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Magnesium intermetallics: synthesis and structure of Eu2Pt2Mg and Sr2Pt2Mg

  • Maximilian Kai Reimann and Rainer Pöttgen EMAIL logo
Published/Copyright: June 17, 2021
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Zeitschrift für Naturforschung B
From the journal Zeitschrift für Naturforschung B Volume 76 Issue 6-7

Abstract

The intermetallic phases Sr2Pt2Mg and Eu2Pt2Mg were obtained by reaction of the elements in sealed tantalum tubes at high temperature. Sr2Pt2Mg crystallizes with the monoclinic Ca2Ir2Si type (C2/c, a = 1020.7(7), b = 597.7(4), c = 827.0(4) pm, β = 103.37(5)°), while Eu2Pt2Mg adopts the orthorhombic W2CoB2-type structure (Immm, a = 440.31(5), b = 582.20(6), c = 914.11(9) pm, wR = 0.0359, 277 F2 values, 14 variables). The magnesium atoms in both structures are coordinated by four Pt2 dumb-bells with a rectangular planar coordination in Eu2Pt2Mg (268 pm Pt–Mg) and a distorted tetrahedral one in Sr2Pt2Mg (273–275 pm Pt–Mg). The Pt–Pt distances are 277 pm in the europium and 269 pm in the strontium compound. The polyanionic [Pt2Mg] units are planar in Eu2Pt2Mg and separated by the europium atoms. The Sr2Pt2Mg structure shows the motif of hexagonal rod packing for the [Pt2Mg] rows that are embedded in a strontium matrix. Chemical bonding and the influence of the valence electron count on the formation of the structure types are discussed.

Keywords: crystal structure; intermetallics; magnesium

1 Introduction

The rare earth (RE) transition metal (T) magnesium systems have intensively been studied in recent years with respect to phase analytical work, crystal chemistry and chemical respectively physical properties [1], [2]. Especially the magnetic properties and the hydrogenation behavior of the RExTyMgz compounds have been investigated, when searching for alternative hydrogen storage materials [3].

With exception of europium compounds, all RExTyMgz phases exhibit trivalent rare earth ions. In all EuxTyMgz phases reported so far europium is divalent and the close crystal chemical relationship with the alkaline earth elements calcium and strontium is evident, although, only few examples are known: EuTMg (T = Pd, Ag, Pt, Au) with TiNiSi-type structure [4], [5], [6], Eu4TMg (T = Pd, Pt, Au) with Gd4RhIn-type structure [7], [8], [9], EuTMg2 (T = Rh, Pd, Ag, Ir, Pt, Au) with MgCuAl2 or YSiPd2-type structure [10] and EuCu9Mg2 which adopts an ordered version of CeNi3 [11]. Some of the europium compounds exhibit comparatively high magnetic ordering temperatures. The most striking example is the 150 K ferromagnet Eu4PdMg [9] which shows a reversible, table-like magnetocaloric effect [8].

In continuation of our phase analytical studies we focused on the interplay between the strontium and europium phases. Since Eu2+ (117 pm) and Sr2+ (118 pm) have similar ionic radii for coordination number 6 [12], many isotypic series exist, e. g. the SrTMg [13]/EuTMg [4], [5], [6] and SrTMg2 [14]/EuTMg2 [10] pairs.

We have now obtained the pair Eu2Pt2Mg/Sr2Pt2Mg. Both compounds surprisingly crystallize with different structure types. Their synthesis and structural characterization are reported herein.

2 Experimental

2.1 Synthesis

Europium ingots (American Elements, 99.99%), dendritic pieces of strontium (Onyxmet, 99.95%), platinum powder (Agosi, 99.9%) and magnesium shavings (Alfa Aesar, 99.8%) were used as starting materials for the synthesis of Sr2Pt2Mg and Eu2Pt2Mg. The moisture sensitive europium and strontium pieces were first cleaned from surface contaminations under dry cyclohexane (over sodium) and cut into small pieces. These pieces were stored in Schlenk tubes prior to the reactions under an atmosphere of 800 mbar dried argon (titanium sponge; T = 873 K), molecular sieve and silica gel. The elements were then weighed in the ideal stoichiometric ratio into tantalum ampoules which were arc-welded [15] under an argon atmosphere of ca. 800 mbar. These ampoules were sealed in evacuated quartz tubes (oxidation protection) and placed inside a muffle furnace.

Similar to the synthesis of Ca2Pt2Mg [16], the samples were heated to 1200 K within 3 h and kept at this temperature for 2 h. The temperature was then slowly reduced to 1140 K over 10 hours to be kept there for another 60 h. The samples were finally cooled to room temperature within 12 h. The polycrystalline samples were separated mechanically from the tantalum ampoules. No reaction with the crucible material was evident. Both samples were very sensitive to moisture and were therefore transferred into Schlenk tubes immediately after the synthesis.

2.2 X-ray diffraction

The Sr2Pt2Mg and Eu2Pt2Mg samples were studied by powder X-ray diffraction (Guinier technique, Enraf-Nonius FR552 camera, CuKα1 radiation, imaging plate detector, Fujifilm BAS-1800). α-Quartz (a = 491.30, c = 540.46 pm) was taken as an internal standard. The lattice parameters (Table 1) were refined from the experimental 2θ values. The indexing of the complex patterns was facilitated by comparison with calculated ones using the LazyPulverix routine [20]. The powder data of Eu2Pt2Mg agree with those determined for the single crystal (Table 2). The pattern of the Eu2Pt2Mg sample is shown as an example in Figure 1.

Table 1:

Lattice parameters (powder data) of Sr2Pt2Mg, Sr2Pt2In, Eu2Pt2Mg, Eu2Pt2Ga and Eu2Pt2In. Standard deviations are given in parentheses.

CompoundStructure typea (pm)b (pm)c (pm)β (deg)V (nm3)Reference
Sr2Pt2MgCa2Ir2Si1020.7(7)597.7(4)827.0(4)103.37(5)0.4909This work
Sr2Pt2InCa2Ir2Si1026.8(2)599.0(1)830.3(2)103.17(1)0.4973[17]
Eu2Pt2MgW2CoB2440.16(9)580.9(1)913.5(2)900.2336This work
Eu2Pt2GaCa2Ir2Si987.75(6)586.21(6)796.77(5)102.257(4)0.4508[18]
Eu2Pt2InCa2Ir2Si1017.2(2)588.7(1)826.5(1)103.76(1)0.4807[19]
Table 2:

Crystal data and structure refinement parameters for the compound Eu2Pt2.043(4)Mg0.957(4), space group Immm, Z = 2.

Refined formulaEu2Pt2.043(4)Mg0.957(4)
Formula weight, g mol−1725.7
Lattice parameters (single-crystal data)
a, pm440.31(5)
b, pm582.20(6)
c, pm914.11(9)
Unit cell volume V, nm30.2343
Calculated density, g cm−310.29
Crystal size, µm345 × 45 × 65
Transmission (min/max)0.089/0.237
Detector distance, mm40
Exposure time, s1800
ω range/increment, deg0–180/1
Integr. parameters (A/B/EMS)14.0/−4.0/0.010
Abs. coefficient, mm−187.1
F(000), e594
θ range, deg4.15–33.28
Range in hkl±6/±8/±14
Total no. reflections1334
Independent reflections/Rint277/0.0222
Reflections with I > 3 σ(I)/Rσ268/0.0058
Data/parameters277/14
Goodness-of-fit on F21.43
R/wR for I > 3 σ(I)0.0153/0.0356
R/wR for all data0.0161/0.0359
Extinction coefficient247(11)
Largest diff. peak/hole, e Å−3+1.58/−1.77
Figure 1: Experimental and calculated Guinier powder pattern (CuKα1 radiation) of Eu2Pt2Mg. Reflections marked with asterisks correspond to the by-product EuPtMg [6].
Figure 1:

Experimental and calculated Guinier powder pattern (CuKα1 radiation) of Eu2Pt2Mg. Reflections marked with asterisks correspond to the by-product EuPtMg [6].

A piece of the Eu2Pt2Mg sample was carefully crushed under Paratone® oil. Irregularly shaped crystal splinters were isolated and glued to quartz fibres using beeswax. The mounted crystals were then additionally coated with Paratone®. The crystal quality was tested on a Buerger camera (white Mo radiation) and a complete intensity data set of a suitable specimen was collected on a STOE IPDS-II diffractometer (graphite-monochromatized MoKα radiation; oscillation mode). A numerical absorption correction was applied to the data set. Details of the data collection, the crystallographic parameters and the refinement are summarized in Table 2.

2.3 Structure refinement

The Eu2Pt2Mg data set showed a body-centred orthorhombic lattice and no further extinctions. The centrosymmetric space group Immm was found to be correct and isotypy with Ca2Pt2Mg [16] and Ca2Pd2Cd [21] (both W2CoB2 type [22]) was already evident from the Guinier powder diffraction data. The starting atomic parameters were deduced with the charge flipping algorithm (program Superflip [23]) and the Eu2Pt2Mg structure was refined by least squares on F2 using the program Jana2006 [24], [25] with anisotropic displacement parameters for all atoms. The occupancy parameters of all Wyckoff sites were carefully refined in order to check for deviations from the ideal composition. The europium and platinum sites were fully occupied within three standard deviations, while higher electron density was observed for the 2a magnesium site. We have then refined this sites with a small degree of magnesium/platinum mixing, leading to the composition Eu2Pt2.043(4)Mg0.957(4) for the investigated crystal. The final difference Fourier synthesis revealed no significant residual peaks. The atomic positions, displacement parameters, and interatomic distances are given in Tables 3 and 4.

Table 3:

Wyckoff sites, atomic coordinates and anisotropic displacement parameters in pm2 for Eu2Pt2.043(4)Mg0.957(4). The anisotropic displacement factor exponent takes the form: –2π2[(ha*)2U11 + … + 2hka*b*U12]. Ueq is defined as a third of the trace of the orthogonalized Uij tensor. U12 = U23 = U13 = 0.

AtomsitexyzU11U22U33Ueq
Eu4j1/200.30151(4)179(2)198(2)168(2)182(1)
Pt14h00.23780(5)1/2158(2)178(2)179(2)172(1)
0.957(4)Mg/0.043(4)Pt22a000142(16)133(14)216(15)164(9)
Table 4:

Interatomic distances in the structure of Eu2Pt2.043(4)Mg0.957(4) given in pm. All standard deviations are less or equal to 0.2 pm.

Eu:2Pt1315.1
4Pt1317.1
2Mg1/Pt2343.0
2Mg1/Pt2352.7
1Eu362.9
4Eu376.9
Pt1:2Mg1/Pt2267.9
1Pt1276.9
1Pt1305.3
2Eu315.1
4Eu317.1
Mg/Pt2:4Pt1267.9
4Eu343.0
4Eu352.7

CCDC 2086275 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.

2.4 EDX data

The Eu2Pt2Mg single crystal was additionally analysed by EDX using a Zeiss EVO® MA10 scanning electron microscope (variable pressure mode (60 Pa); EuF3, Pt and MgO as standards). The point analyses (35 ± 3 at% Eu: 44 ± 3 at% Pt: 21 ± 2 at% Mg) is close to the composition refined from the X-ray data (40: 40.8: 19.2). A more precise measurement was hampered by the Paratone® coating of the highly moisture sensitive crystal. No impurity elements (especially with respect to the tantalum containers) were observed.

3 Crystal chemistry

Sr2Pt2Mg and Eu2Pt2Mg are new representatives of the large family of AE2T2X and RE2T2X intermetallics (AE = alkaline earth metal). The wide majority (>600 entries in the Pearson data base) of these phases (mostly with a trivalent rare earth element) crystallize with the well-known tetragonal Mo2B2Fe-type structure, a ternary ordered version of U3Si2 [1], [26]. The other important structure types for this general composition are W2CoB2 (>160 entries), Mn2AlB2 (>70 entries) and Ca2Ir2Si (16 entries) [1].

We start our crystal chemical discussion with Eu2Pt2Mg. A projection of the Eu2Pt2Mg structure along the short unit cell axis is presented in Figure 2. The platinum atoms have slightly distorted trigonal prismatic coordination by four europium and two magnesium atoms. These Pt@Eu4Mg2 prisms are alternatingly condensed in b direction via edges and via the triangular faces in a direction, forming layers. Adjacent layers are shifted by half the translation period a.

Figure 2: Projection of the Eu2Pt2Mg structure onto the crystallographic bc plane. Europium, platinum and magnesium atoms are drawn as medium grey, blue and magenta circles, respectively. The trigonal prismatic coordination of the platinum atoms is emphasized. Adjacent building units are shifted by half the translation period a, emphasized by thin and thick lines.
Figure 2:

Projection of the Eu2Pt2Mg structure onto the crystallographic bc plane. Europium, platinum and magnesium atoms are drawn as medium grey, blue and magenta circles, respectively. The trigonal prismatic coordination of the platinum atoms is emphasized. Adjacent building units are shifted by half the translation period a, emphasized by thin and thick lines.

Apart from this geometrical description we now turn to the [Pt2Mg] network (Figure 3). The platinum and magnesium atoms all lie on mirror planes at z = 0 and z = 1/2, shifted by 1/2 1/2 1/2 (body-centered lattice). The magnesium atoms have rectangular planar coordination by four Pt2 dumb-bells with Mg–Pt distances of 268 pm. These distances are close to the sum of the covalent radii [27] of 265 pm for Mg + Pt and comparable to data for EuPtMg (276–288 pm) [6] and EuPtMg2 (275–278 pm) [10]. This is compatible with covalent Mg–Pt bonding within the [Pt2Mg] networks. The Pt–Pt distances within the Pt2 dumb-bells of 277 pm compare well with the Pt–Pt distances (12×) of 277 pm in fcc platinum [28]. Isotypic Ca2Pt2Mg (272 pm) and Ca2Pt2Ag (264 pm) [16] have even shorter Pt–Pt distances, most likely due to the much smaller size of the calcium matrix. Crystal Orbital Hamilton Population analysis for Ca2Pt2Mg [16] revealed the highest values for the Pt–Pt interactions followed by Pt–Mg, strongly underlining the bonding picture of a covalently bonded [Pt2Mg]δ– polyanionic network. Within a rigid band model, this picture of chemical bonding can safely be applied to Eu2Pt2Mg studied herein. The [Pt2Mg]δ– polyanions are separated by puckered layers of europium cations. It is not surprising, that, as a consequence of the lower and higher electronegativity of europium and platinum, each europium atom has six nearest platinum neighbors at 315–317 pm.

Figure 3: (left) The unit cell of Eu2Pt2Mg projected onto the bc plane. Europium, platinum and magnesium atoms are drawn as medium grey, blue and magenta circles, respectively. The [Pt2Mg] polyanionic networks extend in ab direction. (right) Projection of one [Pt2Mg] layer with adjacent europium atoms along the c axis.
Figure 3:

(left) The unit cell of Eu2Pt2Mg projected onto the bc plane. Europium, platinum and magnesium atoms are drawn as medium grey, blue and magenta circles, respectively. The [Pt2Mg] polyanionic networks extend in ab direction. (right) Projection of one [Pt2Mg] layer with adjacent europium atoms along the c axis.

A final issue observed for the europium compound is the small degree of Mg/Pt mixing on the 2a Wyckoff site with a refined composition Eu2Pt2.043(4)Mg0.957(4) for the investigated crystal. The W2CoB2 type [22] is a ternary ordered version of K2Au3 [29]. In the case of Eu2Pt2Mg, europium fills the potassium position, while platinum and magnesium are ordered on the two crystallographically independent gold sites 2a and 4h. This readily explains a small homogeneity range Eu2Pt2+xMg1–x, however a binary compound ‘Eu2Pt3’ is not known. Such a small homogeneity range has also been observed for isotypic Ca2Pt2+xAg1–x (x = 0.031(3)–0.047(3)) [16].

Chemical bonding in different alkaline earth based W2CoB2-type phases was intensively studied in recent years in order to elucidate the stability criteria for this type in concurrence to other types like Ca2Pd2Ge (Fdd2) and Ca2Ir2Si (C2/c) [16], [30], [31]. These studies indicated that the valence electron count (VEC) is one of the main reasons which decides for a given structure type. Selected compounds (including the recently reported stannide Eu2Pd2Sn [32]) are compiled in Figure 4. The VEC shows a small range from VEC = 26 to VEC = 28. The similar ionic radii for coordination number 6 [12] for Eu2+ (117 pm) and Sr2+ (118 pm) suggest that an isotypic strontium compound might exist. Our phase analytical studies indeed resulted in the new phase Sr2Pt2Mg. The latter, however, adopts the monoclinic Ca2Ir2Si type [33]. Also the prototype itself is an exception as well as Sr2Pd2Al [31] with VEC = 27 and Ca2Pt2Ge [30] with VEC = 28. Thus also small differences in size or electronegativity play an important role.

Figure 4: Valence electron count (VEC) of selected alkaline earth and europium compounds [1] with W2CoB2 (blue, space group Immm), Ca2Ir2Si (red, space group C2/c) and Ca2Pd2Ge-type structure (green, space group Fdd2). For details see text.
Figure 4:

Valence electron count (VEC) of selected alkaline earth and europium compounds [1] with W2CoB2 (blue, space group Immm), Ca2Ir2Si (red, space group C2/c) and Ca2Pd2Ge-type structure (green, space group Fdd2). For details see text.

So far we did not obtain single crystals of Sr2Pt2Mg and our samples contained a small amount of a yet unknown by-product. In Figure 5 we present a drawing of the Sr2Pt2Mg structure using the refined lattice parameters (Table 1) and the positional parameters of isotypic Sr2Pt2In [17]. The platinum and magnesium atoms also form Pt2Mg2 rhombs; however, within one row they are twisted with respect to each other, leading to a distorted tetrahedral coordination for the magnesium atoms. The Pt–Mg distances of 273 and 275 pm are comparable to those in Eu2Pt2Mg. The bonding to adjacent rows also proceeds via Pt–Pt contacts (269 pm). Topologically one can describe the Sr2Pt2Mg structure as a hexagonal rod packing of the rows of [Pt2Mg] anions that are embedded within a matrix of strontium cations.

Figure 5: The crystal structure of Sr2Pt2Mg drawn with the positional parameters of Sr2Pt2In [17]. Strontium, platinum and magnesium atoms are drawn as medium grey, blue and magenta circles, respectively. The rod packing motif of the [Pt2Mg] rows is emphasized in the drawing on the left. A cutout of the condensed [Pt2Mg] rows is shown at the right. Relevant interatomic distances are given in units of pm.
Figure 5:

The crystal structure of Sr2Pt2Mg drawn with the positional parameters of Sr2Pt2In [17]. Strontium, platinum and magnesium atoms are drawn as medium grey, blue and magenta circles, respectively. The rod packing motif of the [Pt2Mg] rows is emphasized in the drawing on the left. A cutout of the condensed [Pt2Mg] rows is shown at the right. Relevant interatomic distances are given in units of pm.

Corresponding author: Rainer Pöttgen, Institut für Anorganische und Analytische Chemie, Universität Münster, Corrensstrasse 30, 48149Münster, Germany, E-mail:

Acknowledgements

We thank Dipl.-Ing. J. Kösters for the single-crystal data collection.

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: None declared.

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2021-05-25
Accepted: 2021-06-07
Published Online: 2021-06-17
Published in Print: 2021-07-27

© 2021 Walter de Gruyter GmbH, Berlin/Boston

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  9. Crystal structure and physical properties of a new two-dimensional zinc coordination polymer based on 1,4-bis(4-(imidazole-1-yl)benzyl)piperazine and benzophenone-2,4′-dicarboxylate ligands
  10. A new N-oxide benzylisoquinoline alkaloid isolated from the leaves of atemoya (Annona cherimola × Annona squamosa)
  11. One-pot synthesis of 1-(benzothiazolylamino)aryl methyl-2-naphthols and 3-benzothiazolyl 2,3-dihydroquinazolinones using a magnetically recoverable core–shell nanocomposite as catalyst
  12. An efficient click synthesis of chalcones derivatized with two 1-(2-quinolon-4-yl)-1,2,3-triazoles
  13. Facile decoration of CdS nanoparticles on TiO2: robust photocatalytic activity under LED illumination
  14. Book Review
  15. A. Sigel, E. Freisinger and R. K. O. Sigel (Editors and Series Editors): Metal Ions in Bio-Imaging Techniques: Volume 22 of the series Metal Ions in Life Sciences
https://doi.org/10.1515/znb-2021-0069
Keywords for this article
crystal structure; intermetallics; magnesium

Articles in the same Issue

  1. Frontmatter
  2. In this issue
  3. Research Articles
  4. Synthesis and structure of the λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6]
  5. Approximate estimation of the critical diameter in Koenen tests
  6. Laves phases forming in the system ScCo2-“InCo2”-TaCo2
  7. Magnesium intermetallics: synthesis and structure of Eu2Pt2Mg and Sr2Pt2Mg
  8. Intermetallic phases in the Sc–Ir–In system – synthesis and structure of Sc1.024Ir2In0.976 and Sc3Ir1.467In4
  9. Crystal structure and physical properties of a new two-dimensional zinc coordination polymer based on 1,4-bis(4-(imidazole-1-yl)benzyl)piperazine and benzophenone-2,4′-dicarboxylate ligands
  10. A new N-oxide benzylisoquinoline alkaloid isolated from the leaves of atemoya (Annona cherimola × Annona squamosa)
  11. One-pot synthesis of 1-(benzothiazolylamino)aryl methyl-2-naphthols and 3-benzothiazolyl 2,3-dihydroquinazolinones using a magnetically recoverable core–shell nanocomposite as catalyst
  12. An efficient click synthesis of chalcones derivatized with two 1-(2-quinolon-4-yl)-1,2,3-triazoles
  13. Facile decoration of CdS nanoparticles on TiO2: robust photocatalytic activity under LED illumination
  14. Book Review
  15. A. Sigel, E. Freisinger and R. K. O. Sigel (Editors and Series Editors): Metal Ions in Bio-Imaging Techniques: Volume 22 of the series Metal Ions in Life Sciences
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