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Er5re2c7, Tm5re2c7, and Lu5re2c7 with Sc5re2c7 Type, and Yb2rec2 with Pr2rec2 Type Structures R

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Er5re2c7, Tm5re2c7, and Lu5re2c7 with Sc5re2c7 Type, and Yb2rec2 with Pr2rec2 Type Structures R Er5Re2C7, Tm5Re2C7, and Lu5Re2C7 with Sc5Re2C7 Type, and Yb2ReC2 with Pr2ReC2 Type Structures R. Pöttgen, K. H. Wachtmann, W. Jeitschko*, A. Lang, T. Ebel Anorganisch-Chemisches Institut, Universität Münster Wilhelm-Klemm-Straße 8 , D-48149 Münster, Germany Z. Naturforsch. 52 b, 231-236 (1997); received November 15, 1996 Crystal Structure, Magnetic Properties, Rare Earth Metal Rhenium Carbides, Polymeric Rhenium-Carbon Polyanions ErsReiCy, TmsRe 2C7, and LusReaC? were prepared by arc-melting of the elemental compo­ nents and subsequent annealing at 800 °C. ErsRe^Cy forms only after the annealing process, whereas the other two carbides were already present in the as cast samples. They crystallize with a ScsReiC? type structure, which was refined from single-crystal X-ray data of LusRe 2C7: Cmmm, a = 791.44(5), b = 1418.08(8), c = 332.79(2) pm, Z = 2, R = 0.037 for 544 structure factors and 21 variable parameters. The structure contains linear centrosymmetric C 3 units with a C-C bond length of 133(2) pm and isolated carbon atoms in octahedral coordination of four lutetium and two rhenium atoms. The rhenium atoms within the two-dimensionally infinite polymeric sheets [ReiC-tln are electronically saturated as is indicated by the diamagnetism and the semiconductivity of this carbide. Yf> 2ReC2 was prepared by reacting the elements in a sealed tantalum tube with a high-frequency furnace. It crystallizes with a Pr 2ReC2 type structure: Pnma, a = 645.91(6), b = 498.64(6), and c = 966.05(6) pm. Magnetic susceptibility measurements indicate the ytterbium atoms to be trivalent in this compound. Introduction The isotypic carbides Ln 2ReC2 (Ln = Ce-Nd, Sm, Gd-Tm, and Lu) have been prepared by arc-melting We recently reported on a new series of rare [11]. Because of the high vapor pressure of ytter­ earth metal rhenium carbides of the composition bium, the corresponding ytterbium compound could Ln^ResCis with Ln = Y, La-Nd, Gd-Er [1]. At­ not be prepared that way. We have now obtained tempts to prepare the isotypic carbides with thulium Yb 2ReC2 by reaction of the elemental components and lutetium did not result in La^ResCis type com­ in a sealed tantalum tube. pounds, instead with these heavy rare earth elements we obtained the carbides TmsRe 2C7 and Lu5Re2C7, Sample Preparation and Lattice Constants which crystallize with a ScsRe 2C7 type structure [ 2] The lanthanoids were purchased in the form of ingots and which are reported here. With erbium we syn­ (all with nominal purities > 99.9 %). They were cut into thesized both the La^ResCis and ScsRe 2C7 type small pieces of about 2 mm diameter, and cold-pressed carbides, the latter only after the annealing at 800 to pellets (6 mm diameter) together with the appropriate °C. These are the first ternary carbides of the heavy amounts of rhenium powder (Starck, 400 mesh, > 99.9 %) rare earth elements containing C 3 units. Such propa- and graphite flakes (Ventron, 20-60 mesh, 99.5 %). dienyl units were found only in few other carbides: The pellets were reacted in an arc-melting furnace un­ Ln3C4 (Ln = Sc, Y, Ho-Lu) [3,4], Mg 2C3 [5], Y4C7 der an atmosphere of argon (99.996 %). The argon was [6], the two different modifications of H 04C7 [6, 7], purified by repeatedly melting a titanium sponge in a sepa­ the carbides Ln4C7 (Ln = Er, Tm, Lu) [7], and the rate copper chill prior to the reactions. The molten buttons of the samples were always turned over and remelted sev­ ternary carbide chloride Ca 3C3Cl2 [8]. The struc­ eral times to enhance their homogeneity. The weight loss tures of Sc 3C4 and Ca3C3Cl2 were supported by after several meltings was always less than 1 %. The pel­ extended Hückel calculations [9]. A preliminary ac­ lets were subsequently wrapped in tantalum foil, sealed count of some of the work reported here has been into evacuated silica tubes, and annealed at 800 °C for given at a conference [ 10]. three weeks. A well-crystallized sample of Lu 5Re2C7 was obtained * Reprint requests to W. Jeitschko. by annealing an arc-melted button with a high-frequency 0939-5075/97/200-0231 $ 06.00 (c) 1997 Verlag der Zeitschrift für Naturforschung. All rights reserved. K Dieses Werk wurde im Jahr 2013 vom Verlag Zeitschrift für Naturforschung This work has been digitalized and published in 2013 by Verlag Zeitschrift in Zusammenarbeit mit der Max-Planck-Gesellschaft zur Förderung der für Naturforschung in cooperation with the Max Planck Society for the Wissenschaften e.V. digitalisiert und unter folgender Lizenz veröffentlicht: Advancement of Science under a Creative Commons Attribution Creative Commons Namensnennung 4.0 Lizenz. 4.0 International License. 232 R. Pöttgen et al. • Rare Earth Metal Rhenium Carbides Table I. Lattice constants of the orthorhombic carbides with Sc5Re2C7 type and Pr 2ReC2 type structure. The data for the scandium compound were taken from ref. [2], Standard deviations are given in parentheses throughout the paper. Compound a [pm] b [pm] c [pm] V [nm3] Sc5Re2C7 779.26(7) 1362.0(1) 320.62(3) 0.3403 Er<;Re2C7 792.9(1) 1439.4(2) 338.02(6) 0.3858 Tm5Re2C7 792.02(6) 1430.55(9) 335.94(4) 0.3806 T[K] — LusRe->C7 791.44(5) 1418.08(8) 332.79(2) 0.3735 Fig. 1. Temperature dependence of the inverse magnetic Yb2ReC2 645.91(6) 498.64(6) 966.05(6) 0.3111 susceptibility of Yb2ReC 2 measured with a magnetic flux density of 3 T. furnace in a water-cooled silica tube slightly below the (undetermined) melting point for about six hours. of a ferromagnetic impurity. The susceptibilities For the preparation of Yb 2ReC2 the elements with the have therefore been extrapolated to 1/B = 0. The atomic ratio Yb:Re:C = 3.3:1:2 were sealed into a tan­ X vs. 1/B plots were linear. The thus extrapolated talum tube under argon (800 mbar). They were reacted molar susceptibility was only weakly temperature at high temperature (> 1800 °C) for 5 min in a high- dependent and had a value of -20(±5)-10 -9 m3/mol frequency furnace. Subsequently the upper half of the at room temperature, indicating diamagnetism. tube was pulled out of the induction coil and the excess The magnetic susceptibilities of Yb 2ReC2 were ytterbium was distilled at lower temperature to the cooler also slightly field dependent; however, those mea­ end of the tantalum tube. sured with 3 T were already the same as those ob­ The lattice constants of all compounds (Table I) were served at 5 T and therefore an extrapolation to infi­ obtained by least-squares fits of the Guinier powder nite field-strength was not necessary. The tempera­ data using CuKc*i radiation and a-quartz (a = 491.30, ture dependence obeyed the Curie-Weiss law (Fig. c = 540.46 pm) as an internal standard. To assure proper indexing, the observed patterns were compared with the 1). A magnetic moment of ^exP = 4.5(1) per yt­ calculated ones [ 12] assuming the atomic positions as ob­ terbium atom was obtained from the linear portion tained from the structure refinements of Lu 5Re2C7 and of the \/\ vs. T plot above 70 K. This value is in Er2ReC2 [11], good agreement with the theoretical value /ieff = 4.54 for the free ion value of trivalent ytterbium. Chemical and Physical Properties It is also in agreement with the magnetic proper­ ties of the isotypic carbides Ln 2ReC2 (Ln = Y, Tb, Compact ingots of the carbides are light gray; Dy, Ho, Er, and Lu) where the rhenium atoms do powder samples have dark gray color. Single crys­ not carry magnetic moments [13,14]. The magnetic tals of Lu 5Re2C7 exhibit metallic luster. Together susceptibilities of Yb 2ReC2 do not give any indica­ with the isotypic carbide Sc 5Re2C 7, they are the tion for magnetic order down to 2 K. The negative only carbides containing C 3 units that are stable Weiss constant of G = -22(1) K suggests antiferro­ in air. All other C 3 containing carbides [3 - 8] hy­ magnetic order below 2 K. drolyze readily in the presence of moisture. The The electrical resistivities of small ( ca. 0.3 mm di­ stability of the Sc 5Re2C7 type carbides may be at­ ameter) polycrystalline samples of Lu 5Re2C7, iso­ tributed to the transition metal content of these com­ lated from an arc-melted, annealed, crushed button, pounds. The ingots of Yb 2ReC2 decompose com­ were determined with a four-probe technique [15] pletely in moist air within a few days. between 300 and 5 K. Four copper filaments were Magnetic susceptibilities of Lu 5Re2C7 and glued to the sample using a silver epoxy cement. Yb 2ReC2 were determined with a SQUID magne­ The specific resistivities increased with decreasing tometer (MPMS, Quantum Design) between 2 and temperature for all samples as is typical for semi­ 300 K with magnetic flux densities between 1 and conductors. Activation energies calculated from the 5 T. The susceptibilities of Lu 5Re2C7 were small, steepest portions of the In p vs. 1/T plots (an exam­ slightly temperature and field dependent over the ple is shown in Fig. 2) varied between 0.006 and whole temperature range, indicating a small amount 0.03 eV. These values are very small and therefore R. Pöttgen et al. ■ Rare Earth Metal Rhenium Carbides 233 -— T[K] Table II. Crystal data for LugRe 2C7. 100 50 25 10 Formula mass 1331.33 Space group Cmmm (No. 65) Unit cell dimensions see Table I Formula units per cell Z= 2 Calculated density 11.84 g/cm3 Crystal size 25 x 25 x 50 pm3 Absorption correction from ^-scan data Transmission ratio 1.74 (max:min) 0/26 scans up to 26 = 75° Range in hkl ±16, ±29, ±6 Total no.
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