Crystals, Volume 7, Issue 9 (September 2017) – 26 articles

While high-throughput screening for protein crystallization conditions have rapidly evolved in the last few decades, it is also becoming increasingly necessary for the control of crystal size and shape as increasing diversity of protein crystallographic experiments. For example, X-ray crystallography (XRC) combined with photoexcitation and/or spectrophotometry requires optically thin but well diffracting crystals. By contrast, large-volume crystals are needed for weak signal experiments, such as neutron crystallography (NC) or recently developed X-ray fluorescent holography (XFH). In this article, we present, using hemoglobin as an example protein, some techniques for obtaining the crystals of controlled size, shape, and adequate quality. Furthermore, we describe a few case studies of applications of the optimized hemoglobin crystals for implementing the above mentioned crystallographic experiments, providing some hints and tips for the further progress of advanced protein crystallography. Full article

We investigate the microstructure evolution of Ag-alloyed PbTe compounds for thermoelectric (TE) applications with or without additions of 0.04 at. % Bi. We control the nucleation and temporal evolution of Ag₂Te-precipitates in the PbTe-matrix applying designated aging heat treatments, aiming to achieve homogeneous dispersion of precipitates with high number density values, hypothesizing that they act as phonon scattering centers, thereby reducing lattice thermal conductivity. We measure the temperature dependence of the Seebeck coefficient and electrical and thermal conductivities, and correlate them with the microstructure. It is found that lattice thermal conductivity of PbTe-based compounds is reduced by controlled nucleation of Ag₂Te-precipitates, exhibiting a number density value as high as 2.7 × 10²⁰ m⁻³ upon 6 h aging at 380 °C. This yields a TE figure of merit value of ca. 1.4 at 450 °C, which is one on the largest values reported for n-type PbTe compounds. Subsequent aging leads to precipitate coarsening and deterioration of TE performance. Interestingly, we find that Bi-alloying improves the alloys’ thermal stability by suppressing microstructure evolution, besides the role of Bi-atoms as electron donors, thereby maintaining high TE performance that is stable at elevated service temperatures. The latter has prime technological significance for TE energy conversion. Full article

Zn_7/3Sb_2/3O₄ is a secondary phase in ZnO-based varistors. Acceptor impurities, such as Li⁺, increase the resistivity. This effect is produced by a modification of the grain boundary barriers. The role of the cationic distribution in the mentioned events is worth clarifying. The Li_0.5Zn_5/3Sb_2.5/3O₄ room-temperature structure was determined by means of a neutron diffraction and synchrotron X-ray diffraction investigation. The title compound was prepared by conventional ceramic process. The elemental composition of the investigated sample was verified by means of electron microscopy—energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy. The neutron experiment was performed at the high-intensity neutron diffractometer with position-sensitive detector at the D1B beamline of the Laue-Langevin Institute, Grenoble. The high resolution synchrotron measurement was carried out at MCX beamline of Elettra Sincrotrone Trieste. Rietveld analysis was performed with the FullProf program. Li_0.5Zn_5/3Sb_2.5/3O₄ belongs to the spinel family, space group $Fd\overline{3}m$ (227). The measured lattice parameter is a = 8.5567(1) Å. The Li⁺¹ and Zn⁺² ions are randomly distributed among the tetrahedral and octahedral sites as opposed to Sb⁺⁵ ions which have preference for octahedral sites. Fractional coordinate of oxygen, u = 0.2596(1), indicates a slight deformation of the tetrahedral and octahedral sites. The data given in this paper provide structural support for further studies on measurements and microscopic explanations of the interesting properties of this family of compounds. Full article

The goal of this special issue is to obtain new insights into the roles of crystallography in functional materials. This special issue consists of eight papers illustrating the structure and property relationships, as well as applications of selected classes of materials that deal with various aspects of functional materials, ranging from battery, magnetic, photocatalysis, and waveguide materials, to luminescent metal-organic frameworks and borates, semiconductors, and inorganic electrides. This issue provides further evidence of the importance of crystallography in understanding and improving various properties of functional materials, whether they are single crystals, bulk polycrystalline materials, or thin films. Full article

Below $T_{\mathrm{CO}}=157$ K the quasi-one-dimensional charge-transfer salt (TMTTF) ${}_2$ SbF ${}_6$ undergoes a pronounced phase transition to a charge-ordered ground state. We have explored the non-linear and photoconductive behavior as a function of applied voltage, laser pulse energy and temperature. Besides a decay of the photoconductive signal in a double exponential fashion in the millisecond range, we discover current oscillations in the kHz range induced by the application of short laser pulses. While the resonance frequencies do not depend on voltage or laser intensity and vary only slightly with temperature, the amplitude changes linearly with the laser intensity and voltage. We suggest that photo-induced fluctuations of the charge-ordered state alter the current flow of the single particles and hence, the photocurrent. The findings are discussed and compared to comparable phenomena in other low-dimensional electron systems. Full article

A series of LiNi_0.5Mn_1.5O₄ (LNMO) samples were synthesized by adjusting the molar ratio of (NH₄)₂CO₃ to Na₂CO₃ in a mixed precipitant for evaluating the effects of ammonia from (NH₄)₂CO₃ as a complexing agent and Na₂CO₃ as a precipitant on the morphology and electrochemical performances of LNMO. In this research, a rapid precipitation method followed by hydrothermal treatment was used to prepare the precursors of LNMO, and different molar ratios (0:1, 1:2, 1:1, 2:1, 1:0) of (NH₄)₂CO₃ to Na₂CO₃ were used for mixed precipitants. The test results revealed that the cathode material exhibits the best electrochemical performance when the molar ratio of (NH₄)₂CO₃ to Na₂CO₃ is set at 1:2, displaying a specific discharge capacity of 129.4 mA h g⁻¹ at 0.5 C and a capacity retention of 82.3% after 200 charge–discharge cycles. In addition, it still shows a high rate performance with a discharge capacity of 112.7 mA h g⁻¹ at 10 C and 98.8 mA h g⁻¹ at 20 C, which is attributed to an accurate Ni/Mn ratio, smaller primary particle sizes and a porous spherical morphology. Full article

A newly designed Co(II) complex, [Co₃(L)(OAc)₂(CH₃OH)₂]·CH₃OH, by the reaction of a bis(salamo)-type tetraoxime ligand (H₄L) with Co(II) acetate tetrahydrate was synthesized and characterized by elemental analyses, IR, UV-vis spectra and single-crystal X-ray crystallography. The UV-vis titration experiment manifested that a trinuclear (L:M = 1:3) complex was formed. It is worth noting that the two terminal Co(II) (Co1 and Co3) atoms of the Co(II) complex have different coordination modes and geometries unreported earlier. Furthermore, through intermolecular interactions (C–H···O, C–H···π and O–H···O), a 2D layer-like network is constructed. In addition, the fluorescence behaviors, antimicrobial activities and electrochemical properties of H₄L and its Co(II) complex were investigated. Full article

A novel inorganic-organic hybrid supramolecular macrocyclic compound, (4-nitroanilinium)(18-crown-6)(PF₆)(1), was synthesized and characterized by infrared spectroscopy, thermogravimetric analysis, elemental analysis, differential scanning calorimetry (DSC), and single-crystal X-ray diffraction. Crystal 1 is found to comprise 1D C–H···F–P hydrogen-bonded chains of (4-nitroanilinium⁺)(18-crown-6) supramolecular cations and PF₆⁻ anions. DSC measurements confirm that 1 undergoes a reversible phase transition at 255 K with a hysteresis width of 6 K. A strong dielectric response is observed above 250 K at a low frequency (500 Hz), suggesting the occurrence of proton transfer in the C–H···F–P hydrogen bonds. A precise analysis on the main packing and structural differences, as well as the changes in the intermolecular interaction between the low- and high-temperature phases, reveals that C–H···F–P hydrogen bonds are the main factors affecting phase transition and dielectric behavior. Full article

This study, using atomic-force and polarized-optical light (AFM and POM) microscopies on the extinction banded spherulites of poly(dodecamethylene terephthalate) (P12T) at high T_c = 110 °C with a film thickness kept at 1–3 µm, has verified that banded spherulites can be composed of stacks of entirely single-crystal-like lamellae free of any twisting, flipping, or bending, and no branching of lamellae. Defects in the crystal packing of extinction bands are present in both intra-band and inter-band regions. The intra-band defects originate from the miss-match in spiral-circling into circular bands while the inter-band defects are in the interfaces between successive bands where single crystals in the ridge are jammed to deformation, then suddenly precipitate prior to initiating another cycle of banding. The fish-scale lamellae, at the initiation of a cycle, are orderly packed as terrace-like single crystals; conversely, near or on the defected regions, they are highly jammed or squeezed and deformed to beyond recognition of their original single-crystal nature. Full article

Here, we investigate the strengths of R–X···π interactions, involving both chlorine and bromine, in model systems derived from protein-ligand complexes found in the PDB. We find that the strengths of these interactions can vary significantly, with binding energies ranging from −2.01 to −3.60 kcal/mol. Symmetry adapted perturbation theory (SAPT) analysis shows that, as would be expected, dispersion plays the largest role in stabilizing these R–X···π interactions, generally accounting for about 50% to 80% of attraction. R–Br···π interactions are, for the most part, found to be stronger than R–Cl···π interactions, although the relative geometries of the interacting pair and the halogen’s chemical environment can also have a strong impact. The two factors that have the strongest impact on the strength of these R–X···π interactions is the distance between the halogen and the phenyl plane as well as the size of the halogen σ-hole. Full article

Nanoprobes are one of the most important components in several fields of nanoscience to study materials, molecules and particles. In scanning probe microscopes, the nanoprobes consist on silicon tips coated with thin metallic films to provide additional properties, such as conductivity. However, if the experiments involve high currents or lateral frictions, the initial properties of the tips can wear out very fast. One possible solution is the use of hard coatings, such as diamond, or making the entire tip out of a precious material (platinum or diamond). However, this strategy is more expensive and the diamond coatings can damage the samples. In this context, the use of graphene as a protective coating for nanoprobes has attracted considerable interest. Here we review the main literature in this field, and discuss the fabrication, performance and scalability of nanoprobes. Full article

High-quality mixed-cation lead mixed-halide (FAPbI₃)_0.85(MAPbBr₃)_0.15 perovskite films have been prepared using CH₃NH₃Cl additives via the solvent engineering method. The UV/Vis result shows that the addition of additives leads to enhanced absorptions. XRD and SEM characterizations suggest that compact, pinhole-free and uniform films can be obtained. This is attributable to the crystallization improvement caused by the CH₃NH₃Cl additives. The power conversion efficiency (PCE) of the F-doped SnO₂ (FTO)/compact-TiO₂/perovskite/Spiro-OMeTAD/Ag device increases from 15.3% to 16.8% with the help of CH₃NH₃Cl additive. Full article

The solid-state reaction of WO₃ with W was studied in order to clarify the phase formation in the binary system W-O around the composition WO_x (2.50 ≤ x ≤ 3) during spark plasma sintering (SPS). A new phase “WO_2.82” is observed in the range 2.72 ≤ x ≤ 2.90 which might have the composition W₁₂O₃₄. The influence of the composition on the thermoelectric properties was investigated for 2.72 ≤ x ≤ 3. The Seebeck coefficient, electrical conductivity and electronic thermal conductivity are continuously tunable with the oxygen-to-tungsten ratio. The phase formation mainly affects the lattice thermal conductivity κ_lat which is significantly reduced until 700 K for the sample with the composition x = 2.84, which contains the phases W₁₈O₄₉ and “WO_2.82”. In single-phase WO_2.90 and multi-phase WO_x materials (2.90 ≤ x ≤ 3), which contain crystallographic shear plane phases, a similar reduced κ_lat is observed only below 560 K and 550 K, respectively. Therefore, the composition range x < 2.90 in which the pentagonal column structural motif is formed might be more suitable for decreasing the lattice thermal conductivity at high temperatures. Full article

Abstract: As a recycled material, flue gas desulfurization gypsum has been used to prepare calcium sulfate hemihydrate whisker (CSHW) through hydrothermal synthesis for several decades. However, the subsequent utilization of this resultant material has not yet received considerable attention. In the present research, CSHW was successfully synthesized at a certain region, and was used for the adsorption of lead ions from aqueous solutions, thereby broadening the research field for the practical application of CSHW. Its adsorption capacity was significantly influenced by various parameters, particularly, the pH level and initial lead concentration. The pH value highly affected the hydrolysis degree of lead ions and dominated the adsorption of lead. The equilibrium isotherms under two different temperatures were simulated using Langmuir, Freundlich, and Temkin models. Both Langmuir and Temkin models showed a good fit to the data. Combined with the well-fitted pseudo-second-order model, the adsorption mechanism was thought to be a chemisorption process that was enforced by the ion exchange reaction. In addition, the specific crystal structure of CSHW revealed that ion exchange reaction occurred on the (010) and (100) facets due to their preferential growth and negatively charged property. The residual solid phase after adsorption was collected and detected using X-ray diffraction and scanning electron microscopy with energy dispersive X-ray spectroscopy. Results revealed that PbSO₄ was formed on the surface of CSHW. The alkaline condition introduced the tribasic lead sulfate, and thus reduced the stability of the adsorption system. Full article

p-Type doping represents a key step towards III-nitride (InN, GaN, AlN) optoelectronic devices. In the past, tremendous efforts have been devoted to obtaining high quality p-type III-nitrides, and extraordinary progress has been made in both materials and device aspects. In this article, we intend to discuss a small portion of these processes, focusing on the molecular beam epitaxy (MBE)-grown p-type InN and AlN—two bottleneck material systems that limit the development of III-nitride near-infrared and deep ultraviolet (UV) optoelectronic devices. We will show that by using MBE-grown nanowire structures, the long-lasting p-type doping challenges of InN and AlN can be largely addressed. New aspects of MBE growth of III-nitride nanostructures are also discussed. Full article

Two newly designed complexes, [Zn(L¹)(EtOH)] (1) and [{Zn(L²)(OAc)₂}₂Zn]·CHCl₃ (2) derived from salamo and half-salamo chelating ligands (H₂L¹ and HL²) have been synthesized and characterized by elemental analyses, IR and UV-VIS spectra, fluorescence spectra, and X-ray crystallography. Complex 1 shows a slightly distorted tetragonal pyramid and forms an infinite 3D supramolecular structure. All of the Zn(II) ions in complex 2 are hexa-coordinated with slightly distorted octahedral geometries. Complex 2 possesses an infinite 2D space structure. The fluorescence titration experiments were used to characterize fluorescence properties of complexes 1 and 2. And the normalized fluorescent spectra exhibit that complexes 1 and 2 have favourable fluorescent emissions in different solvents. Full article

A novel ultrathin g-C₃N₄ nanosheet-modified BiOCl hierarchical flower-like plate heterostructure (abbreviated as BC/CN) was constructed via a thermal polymerization of urea precursor followed with hydrolysis route. The as-prepared samples were well characterized by various analytical techniques. The morphological observation showed that hierarchical flower-like BiOCl nanoplates were discretely anchored on the surface of ultra-thin C₃N₄ nanosheets. The photocatalytic performance of the as-prepared photocatalysts was evaluated by degradation of methylene blue (MB) under visible-light irradiation. The results showed that BC/CN photocatalyst exhibited enhanced photostability and photocatalytic performance in the degradation process. On the basis of experimental results and the analysis of band energy structure, it could be inferred that the enhanced photocatalytic performance of BC/CN photocatalyst was intimately related with the hybridization of hierarchical flower-like BiOCl nanoplates with ultrathin g-C₃N₄ nanosheets, which provided good adsorptive capacity, extended light absorption, suppressed the recombination of photo-generated electron–hole pairs, and facilitated charge transfer efficiently. Full article

Two-dimensional semiconductors, such as transition-metal dichalcogenides (TMDs) and black phosphorous (BP), have found various potential applications in electronic and opto-electronic devices. However, several problems including low carrier mobility and low photoluminescence efficiencies still limit the performance of these devices. Interfacing 2D semiconductors with functional oxides provides a way to address the problems by overcoming the intrinsic limitations of 2D semiconductors and offering them multiple functionalities with various mechanisms. In this review, we first focus on the physical effects of various types of functional oxides on 2D semiconductors, mostly on MoS₂ and BP as they are the intensively studied 2D semiconductors. Insulating, semiconducting, conventional piezoelectric, strongly correlated, and magnetic oxides are discussed. Then we introduce the applications of these 2D semiconductors/functional oxides systems in field-effect devices, nonvolatile memory, and photosensing. Finally, we discuss the perspectives and challenges within this research field. Our review provides a comprehensive understanding of 2D semiconductors/functional oxide heterostructures, and could inspire novel ideas in interface engineering to improve the performance of 2D semiconductor devices. Full article

The growth of single crystalline films (SCFs) with excellent scintillation properties based on the Tb_1.5Gd_1.5Al_5−yGa_yO₁₂:Ce mixed garnet at y = 2–3.85 by Liquid Phase Epitaxy (LPE) method onto Gd₃Al_2.5Ga_2.5O₁₂ (GAGG) substrates from BaO based flux is reported in this work. We have found that the best scintillation properties are shown by Tb_1.5Gd_1.5Al₃Ga₂O₁₂:Ce SCFs. These SCFs possess the highest light yield (LY) ever obtained in our group for LPE grown garnet SCF scintillators exceeding by at least 10% the LY of previously reported Lu_1.5Gd_1.5Al_2.75Ga_2.25O₁₂:Ce and Gd₃Al_2–2.75 Ga_3–2.25O₁₂:Ce SCF scintillators, grown from BaO based flux. Under α-particles excitation, the Tb_1.5Gd_1.5 Al₃Ga₂O₁₂:Ce SCF show LY comparable with that of high-quality Gd₃Al_2.5Ga_2.5O₁₂:Ce single crystal (SC) scintillator with the LY above 10,000 photons/MeV but faster (at least by 2 times) scintillation decay times t_1/e and t_1/20 of 230 and 730 ns, respectively. The LY of Tb_1.5Gd_1.5Al_2.5Ga_2.5O₁₂:Ce SCFs, grown from PbO flux, is comparable with the LY of their counterparts grown from BaO flux, but these SCFs possess slightly slower scintillation response with decay times t_1/e and t_1/20 of 330 and 990 ns, respectively. Taking into account that the SCFs of the Tb_1.5Gd_1.5Al_3–2.25Ga_2–2.75O₁₂:Ce garnet can also be grown onto Ce³⁺ doped GAGG substrates, the LPE method can also be used for the creation of the hybrid film-substrate scintillators for simultaneous registration of the different components of ionization fluxes. Full article

Crystallographic studies frequently involve the determination of a previously unknown crystal structure; General Structure Analysis System (GSAS)-II provides two methods for this purpose. The Monte Carlo/simulated annealing method is fundamentally stochastic in nature; random trials are tested for suitability by comparing calculated structure factors with a suite of observed ones. In contrast, the charge flipping method may begin with a suite of random structure factor phases, but the subsequent mathematical steps are entirely deterministic even though they appear to display chaotic behavior. This paper will briefly describe these methods as implemented in GSAS-II, illustrating their use with examples. Full article

The crystal structures of salts 6–9 prepared from (R)-2-methoxy-2-(1-naphthyl)propanoic acid [(R)-MαNP acid, (R)-1] and (R)-1-arylethylamines [salt 6, (R)-1-(4-methoxyphenyl)ethylamine∙(R)-1; salt 7, (R)-1-(4-fluorophenyl)ethylamine∙(R)-1; salt 8, (R)-1-(4-chlorophenyl)ethylamine∙(R)-1; and salt 9, (R)-1-(3-chlorophenyl)ethylamine∙(R)-1] were elucidated by X-ray crystallography. The solid-state associations and conformations of the MαNP salts were defined using the concepts of supramolecular- and planar chirality, respectively, and the crystal structures of salts 6–9 were interpreted as a three-step hierarchical assembly. The para-substituents of the (R)-1-arylethylammonium cations were found on sheet structures consisting of 2₁ columns. Thus, salts possessing smaller para-substituents, that is, salt 7 (p-F) and salt 9 (p-H), and larger para-substituents, that is, salt 6 (p-OMe) and salt 8 (p-Cl), crystallized in the space groups P2₁ and C2, respectively. Additionally, weak intermolecular interactions, that is, aromatic C–H···π, C–H···F, and C–H···O interactions, were examined in crystalline salts 6–9. Full article

Polycrystalline Bi₂Se_3−xTe_x (x = 0~1.5) samples were prepared by self-propagating high-temperature synthesis (SHS) combined with spark plasma sintering (SPS) and their thermoelectric properties were investigated. The SHS-SPS process can shorten the time with few energy consumptions, and obtain almost pure Bi₂Se₃-based phases. Consequently, the Se vacancies and anti-site defects contribute to the converged carrier concentration of ~2 × 10¹⁹ cm⁻³ while the increased carrier effective mass enhances the Seebeck coefficient to more than −158 μV K⁻¹ over the entire temperature range. The lattice thermal conductivity is suppressed from 1.07 Wm⁻¹ K⁻¹ for the pristine specimen to ~0.6 Wm⁻¹ K⁻¹ for Te-substitution samples at 300 K because of point defects caused by the difference of mass and size between Te and Se atoms. Coupled with the enhanced power factor and reduced lattice thermal conductivity, a high ZT of 0.67 can be obtained at 473 K for the Bi₂Se_1.5Te_1.5 sample. Our results reveal that Te-substitution based on the SHS-SPS method is highly-efficient and can improve the thermoelectric properties of Bi₂Se₃-based materials largely. Full article

The electrostatic potential near to the oxygen atom in each of the cyclic ethers 2,5-dihydrofuran, oxetane and oxirane has been calculated by using a distributed multipole analysis (DMA) of each molecule. The electrostatic potential energy V(φ) of a unit non-perturbing positive charge was calculated (via the DMA of the cyclic ether molecule) as a function of the angle φ between the C₂ axis of the cyclic ether and a vector of length r from the O atom to the unit charge. The resulting potential energy functions each has two equivalent minima. The angles φ_min at the minima are compared with the angles φ₀ and φ_e made by the O⋯H bond with the C₂ axes in the cyclic ether⋯HF complexes, as determined by rotational spectroscopy and ab initio calculations at the CCSD(T)-F12c/cc-pVTZ-F12 level of theory, respectively. An electrostatic model of cyclic ether⋯HF complexes in which the DMA of the cyclic ether interacts with a simple extended electric dipole representation of HF is also used to calculate the variation of the potential energy V_HF(φ) of the HF molecule with φ. The angles φ_min generated by this model are also compared with φ₀ and φ_e. The extent to which the electrostatic potential and the extended electric dipole HF model can be used as probes for the directions of non-bonding electron pairs carried by O in these cyclic ethers is discussed. Full article

We investigated the electro-optic characteristics of a polymer-stabilized, in-plane-switching (IPS) liquid crystal cell as the UV curing temperature was varied. We found that the response time of an IPS cell could be reduced through low-temperature UV curing of a low concentration of polymer material. We also found that fast switching could be achieved at a low operating voltage and with little light leakage in the dark state. Low-temperature curing of the polymer structure could greatly reduce the average distance between polymer bundles even at low polymer concentrations. Therefore, the decrease in transmittance of a polymer-stabilized IPS cell could be minimized by increasing the cell gap without sacrificing the response time because of the sufficiently high anchoring strength of the polymer structure obtained through low-temperature UV curing. Full article

The chlorinated ethanoanthracenes: 4,5,12- and 1,8,12-(trichloro-9,10-dihydro-9,10-ethanoanthracene-12-carbonitriles) (1 and 2), which are regioisomers, were synthesized and characterized using nuclear magnetic resonance (¹H- and ¹³C-NMR) and infrared (IR) spectroscopic techniques. The structure of isomer 1 was further confirmed using a single-crystal X-ray technique. The relative stabilities of the title compounds were calculated using the density functional theory (DFT) method on the basis of their total energies and thermodynamic parameters. Isomer 1 is thermodynamically more stable than isomer 2 in the gas phase and in solution. The calculated molecular geometry of isomer 1 agreed well with the experimental X-ray structure. The atomic charge distribution at the different atomic sites was calculated using natural bond orbital analysis. Isomer 2 was predicted to be more polar than isomer 1. Full article

Yb and In double-filled and Fe substituted polycrystalline p-type skutterudite antimonides were synthesized by direct reaction of high-purity elements, followed by solid-state annealing and densification by hot pressing. The stoichiometry and filling fraction were determined by both Rietveld refinement of the X-ray diffraction data and energy dispersive spectroscopic analyses. The transport properties were measured between 300 K and 830 K, and basically indicate that the resistivity and Seebeck coefficient both increase with increasing temperature. In both specimens, the thermal conductivity decreased with increasing temperature up to approximately 700 K, where the onset of bipolar conduction was observed. A maximum ZT value of 0.6 at 760 K was obtained for the Yb_0.39In_0.018Co_2.4Fe_1.6Sb₁₂ specimen. Full article