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New Heusler compounds NiRh2Sb and CuRh2Sb are synthesized in nano-scale and in bulk. The nanoparticles prove to be excellent catalysts for electrochemical water splitting.

Crystal structure data for potassium orthoselenate(IV), K2SeO3, are reported for the first time. Colorless, block-shaped crystals were grown in a potassium hydroflux, i.e. under ultra-alkaline conditions, within 10 h. K2SeO3 crystallizes isostructural with Na2SO3 and K2TeO3 in the trigonal space group P\overline{3} with lattice parameters a = 6.1063 (4) Å and c = 6.9242 (4) Å at 100 (1) K. In the trigonal–pyramidal, C 3v-symmetric [SeO3]2– anion, the bond length is 1.687 (1) Å, and the bond angle is 103.0 (1)°. Two of the three unique potassium cations exhibit a coordination number of six, and the third a coordination number of nine.

Single crystals of LaTe1.9 (lanthanum telluride) have been obtained by chemical transport reactions with iodine as transport agent. LaTe1.9 adopts the CeSe1.9 structure type and crystallizes in the space group P42/n with lattice parameters a = 10.1072 (3) Å and c = 18.2874 (6) Å. The crystal structure comprises an alternating stacking of puckered [LaTe] slabs and planar [Te] layers along [001]. The planar [Te] layer is dominated by dumbbell-shaped Te2 2− anions along an isolated Te2− anion and a vacancy. The Te2 2− anions form an eight-membered ring enclosing the vacancy in the centre.

The study of Bi2Rh formation in a polyol process revealed a two-step mechanism. BiRh is formed by co-reduction of bismuth and rhodium cations and converted into Bi2Rh by Bi diffusion. Various starting materials and reaction parameters are examined.

Layered rare-earth delafossites $ARX_2$ with $R$ = Yb(III) or Ce(III) have received a lot of interest as potential hosts for a quantum spin-liquid ground state. Some systems of this family that show no long-range order down to the lowest measured temperatures, such as NaYbO$_2$, NaYbS$_2$, and NaYbSe$_2$, are presumed to be in a quantum spin-liquid state. However, other isostructural compounds are known to order antiferromagnetically at subkelvin temperatures. Among them, KCeS$_2$ exhibits stripe-$yz$ magnetic order in the triangular-lattice planes that sets in below 400 mK. Here we investigate the spin-wave spectrum of this ordered phase with powder inelastic neutron scattering and describe it using a model Hamiltonian obtained from first-principles calculations based on the complete $|J,m_J\rangle$ multiplet description of the Ce sites with an anisotropic nearest-neighbor exchange interaction. Combing the current understanding of the exchange interaction in the systems with the effects of texturing in the powder, we have been able to model the inelastic neutron scattering spectrum with high fidelity., 6 pages, 3 figures, accepted to Phys. Rev. B

Orange‐colored crystals of the oxoferrate tellurate K12+6x Fe6Te4−x O27 [x=0.222(4)] were synthesized in a potassium hydroxide hydroflux with a molar water–base ratio n(H2O)/n(KOH) of 1.5 starting from Fe(NO3)3 ⋅ 9H2O, TeO2 and H2O2 at about 200 °C. By using (NH4)2TeO4 instead of TeO2, a fine powder consisting of microcrystalline spheres of K12+6x Fe6Te4−x O27 was obtained. K12+6x Fe6Te4−x O27 crystallizes in the acentric cubic space group I 4‾ 3d. [FeIIIO5] pyramids share their apical atoms in [Fe2O9] groups and two of their edges with [TeVIO6] octahedra to form an open framework that consists of two loosely connected, but not interpenetrating, chiral networks. The flexibility of the hinged oxometalate network manifests in a piezoelectric response similar to that of LiNbO3.The potassium cations are mobile in channels that run along the directions and cross in cavities acting as nodes. The ion conductivity of cold‐pressed pellets of ball‐milled K12+6x Fe6Te4−x O27 is 2.3×10−4 S ⋅ cm−1 at room temperature. Magnetization measurements and neutron diffraction indicate antiferromagnetic coupling in the [Fe2O9] groups., K(nockout) response: K12+6x Fe6Te4−x O27 was synthesized under hydroflux conditions. The acentric cubic crystal structure comprises two non‐interpenetrating chiral oxometalate networks formed by edge‐ or corner‐sharing [TeVIO6] and [FeIIIO5] polyhedra. The potassium ions are mobile in the labyrinth between the networks. The magnetic moments of the iron cations are pairwise antiparallel, and the compound exhibits a strong piezoelectric response.

Crystals of RETe1.875±δ (RE = Ce, Pr, Sm, Gd; 0.004 ≤ δ ≤ 0.025) were grown using alkali halide flux and chemical transport reactions. The crystal structures are described in space group Amm2 (no. 38), with lattice parameters of a = 13.3729(5) A, b = 17.7918(5) A, c = 18.1561(4) A for CeTe1.87(1) (T = 100 K), a = 13.271(2) A, b = 17.747(3) A, c = 18.160(3) A for PrTe1.85(1) (T = 100 K), a = 13.1251(6) A, b = 17.4269(8) A, c = 17.8808(8) A for SmTe1.87(1) (T = 100 K), and a = 13.1762(4) A, b = 17.4995(5) A, c = 17.9591(5) A for GdTe1.88(1) (T = 296 K). The structures contain alternating stacks of puckered [RETe] slabs and planar [Te] layers. The latter are composed of small anionic entities, such as Te2- and Te22-, along with a large anionic eight-membered Te ring, as supported by electron localizability indicator-based bond analysis for an ordered model of GdTe1.875. Slightly different patterns for individual compounds indicate a considerable structural flexibility. Temperature-dependent resistance measurements confirm semiconducting behavior for PrTe1.875±δ and GdTe1.875±δ (magnetic data evidence RE3+ and an antiferromagnetic transition at TN = 4 K for CeTe1.875±δ and TN = 11 K for GdTe1.875±δ), whereas PrTe1.875±δ and SmTe1.875±δ show no long-range order down to 2 K.

Ionic liquids and deep eutectic solvents are of growing interest as solvents for the resource‐efficient synthesis of inorganic materials. This Review covers chemical reactions of various deep eutectic solvents and types of ionic liquids, including metal‐containing ionic liquids, [BF4]−‐ or [PF6]−‐based ionic liquids, basic ionic liquids, and chalcogen‐containing ionic liquids. Cases in which cations, anions, or both are incorporated into the final products are also included. The purpose of this Review is to raise caution about the chemical reactivity of ionic liquids and deep eutectic solvents and to establish a guide for their proper use., The chemical reactivity of ionic liquids and deep eutectic solvents can intentionally be exploited as a synthetic tool to prepare inorganic materials that are difficult or even impossible to obtain by traditional synthetic routes. This Review summarizes recent developments in inorganic syntheses that take advantage of reactions with ionic liquids or deep eutectic solvents.

The phase equilibria in the SnTe-Sb2Te3 system were re-investigated by a combination of Differential Thermal Analysis (DTA), Powder x-ray Diffraction (PXRD), and Scanning Electron Microscope equipped with Energy Dispersive x-ray Spectrometer (SEM-EDS) techniques. In an earlier reported version, this phase diagram was described as quasi-binary with only one intermediate compound, namely SnSb2Te4. Here we report the existence of the new van der Waals type compound SnSb4Te7 for the first time. Considerable homogeneity ranges for both ternary compounds are also revealed. According to DTA results, peritectic melting was found for both compounds. The corresponding temperatures were found to be 595 and 593 °C for SnSb2Te4 and SnSb4Te7, respectively. The PXRD pattern of the newly found phase was analyzed through the Rietveld method and the crystal structure was solved. In the considered quasi-binary system, two wide solid-solubility areas based on the constitutive compounds were also revealed.

Single crystals of a new twinned hexagonal perovskite compound Sr8Os6.3O24 have been synthesized, and structural and magnetic properties have been determined. The compound crystallizes in a hexagon...

The low temperature syntheses of AuTe2 and Ag2Te starting from the elements were investigated in the ionic liquids (ILs) [BMIm]X and [P66614]Z ([BMIm]+=1‐butyl‐3‐methylimidazolium; X = Cl, [HSO4]−, [P66614]+ = trihexyltetradecylphosphonium; Z = Cl−, Br−, dicyanamide [DCA]−, bis(trifluoromethylsulfonyl)imide [NTf2]−, decanoate [dec]−, acetate [OAc]−, bis(2,4,4‐trimethylpentyl)phosphinate [BTMP]−). Powder X‐ray diffraction, scanning electron microscopy, and energy‐dispersive X‐ray spectroscopy revealed that [P66614]Cl is the most promising candidate for the single phase synthesis of AuTe2 at 200 °C. Ag2Te was obtained using the same ILs by reducing the temperature in the flask to 60 °C. Even at room temperature, quantitative yield was achieved by using either 2 mol % of [P66614]Cl in dichloromethane or a planetary ball mill. Diffusion experiments, 31P and 125Te‐NMR, and mass spectroscopy revealed one of the reaction mechanisms at 60 °C. Catalytic amounts of alkylphosphanes in commercial [P66614]Cl activate tellurium and form soluble phosphane tellurides, which react on the metal surface to solid telluride and the initial phosphane. In addition, a convenient method for the purification of [P66614]Cl was developed.

Intermetallic phases are usually obtained by crystallization from the melt. However, phases containing elements with widely different melting and boiling points, as well as nanoparticles, which provide a high specific surface area, are hardly accessible via such a high-temperature process. The polyol process is one option to circumvent these obstacles by using a solution-based approach at moderate temperatures. In this study, the formation of Bi2Ir nanoparticles in a microwave-assisted polyol process was investigated. Solutions were analyzed using UV–Vis spectroscopy and the reaction was tracked with synchrotron-based in situ powder X-ray diffraction (PXRD). The products were characterized by PXRD and high-resolution transmission electron microscopy. Starting from Bi(NO3)3 and Ir(OAc)3, the new suboxide Bi4Ir2O forms as an intermediate phase at about 160 °C. Its structure was determined by a combination of PXRD and quantum-chemical calculations. Bi4Ir2O decomposes in vacuum at about 250 °C and is reduced to Bi2Ir by hydrogen at 150 °C. At about 240 °C, the polyol process leads to the immediate reduction of the two metal-containing precursors and crystallization of Bi2Ir nanoparticles.

Five substituted oxohydroxoferrates K2–x(Fe,M)4O7–y(OH)y (M=Si, Ge, Ti, Mn, Ir) were synthesized in a potassium hydroxide hydroflux with a molar base‐water ratio q(K) of about 0.9. While the hexagonal prisms of K2–x(Fe,Ti)4O7–y(OH)y crystallize in P63/mcm, all other compounds form hexagonal plates with the trigonal space group Purn:x-wiley:14341948:media:ejic202000891:ejic202000891-math-0001 1 m. The crystal structure of the oxohydroxoferrates resembles ß‐alumina. It consists of honeycomb layers urn:x-wiley:14341948:media:ejic202000891:ejic202000891-math-0002 Fe2O6] of edge‐sharing [FeO6] octahedra, where the hexagonal voids are capped by vertex‐sharing [FeO4] tetrahedra pairs. The cavities between the oxoferrate layers host the potassium ions. Depending on M, the substitution affects different iron positions and varies between 5 and 20 %. The magnetic structures of the antiferromagnetic compounds were determined by neutron powder diffraction. The potassium ion conductivity was characterized by electrochemical impedance spectroscopy at room temperature. By storing the oxohydroxoferrates in air or annealing them at 700 °C the ion conductivity was significantly increased, e. g. to 5.0 ⋅ 10−3 S cm−1 for a pressed pellet of the iridium substituted compound.

The two-dimensionally incommensurately modulated crystal structures of the compoundsRETe1.94(1)(RE= La, Pr, Nd) were investigated by single-crystal X-ray diffraction. The compounds crystallize in the tetragonal superspace groupP4/n(αβ½)00(−βα½)00 (No. 85.2.58.2) withq1= αa*+βb*+½c* andq2= −βa*+αb*+½c* and share a common motif of an alternating stacking of a puckered [RETe] layer and a planar [Te] layer. This basic structural motif is observed for all reported compounds with unusually large anisotropic displacement parameters in the planar [Te] layer. Taking the modulation into account, a distortion from this perfect square planar net is noted along with vacancies in the planar [Te] layer. The distortion leads to the formation of different discrete anions, like Te2−, Te22−and Te32−, similar to previously reported structures forREX2–δcompounds (RE= trivalent rare earth metal,X= S, Se, Te). The Te–Te distances in the modulated [Te] layer are found in a narrow range as compared to those in the corresponding sulfides and selenides.

A series of solid solutions (Li2Fe1-yMny)SO with a cubic antiperovskite structure was successfully synthesized. The composition (Li2Fe0.5Mn0.5)SO was intensively studied as a cathode in Li-ion batteries showing a reversible specific capacity of 120 mA h g-1 and almost a 100% Coulombic efficiency after 50 cycles at 0.1C meaning extraction/insertion of 1 Li per formula unit during 10 h. Operando X-ray absorption spectroscopy confirmed the redox activity of both Fe2+ and Mn2+ cations during battery charge and discharge, while operando synchrotron X-ray diffraction studies revealed a reversible formation of a second isostructural phase upon Li-removal and insertion at least for the first several cycles. In comparison to (Li2Fe)SO, the presence of Mn stabilizes the crystal structure of (Li2Fe0.5Mn0.5)SO during battery operation, although post mortem TEM studies confirmed a gradual amorphization after 50 cycles. A lower specific capacity of (Li2Fe0.5Mn0.5)SO in comparison to (Li2Fe)SO is probably caused by slower kinetics, especially in the two-phase region, as confirmed by Li-diffusion coefficient measurements.

Colorless crystals of the barium rare earth hydrogarnets Ba3[RE(OH)6]2 (RE = Sc, Y, Ho–Lu) were synthesized under hydroflux conditions with KOH at about T = 200 °C starting from the respective RE 2O3 and Ba (NO3)2. Single-crystal X-ray diffraction analysis on these distorted rhombic dodecahedra revealed the cubic space group Ia 3 ‾ $‾{3}$ d (no. 230). The crystal structures of the hydrogarnets Ba3[RE(OH)6]2 are discussed and compared with those of other hydrogarnets. The occurrence of additional reflections, which do not fulfill the reflection conditions of Ia 3 ‾ $‾{3}$ d, is analyzed and described by Renninger or λ/2 effects. A correlation is established between the space group adopted by a hydrogarnet and characteristic interatomic distances. In addition, single-crystal structure data of the strontium indium hydrogarnet Sr3[In(OH)6]2 are provided.

Topological insulators (TIs) gained high interest due to their protected electronic surface states that allow dissipation‐free electron and information transport. In consequence, TIs are recommended as materials for spintronics and quantum computing. Yet, the number of well‐characterized TIs is rather limited. To contribute to this field of research, we focused on new bismuth‐based subiodides and recently succeeded in synthesizing a new compound Bi12Rh3Sn3I9, which is structurally closely related to Bi14Rh3I9 – a stable, layered material. In fact, Bi14Rh3I9 is the first experimentally supported weak 3D TI. Both structures are composed of well‐defined intermetallic layers of ∞ 2[(Bi4Rh)3I]2+ with topologically protected electronic edge‐states. The fundamental difference between Bi14Rh3I9 and Bi12Rh3Sn3I9 lies in the composition and the arrangement of the anionic spacer. While the intermetallic 2D TI layers in Bi14Rh3I9 are isolated by ∞ 1[Bi2I8]2− chains, the isoelectronic substitution of bismuth(III) with tin(II) leads to ∞ 2[Sn3I8]2− layers as anionic spacers. First transport experiments support the 2D character of this material class and revealed metallic conductivity., Insulating: Bi12Rh3Sn3I9, a weak 3D topological insulator (TI) is derived from Bi14Rh3I9, which was the first weakly coupling (“weak”) 3D TI; a bulk semiconductor that hosts protected electronic surface states that allow dissipation‐free electron and information transport due to the specific symmetries of its electronic band structure. In consequence of their topological properties, TIs are envisioned as promising candidates for high‐performance spin field‐effect transistors and quantum bits.

Yellow prismatic crystals of rubidium bromido-antimonate(III) Rb7Sb3Br16 and of two different modifications of thallium bromido-bismuthate(III) Tl7Bi3Br16 were obtained by solvent-free synthesis and by precipitation from acidic aqueous solutions. X-ray diffraction analyses revealed the Tl7Bi3I16-type for α-Tl7Bi3Br16 (orthorhombic, Cmcm, a = 2324.31(8) pm, b = 1346.69(4) pm, c = 3460.0(1) pm; Pearson symbol oC312) and a new structure type for β-Tl7Bi3Br16 (monoclinic, C2/c, a = 2331.87(5) pm, b = 1343.33(3) pm, c = 3546.01(7) pm, β = 102.708(1)°; mC312). The antimonate Rb7Sb3Br16 adopts the Tl7Bi3I16-type, too (orthorhombic, Cmcm, a = 2347.16(3) pm, b = 1357.89(5) pm, c = 3539.47(9) pm; oC312). The crystal structures of α- and β-Tl7Bi3Br16 comprise alternating slabs of isolated [BiBr6]3– octahedra and [Bi2Br10]4– octahedra pairs. Both structure types are hierarchically organized and can be regarded as sphere close packing with the same stacking sequence, if octahedra and octahedra pairs are replaced by spheres of equal size. The structural relationship between the Tl7Bi3I16-type and the hydrate Na7Bi3Br16 · 18H2O, which comprises similar structural features, is discussed.

Crystals of the rare earth metal polytelluride LaTe1.82(1), namely, lanthanum telluride (1/1.8), have been grown by molten alkali halide flux reactions and vapour-assisted crystallization with iodine. The two-dimensionally incommensurately modulated crystal structure has been investigated by X-ray diffraction experiments. In contrast to the tetragonal average structure with unit-cell dimensions ofa= 4.4996 (5) andc= 9.179 (1) Å at 296 (1) K, which was solved and refined in the space groupP4/nmm(No. 129), the satellite reflections are not compatible with a tetragonal symmetry but enforce a symmetry reduction. Possible space groups have been derived by group–subgroup relationships and by consideration of previous reports on similar rare earth metal polychalcogenide structures. Two structural models in the orthorhombic superspace group,i.e.Pmmn(α,β,1 \over 2)000(−α,β,1 \over 2)000 (No. 59.2.51.39) andPm21n(α,β,1 \over 2)000(−α,β,1 \over 2)000 (No. 31.2.51.35), with modulation wave vectorsq1 = αa* + βb* + 1 \over 2c* andq2= −αa* + βb* + 1 \over 2c* [α = 0.272 (1) and β = 0.314 (1)], have been established and evaluated against each other. The modulation describes the distribution of defects in the planar [Te] layer, coupled to a displacive modulation due to the formation of different Te anions. The bonding situation in the planar [Te] layer and the different Te anion species have been investigated by density functional theory (DFT) methods and an electron localizability indicator (ELI-D)-based bonding analysis on three different approximants. The temperature-dependent electrical resistance revealed a semiconducting behaviour with an estimated band gap of 0.17 eV.

Single crystals of LaTe

High-efficient and fast adsorption of uranium is important to reduce the hazards caused by the uranium contamination of water environment due to the increased human activities. Herein, brewer's spent grain (BSG)-supported superabsorbent polymers (SAP) with different cross-linking densities are prepared as cheap and eco-friendly adsorbents for the first time via one-pot swelling and graft polymerization. A 7 wt% NaOH solution is used to swell BSG before grafting and subsequently neutralize the acrylic acid to control the reaction rate without producing alkaline wastewater. Compared with the traditional methods, swelling improves the grafting density and the utilization of raw materials due to the increased disorder degree of the BSG fibers. This results in the grafting of abundant carboxyl and amide groups onto the BSG backbone, forming a strongly hydrophilic polymer network of the BSG-SAP. Compared with the reference polymers without BSG, BSG-SAP presents higher adsorption capacity and enhanced reusability. The highly cross-linked BSG-SAP (BSG-SAP-H) shows an outstanding adsorption capacity of U(VI) (1465 mg/g at pH

Elemental tellurium readily dissolves in ionic liquids (ILs) based on tetraalkylphosphonium cations even at temperatures below 100 °C. In the case of ILs with acetate, decanoate, or dicyanamide anions, dark red to purple colored solutions form. A study combining NMR, UV-Vis and Raman spectroscopy revealed the formation of tellurium anions (Te

Intermetallic phases are usually obtained by crystallization from the melt. However, phases containing elements with widely different melting and boiling points, as well as nanoparticles, which provide a high specific surface area, are hardly accessible

Poly- and single-crystalline samples of ${\mathrm{Ba}}_{5}{(\mathrm{Os}{\mathrm{O}}_{5})}_{3}\mathrm{Cl}$ have been successfully synthesized. ${\mathrm{Ba}}_{5}{(\mathrm{Os}{\mathrm{O}}_{5})}_{3}\mathrm{Cl}$ crystallizes in the noncentrosymmetric space group $P{6}_{3}cm$. ${\mathrm{Ba}}_{5}{(\mathrm{Os}{\mathrm{O}}_{5})}_{3}\mathrm{Cl}$ shows a ferromagnetic order below 5 K and a possible ferroelectric order below 150 K. A multiferroic state with both ferromagnetic and ferroelectric ordering is established, although the ferromagnetic and ferroelectric orders are not coupled. The experimental effective moment and the saturated magnetization for ${\mathrm{Ba}}_{5}{(\mathrm{Os}{\mathrm{O}}_{5})}_{3}\mathrm{Cl}$ are close to the spin-only value, indicating that the spin-orbit coupling does not play an important role, which is due to the large crystal field and spin splitting in ${\mathrm{Ba}}_{5}{(\mathrm{Os}{\mathrm{O}}_{5})}_{3}\mathrm{Cl}$.

Single-crystals of thallium(I) iodide oxide Tl3IO were obtained as by-product in a hydro­flux synthesis at 473 K for 10 h. The oxygen atoms center thallium octa­hedra. The [OTl6] octa­hedra share trans faces, forming a linear chain along [001]. Twelve thallium atoms surround each iodine atom in an [ITl12] anti-cubocta­hedron. Thallium and iodine atoms together form a hexa­gonal close-sphere packing, in which every fourth octa­hedral void is occupied by oxygen., Single-crystals of thallium(I) iodide oxide Tl3IO were obtained as by-product in a hydro­flux synthesis at 473 K for 10 h. A potassium hydroxide hydro­flux with a water-base molar ratio of 1.6 and the starting materials TlNO3, RhI3 and Ba(NO3)2 was used, resulting in a few black needle-shaped crystals. X-ray diffraction on a single-crystal revealed the hexa­gonal space group P63/mmc (No. 194) with lattice parameters a = 7.1512 (3) Å and c = 6.3639 (3) Å. Tl3IO crystallizes as hexa­gonal anti-perovskite (anti-BaNiO3 type) and is thus structurally related to the alkali-metal halide/auride oxides M 3 XO (M = K, Rb, Cs; X = Cl, Br, I, Au). The oxygen atoms center thallium octa­hedra. The [OTl6] octa­hedra share trans faces, forming a linear chain along [001]. Twelve thallium atoms surround each iodine atom in an [ITl12] anti-cubocta­hedron. Thallium and iodine atoms together form a hexa­gonal close-sphere packing, in which every fourth octa­hedral void is occupied by oxygen.

Ionic liquids (ILs) are widely used as versatile solvents for the synthesis of nanomaterials. However, the effect of IL impurities on the formation of nanomaterials is often neglected. Herein, we report on the formation of tellurium (Te) nanoparticles from the reaction of trialkylphosphane tellurides, formed by reactive dissolution of Te in dried commercial trihexyltetradecylphosphonium chloride ([P66614]Cl) at high temperatures, with common polar protic solvents (e.g. water, alcohols, or amides). Highly homogeneous Te nano- and microstructures with various sizes and morphologies including three-dimensional (3D) Te fusiform assemblies and 3D aloe-like Te microarchitectures are obtained. Our investigation shows that trace amounts of HCl impurities in [P66614]Cl tend to remain as [P66614][HCl2] due to the strong interaction with Cl−. The addition of a polar, protic solvent liberates active HCl from the HCl2− anion which we found to play an essential role in the formation of Te particles due to the accelerating effect of P–Te bond cleavage. This approach presents a general and convenient synthetic strategy for the preparation of Te nano- and microstructures.

A new coordination polymer [Hg(LI)I]n (1) and a new discrete coordination complex [Hg(HLII)I2] (2) are synthesized and X-ray characterized. The existence of positive π-holes at the spodium atoms in both compounds is evidenced by DFT calculations. In 1, a Hg-S semicoordination bond and a HgI spodium bond are formed at opposite sides of the π-hole. In 2, two different HgI spodium bonds are formed at both sides of the π-hole. This is the first study describing structure-guiding π-hole spodium bonding.

SnSb alloy, which can be used as an anode in a sodium-ion cell, was synthesized following a resource-efficient route at low temperature. This one-pot approach greatly reduces the energy consumption and maximizes the efficient use of raw materials. The reaction of elemental tin and antimony in the ionic liquid (IL) trihexyltetradecylphosphonium chloride ([P66614]Cl) at 200 °C led to a microcrystalline powder of single-phase SnSb within 10 h with very high yield (95%). Liquid-state nuclear magnetic resonance spectroscopy revealed that the IL remains essentially stable during the reaction. It was recovered almost quantitatively by distilling off the organic solvent used for product separation. Composites of SnSb powder and carbon nanotubes (CNTs) were fabricated by a simple ball milling process. Electrochemical measurements demonstrate that the Na‖SnSb/CNTs cell retains close to 100% of its initial capacity after 50 cycles at a current of 50 mA g−1, which is much better than the Na‖SnSb cell. The greatly increased capacity retainability can be attributed to the conductive network formed by CNTs inside the SnSb/CNTs electrode, providing 3D effective and fast electronic pathways during sodium intercalation and de-intercalation.