24.0 K the spectrum reveals the onset of antiferromagnetic exchange. At 4.2 and 16 K, a single magnetic sextet is observed with hyperfine fields of 51.36(1) and 42.74(1) T, respectively, with an angle, θ, of 90° between the principal axis of the electric field gradient tensor in the basal plane of the trigonal unit cell and the hyperfine field along the c axis. The spectra obtained between 21 and 18 K have been fitted with two equal-area magnetic sextets with θ angles of 25 and 85°, angles which indicate that the iron(III) magnetic moments are canted away from the c axis. The reduced hyperfine field versus reduced temperature plot indicates a departure from a Brillouin S = 5/2 behavior, as a result of some magnetostriction at the Néel temperature. The Mössbauer spectra of class 1 mixed-valence SrFe3(PO4)3, measured between 4.2 and 300 K, exhibit hyperfine parameters characteristic of two high-spin iron(II) ions and one high-spin iron(III) ion in a pseudooctahedral oxygen environment. At and above 40 K, the spectra show two paramagnetic quadrupole doublets, whereas at 39.0 K the spectrum reveals the onset of ferrimagnetic exchange. Between 4.2 and 30 K, the spectra have been fitted with two magnetic sextets with θ angles of 85 and 10° for the iron(II) and iron(III) sites, respectively. The reduced hyperfine field versus reduced temperature plots for the iron(II) and iron(III) sites show a distinct departure from Brillouin S = 2 and S = 5/2 behavior, respectively, a departure that suggests a first-order magnetic transition at 39.5(5) K with differing magnetostrictions at the iron(II) and iron(III) sites.

Novel synthetic approach to the preparation of single-phase BixLa1−xMnO3+δ solid solutions

In this study, the BixLa1−xMnO3+δ solid solutions (x from 0 to 0.65) were synthesized using sol–gel combustion method with citric acid as a fuel and complexing agent. It was shown that changes in chemical composition of the materials lead to the evolution of crystal structure, morphology, and magnetic properties. The thermal behavior of precursor gel was investigated by thermogravimetric and differential scanning calorimetry (TG-DSC) measurements. X-ray diffraction (XRD) analysis demonstrated that all samples were monophasic. The Rietveld analysis showed that the structure can be indexed by trigonal or cubic unit cell depending on Bi3+ content. Scanning electron microscopy (SEM) was used to evaluate morphological features of the synthesized materials and revealed that Bi3+ ions significantly promote growth of the grains. The sol–gel-derived BixLa1−xMnO3+δ specimens were also characterized by FT-IR spectroscopy and magnetization measurements, which showed a clear correlation between magnetic properties and crystal structure of the materials.