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Lithium Alkaline Earth Tetrelides of the Type Li Aett (Ae = Ca, Ba, Tt = Si

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Lithium Alkaline Earth Tetrelides of the Type Li Aett (Ae = Ca, Ba, Tt = Si Z. Naturforsch. 2017; 72(11)b: 847–853 Dominik Stoiber, Matej Bobnar, Peter Höhn and Rainer Niewa* Lithium alkaline earth tetrelides of the type Li2AeTt (Ae = Ca, Ba, Tt = Si, Ge, Sn, Pb): synthesis, crystal structures and physical properties https://doi.org/10.1515/znb-2017-0103 Heusler-type (MnCu2Al) structure with occupancy of octa- Received June 28, 2017; accepted July 20, 2017 hedral holes by Li and mixed Li/Mg occupancy in tetrahe- dral holes of the fcc packing of Tt. More recently, Li MgSi Abstract: Single crystals of the compounds Li AeTt 2 2 was reported [3, 4] with ordered lithium and magnesium (Ae = Ca, Ba, Tt = Si, Ge, Sn, Pb) were grown in reactive arrangements leading to lower crystallographic symmetry. lithium melts in sealed tantalum ampoules from an equi- One model comprises a 2 × 2 × 2 superstructure, the second molar ratio of the alkaline earth metal and the respective a more complicated order. The compounds Li CaSn and group 4 element. All compounds, with the exception of 2 Li CaPb also exhibit a Heusler-type crystal structure, but Li CaSn and Li CaPb, are isotypic and crystallize in an 2 2 2 in contrast to the Mg containing phases with an ordered orthorhombic unit cell (space group Pmmn, no. 59). The arrangement of fully occupied sites with Li in tetrahedral crystal structure can be characterized as superimposed and Ca in octahedral coordination by Tt, due to the larger corrugated networks of Li Tt connected by calcium or 2 difference in ionic radii compared to the magnesium com- barium atoms within the third dimension. Li CaSn and 2 pounds. A similar trend is observed, for example, in α- Li CaPb crystallize in the cubic space group Fm3m̅ (no. 2 LiMgN (disordered) [5], β-LiMgN (ordered) [5] and LiCaN 225) in a Heusler-type (MnCu Al) structure. According to 2 (ordered) [6], although in fluorite-type arrangements. Of magnetic susceptibility and electric resistivity measure- the analogous tetrel compounds with other alkaline earth ments, the compounds Li BaGe, Li BaSn, and Li BaPb rep- 2 2 2 metals only Li BaSi [7] has been known for about half resent diamagnetic activated semiconductors. 2 a century, while to the best of our knowledge no other Keywords: crystal structure determination; Heusler element combinations have been reported. Li2KAs [8] was phases; semiconductors; tetrelides. reported to have the same moisture sensitivity and silver metallic luster as the new compounds Li2CaTt (Tt = Si, Ge) and Li BaTt (Tt = Ge, Sn, Pb) reported in this work, which Dedicated to: Professor Dietrich Gudat on the occasion of his 60th 2 birthday. are all isotypic to Li2BaSi. 2 Experimental 1 Introduction The syntheses of the title compounds were carried out in Ternary compounds Li2MgTt (Tt = Si, Ge, Sn, Pb) [1, 2] are tantalum ampoules by reacting equimolar amounts of the known and the silicon containing compound has been alkaline earth metal and the group 4 element in an excess studied in the course of the ever increasing demand for of lithium, which served as reactant and flux. Single crys- new materials with emphasis on hydrogen storage [3] and tals of up to 4 mm length (Fig. 1) were obtained by heating lithium ion conductivity [4] for usage as electrode mate- the reaction mixture to 800°C, subsequent slow cooling to rial. All above compounds were reported to crystallize in a 400°C with 2 K h−1 and followed by cooling to room tem- perature. Dissolution of the excess lithium was carried out by extraction with liquid ammonia. An alternative *Corresponding author: Rainer Niewa, Institut für Anorganische route using the same starting materials but employing Chemie, Universität Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart, HCTAF (high temperature centrifugation aided filtration, Germany, Tel: +49(0)711/685-64217, −1 Tmax = 750°C, ΔT = 1 K h , Tcent = 300°C) [9] led to single E-mail: [email protected] crystals of similar size in single-phase samples for all Ba Dominik Stoiber: Institut für Anorganische Chemie, Universität Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart, Germany phases. Phase-pure single crystalline samples can gen- Matej Bobnar and Peter Höhn: Max-Planck-Institut für Chemische erally be obtained according to powder X-ray diffraction Physik fester Stoffe, Nöthnitzer Str. 40, 01187 Dresden, Germany (Fig. 2). 848 D. Stoiber et al.: Li2AeTt: synthesis, crystal structures and physical properties X-Shape program followed by a crystal structure refine- ment with the Shelx software [10]. Further details of the crystal structure investiga- tions may be obtained from FIZ Karlsruhe, 76344 Eggen- stein-Leopoldshafen, Germany (fax: +49-7247-808-666; e-mail: [email protected]) on quoting the depo- sition numbers CSD-433265, CSD-433266, CSD-433267, CSD-433268, CSD-433269, CSD-433270, CSD-433271 and CSD-433272. The resistivities of polycrystalline agglomerates of 3 3 Li2BaSn (1.2 × 4.2 × 1.3 mm ) and Li2BaPb (0.6 × 0.8 × 1 mm ) were measured with a home-built resistivity equipment, which allows for the samples to be handled in an inert atmosphere. The samples were contacted using Ag paint and 25 μm thick Pt wires. The magnetic susceptibilities of Li2BaGe, Li2BaSn, and Fig. 1: Needle-like single crystals of Li2BaGe with mm-scale below. Li2BaPb were measured on a SQUID magnetometer (MPMS- XL7, Quantum Design) in the external fields of μ0H = 3.5 and 7 T using gel capsules as containers for the samples. Powder X-ray diffraction measurements were carried out at room temperature on a Stoe Stadi-p diffractometer with MoKα1 radiation and a Ge(111) monochromator using the STOE sample holders and geometry. The data collec- 3 Results and discussion tion was performed with a Mythen 1 K detector in a 2θ range of 5–50°. X-ray diffraction intensity data of single 3.1 Crystal structure description crystals sealed in glass capillaries were collected at room temperature on a Bruker κ-CCD single crystal diffracto- The isotypes Li2AeTt (Ae = Ca, Tt = Si, Ge, and Ae = Ba, meter using MoKα1 radiation with a maximum 2ϑ of 55°. Tt = Si, Ge, Sn, Pb) crystallize in the orthorhombic space A numerical absorption correction was applied using the group Pmmn (no. 59), while Li2CaSn and Li2CaPb realize Fig. 2: Measured (blue) and simulated (red) powder patterns of a ground single crystalline sample of Li2BaSi. D. Stoiber et al.: Li2AeTt: synthesis, crystal structures and physical properties 849 via edges into two-dimensional slabs, in which the group 4 element occupies the extreme positions of the corruga- tion (Fig. 4, middle). The slabs are superimposed along the c-axis. The Ca and Ba atoms are located in between the slabs and coordinated by the group 4 element in form of a distorted tetrahedron. As a result, the group 4 element is surrounded by six lithium ions in one hemisphere and Scheme 1: Overview of the different crystal structures of com- four barium ions in the other, resulting in a ten-fold coor- pounds Li AeTt (Ae = Mg, Ca, Ba, Tt = Si, Ge, Sn, Pb). 2 dination (Fig. 4, right). Remarkably, comparing the unit cell parameters of the a cubic Heusler-type arrangement in Fm3m̅ (no. 225). two silicon or germanium compounds (Tables 1 and 2), the A graphical representation of this situation in relation b and c axes remain almost constant and only the a axis is to the respective magnesium compounds can be found significantly altered. The two-dimensional lithium-tetrel in Scheme 1. Upon changing the alkaline earth metal to network is rigid along the b axis but, due to the sinusoidal strontium a different composition appears, which we corrugation, flexible along the a axis. The shorter wave- will report in an independent contribution. Crystallo- length of the corrugated net leads to a larger amplitude, graphic data of the title compounds are summarized in which should result in an increase of the c axis. However, Tables 1 and 2, atomic positions in Tables 3 and 4. The this is compensated by the smaller ionic radius of calcium orthorhombic Li2BaSi-type compounds can be obtained in compared to barium. Fig. 3 illustrates the situation: the single-phase as needle-like crystals with length of several angle α shows that the corrugated network of lithium and mm (see Figs. 1 and 2). The crystal structures of these the tetrel in the crystal structure is merely compressed/ compounds are composed of slabs of a corrugated two- expanded along the a axis for the barium (α = 89.74°) com- dimensional network formed by lithium and the group pared to the calcium (α = 73.79°) compound. 4 element. Calcium or barium, respectively, are incorpo- Upon comparison of the unit cell parameters of the rated between these slabs (Fig. 3). Lithium is triangularly silicon with the germanium compound and the tin with coordinated by the group 4 element and located slightly the lead compound an only conspicuously minor change out of plane (Fig. 4, left). These triangles are connected strikes the eye. This indicates that the elements that differ Table 1: Selected crystal structure data and results from structure determination of Li2CaTt (Tt = Si, Ge, Sn, Pb). Compound Li2CaSi Li2CaGe Li2CaSn Li2CaPb Crystal system Orthorhombic Cubic Space group Pmmn Fm3m̅ Unit cell parameters a/Å 5.7495(3) 5.7743(4) 6.9352(4) 6.9835(4) b/Å 4.6236(3) 4.6498(3) a a c/Å 6.3432(4) 6.3683(4) a a V/Å3 168.62(2) 170.98(2) 333.56(3) 340.58(3) Z 2 4 −3 Dx/g · cm 1.62 2.46 3.44 5.09 Absorption correction Numerical μ/mm−1 1.9 10.1 8.9 50.8 F(000)/e− 80 116 304 432 2θmax/deg 55.70 55.55 54.56 54.15 h, k, l range −7:7, −6:6, −8:8 −6:5, −7:7, −8:8 −8:8, −8:8, −8:8 −8:8, −8:7, −8:8 Refl.
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