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Crystal structure of Eu2Pd3.37(1)Zn13.63(1)

  • Steffen Klenner , Theresa Block and Rainer Pöttgen ORCID logo EMAIL logo
Published/Copyright: March 21, 2023
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Zeitschrift für Kristallographie - New Crystal Structures
From the journal Zeitschrift für Kristallographie - New Crystal Structures Volume 238 Issue 3

Abstract

Eu2Pd3.37Zn13.63, trigonal, R 3 ‾ m (no. 166), a = 9.1693(7) Å, c = 13.2443(13) Å, V = 964.34(14) Å3, Z = 3, Rgt (F) = 0.0268, wR ref(F 2) = 0.0287, T = 293 K.

CCDC no.: 2247512

Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Projection of the Eu2Pd3.37Zn13.63 structure onto the xy plane (right). Europium, palladium and zinc atoms are drawn as medium grey, blue and magenta circles, respectively. Mixed occupied sites are indicated by segments. A cutout with one row of condensed Eu@(Pd/Zn)19 polyhedra is shown left.

Projection of the Eu2Pd3.37Zn13.63 structure onto the xy plane (right). Europium, palladium and zinc atoms are drawn as medium grey, blue and magenta circles, respectively. Mixed occupied sites are indicated by segments. A cutout with one row of condensed Eu@(Pd/Zn)19 polyhedra is shown left.

Table 1:

Data collection and handling.

Crystal: Grey block
Size: 0.030 × 0.040 × 0.075 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 39.0 mm−1
Diffractometer, scan mode: IPDS Stoe, ω scans
θ max, completeness: 33.3°, >99%
N(hkl)measured, N(hkl)unique, R int: 9175, 488, 0.037
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 417
N(param)refined: 26
Programs: X-Area [1], JANA2006 [2], SUPERFLIP [3, 4]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

Atom x Y z U iso*/U eq
Eu1 0 0 0.34506(2) 0.01304(7)
Pd1a 0.5 0 0.5 0.01283(13)
Zn1b 0.5 0 0.5 0.01283(13)
Zn2c 0.50154(2) 0.49846(2) 0.15132(4) 0.01548(15)
Pd2d 0.50154(2) 0.49846(2) 0.15132(4) 0.01548(15)
Zn3 0.29377(5) 0 0 0.01484(12)
Zn4 0 0 0.10343(5) 0.01629(16)

  1. aOccupancy: 0.917(10), bOccupancy: 0.083(10), cOccupancy: 0.897(8), dOccupancy: 0.103(8).

Source of material

Crystals of the title compound Eu2Pd3.37Zn13.63 were obtained by induction melting of the elements (3:4:12 atomic ratio) in a sealed tantalum ampoule in a water-cooled sample chamber. Starting materials were europium ingots (American Elements, 99.99%), palladium sheets (Agosi, 99.99%) and zinc granules (99.9%, Merck). The sample was first heated to 1473 K, kept for 5 min and quenched. The ampoule was then sealed in an evacuated silica tube, heated to 1223 K with a heating rate of 100 K h−1. The sample was kept at 1223 K for 24 h followed by slow cooling (1 K h−1) to room temperature. Eu2Pd3.37Zn13.63 is light grey with metallic luster and stable in air.

Experimental details

The Eu2Pd3.37Zn13.63 crystals were selected from the mechanically fragmented sample of the nominal composition 3Eu:4Pd:12Zn. The crystal quality was first tested through Laue photographs (Buerger camera, image plate detection system). Single crystal X-ray diffraction was performed at room temperature on a Stoe IPDS–II diffractometer (graphite monochromatized MoKα radiation; oscillation mode). A numerical absorption correction was applied. The starting atomic parameters were deduced with the charge-flipping algorithm [3] implemented in Superflip [4] and the structure was refined on F 2 with the Jana2006 software package [2], with anisotropic displacement parameters for all atoms. Separate refinement of the occupancy parameters indicated small degrees of Pd/Zn mixing for the 9d and 18h sites, which were refined as least-squares variables in the final cycles. The Eu2Pd3.37Zn13.63 crystal is a reverse/obverse twin with a domain ratio of 0.971(4):0.029(4).

Comment

Eu2Pd3.37Zn13.63 crystallizes with the Th2Zn17 type structure [5], space group R 3 ‾ m and completes the series of RE 2Pd3−x Zn14+x compounds [6]. Comparison with the RE 2Pd3−x Zn14+x phases reveals two peculiarities: (i) the solid solution of the europium compound tends towards higher palladium content and (ii) the cell volume is larger than that of the lanthanum representative, indicating divalent europium. The Th2Zn17 type structure has four crystallographically independent zinc sites and allows for different coloring variants (Table 3). Typical binary examples are Ce2Fe17 [7], Zr2Be17 [8] or Ba2Mg17 [9]. Ternary ordered variants have been observed for Ce2Co15Al2 [7] and Gd2Co3Zn14 [6]. Eu2Pd3.37Zn13.63 is close to the latter ordering variant, however, the 9d and 18h sites still show small degrees of Pd/Zn and Zn/Pd mixing, respectively. Such small homogeneity ranges have been observed for most of the many ternary Th2Zn17 type representatives [10]. The europium atoms in the Eu2Pd3.37Zn13.63 structure have the coordination number 19 by palladium and zinc. These Eu@(Pd/Zn)19 polyhedra are condensed via common hexagon faces and these double units are stacked in ABC sequence (rhombohedral space group symmetry). The coordination polyhedron around europium is a slightly distorted hexa-capped hexagonal prisms with an additional Zn3 atom. This coordination reminds of the CaCu5 type [11], one of the basic binary intermetallic structure types. Indeed, the Th2Zn17 type derives from the CaCu5 structure [12] by an ordered replacement of 2/3 of the calcium atoms by europium and of 1/3 by a Zn32 dumb-bell while the remaining palladium and zinc atoms replace the copper atoms. The Zn32 dumb-bells are emphasized in the figure between adjacent Eu@(Pd/Zn)19 polyhedra. The Zn3–Zn3 distances of 274 pm are close to the Zn–Zn distances in hcp zinc (six times 266 and six times 291 pm) [13]. The Pd–Zn distances within the three-dimensional [Pd3.37Zn13.63] network of Eu2Pd3.37Zn13.63 range from 260 to 278 pm, which is slightly longer than the sum of the covalent radii [14] of 253 pm for Pd + Zn. This is similar to the series of dimorphic equiatomic REPdZn phases [15].

Table 3:

Examples of coloring variants for Th2Zn17 type representatives (space group R 3 ‾ m , Pearson code hR57 and Wyckoff sequence hfdc2).

Compound 6c 6c 9d 18f 18h Ref.
Th2Zn17 Th Zn Zn Zn Zn [5]
Ce2Fe17 Ce Fe Fe Fe Fe [7]
Zr2Be17 Zr Be Be Be Be [8]
Ba2Mg17 Ba Mg Mg Mg Mg [9]
Ce2Co15Al2 Ce Al Co Co Co [7]
Gd2Co3Zn14 Gd Zn Co Zn Zn [6]
Corresponding author: Rainer Pöttgen, Institut für Anorganische und Analytische Chemie, Universität Münster, Corrensstrasse 30, 48149 Münster, Germany, E-mail:

Acknowledgements

We thank Dipl.–Ing. J. Kösters for the intensity data collection.

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

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

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Received: 2023-02-24
Accepted: 2023-03-09
Published Online: 2023-03-21
Published in Print: 2023-06-27

© 2023 the author(s), published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  17. Crystal structure of cyclo-(bis(µ2-3,3′-(1H-imidazole-3-ium-1,3-diyl)dipropionato-κ4 O,O′:O″,O″′)-dinitrato-κ2 O,O′-tetraoxido-diuranium(VI) C18H22N6O18U2
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  24. Crystal structure of tetrapropylammonium guanidinium 4,4′-sulfonyldibenzoate monohydrate, C27H44N4O7S
  25. Crystal structure of bis(tetrapropylammonium) terephthalate – 1-(diaminomethylene)thiourea – water (1/2/4) C18H40N5O4S
  26. Crystal structure of (E)-7-fluoro-2-(4-morpholinobenzylidene)-3,4-dihydronaphthalen-1(2H)-one, C21H20FNO2
  27. The crystal structure of poly[diaqua-bis(μ 3-5-bromobenzene-1,3-dicarboxylato-κ 3 O,O,O′)-(μ 2-1,3-bis-(4-pyridyl)-propane-κ 2 N,N′)-dizinc(II))] – 5-bromobenzene-1,3-dicarboxylic acid [2/1], C37H29Br3N2O14Zn2
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https://doi.org/10.1515/ncrs-2023-0091
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Articles in the same Issue

  1. Frontmatter
  2. New Crystal Structures
  3. Crystal structure of phenyl(3,3-dichloro-1,3-dihydro-2H-pyrrolo[2,3-b]pyridin-2-one)methanone, C7H4Cl2N2O
  4. Crystal structure of poly[diaqua-bis(μ 2-1,4-diaminobutane-N:N′)cobalt(II)] dichloride, C8H28Cl2CoN4O2
  5. Synthesis and crystal structure of (4aR,7S)-7-hydroxy-7-isopropyl-1,1-dimethyldecahydro-2H,6H-8a,4a-(epoxymethano)phenanthren-12-one, C20H32O3
  6. The crystal structure of 1-(2-chlorobenzyl)-3-(3,5-dichlorophenyl)urea, C14H11Cl3N2O
  7. Crystal structure of tetrapropylammonium-1,3,5-thiadiazole-5-amido-2-carbamate – 1,2,4-thiadiazole-3,5-diamine – water (1/1/1), C17H37N9O3S2
  8. Tetrabutylammonium 1,3,5-thiadiazole-5-amido-2-carbamate—1,2,4-thiadiazole-3,5-diamine— water (1/1/1), C21H45N9O3S2
  9. The crystal structure of ((E)-2,4-dichloro-6-(((2-hydroxy-5-nitrophenyl)imino)methyl)phenolato-κ 3 N,O,O′)tris(pyridine-κN)manganese(II), C28H21Cl2MnN5O4
  10. The crystal structure of aqua-bis{2-bromo-6-((2-(2-phenylacetyl)hydrazineylidene)methyl)phenolato-κ3 N,O,O′}-dimethylformamide-κ1 O-erbium(III) chloride – dimethylformamide – water (1/2/1), C39H49N7O9Br2ClEr
  11. Crystal structure of (diaqua-bis(phenanthroline-K 2 N,N′)-tetrakis(m 2-3,4,5,6-tetrafluorophthalato-K 4 O,O:O′:O″;K 2 O:O′)dierbium (III) phenanthroline (1/2), C80H38Er2F16N8O18
  12. Crystal structure of (E)-7-methoxy-2-(4-methoxy-2-(trifluoromethyl)benzylidene)-3,4-dihydronaphthalen-1(2H)-one, C20H17F3O3
  13. The crystal structure of 4–(4,4,5,5–tetramethyl–1,3,2–dioxaborolan–2–yl)morpholine, C10H20BNO3
  14. The crystal structure of catena–poly[aqua(1-naphthoato-κ 2 O,O′)-(μ-1-naphthoato-κ 4 O:O,O′:O′)lead(II)], C22H16O5Pb
  15. The crystal structure of 1-(4-chlorophenyl)-3-cycloheptylurea, C14H19ClN2O
  16. The crystal structure of 4-(pyren-1-yl)butyl-4-nitrobenzoate, C27H21NO4
  17. Crystal structure of cyclo-(bis(µ2-3,3′-(1H-imidazole-3-ium-1,3-diyl)dipropionato-κ4 O,O′:O″,O″′)-dinitrato-κ2 O,O′-tetraoxido-diuranium(VI) C18H22N6O18U2
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  19. Redetermination of crystal structure of [bis(pyridin-2-ylmethyl)amine-κ 3 N,Nʹ,Nʺ]chloridopalladium(II) chloride monohydrate
  20. Crystal structure of catena-poly[triaqua-[bis(m2-4-(1H-1,2,4-triazol-1-yl)benzoato-k2O:O')-(4-(1H-1,2,4-triazol-1-yl)benzoato-k1O)-praseodymium (III) monohydrate], C27H26N9O10Pr
  21. Crystal structure of trans-diaqua-bis(methyl methylcarbamohydrazonothioato-κ2 N,N′) nickel(II) iodide semihydrate, C6H22N6O2NiS2I2·0.5H2O
  22. The crystal structure of 2-(2-fluoro-4-methyl-5-((2,2,2-trifluoroethyl)thio)phenyl)isoindolin-1-one, C17H13F4NOS
  23. The crystal structure of di-μ-1-naphthylacetato-κ 3 O,O′:O;κ 3 O:O,O′-bis[(1-naphthylacetato-κ 2 O,O′)(2,2′-bipyridine-κ 2 N,N′)lead(II)] monohydrate, C68H54N4O9Pb2
  24. Crystal structure of tetrapropylammonium guanidinium 4,4′-sulfonyldibenzoate monohydrate, C27H44N4O7S
  25. Crystal structure of bis(tetrapropylammonium) terephthalate – 1-(diaminomethylene)thiourea – water (1/2/4) C18H40N5O4S
  26. Crystal structure of (E)-7-fluoro-2-(4-morpholinobenzylidene)-3,4-dihydronaphthalen-1(2H)-one, C21H20FNO2
  27. The crystal structure of poly[diaqua-bis(μ 3-5-bromobenzene-1,3-dicarboxylato-κ 3 O,O,O′)-(μ 2-1,3-bis-(4-pyridyl)-propane-κ 2 N,N′)-dizinc(II))] – 5-bromobenzene-1,3-dicarboxylic acid [2/1], C37H29Br3N2O14Zn2
  28. The crystal structure of 2-bromo-1,3-phenylene bis(4-methylbenzenesulfonate), C20H17BrO6S2
  29. Crystal structure of europium dichromium icosaaluminum, EuCr2Al20
  30. The crystal structure of N′1,N′3-di((E)-benzylidene) isophthalohydrazide dihydrate, C 22 H 22 N 4 O 4
  31. Crystal structure of 7α,11α-dihydroxy-15-oxo-ent-kauran-16-en-19,6β-olide, C20H26O5
  32. Crystal structure of 4-chloro-N′-[(1E)-pyridin-3-ylmethylidene]benzohydrazide, C13H10ClN3O
  33. The crystal structure of (Z)-3-(1-(2-((E)-4-isopropylbenzylidene)hydrazinyl)ethylidene) chroman-2,4-dione, C21H20N2O3
  34. Crystal structure of E-7-fluoro-2-(2-(trifluoromethyl)benzylidene)-3,4-dihydronaphthalen-1(2H)-one, C18H12F4O
  35. Crystal structure of bis(6-aminopyridine-2-carboxylato–k2O,N)-bis(N,N-dimethylformamide-k1 O)zinc(II), C18H24N6O6Zn
  36. Crystal structure of 5-(adamantan-1-yl)-3-[(4-{[2-(trifluoromethyl)phenyl]-methyl}piperazin-1-yl)methyl]-1,3,4-oxadiazole-2(3H)-thione, C25H31F3N4OS
  37. Crystal structure of tetrapropylammonium bicarbonate–1-(diaminomethylene)thiourea – water (2/2/1), C30H72N10O7S2
  38. Crystal structure of tris(2,2′-bipyridine-κ2 N,N′)iron(II) triiodide – dichloromethane (2/1), C61H50Cl2Fe2I12N12
  39. Crystal structure of 2-amino-3-[2-(1,3,3-trimethyl-1,3-dihydro-indol-2-ylidene)-ethylideneamino]-but-2-enedinitrile, C17H17N5
  40. The crystal structure of 1-(2-chlorophenyl)-3-cycloheptylurea, C14H19ClN2O
  41. Crystal structure of potassium bis(pentaselenido-κ 2 Se 1,Se 5)palladate(II), K2[Pd(Se5)2]
  42. The crystal structure of 5,10-bis(2-methoxyethyl)-5,10-dihydro-[1,2,3,4]tetrathiocino[5,6-b:8, 7-b′]diindole, C22H22N2O2S4
  43. The crystal structure of 4-(4-iodophenyl)-5H-1,2,3-dithiazole-5-thione, C8H4INS3
  44. Crystal structure of bis{μ2-(4-acetyl-phenoxy)acetato-κ2 O:O′}-bis{μ2-(4-acetyl-phenoxy)acetato-κ3 O,O′:O)- bis{(4-acetyl-phenoxy)acetato-κ2 O,O′}-bis(phenanthrolin-κ2 N,N′)didysprosium(III) tetrahydrate, C84H78N4O28Dy2
  45. Crystal structure of Eu2Pd3.37(1)Zn13.63(1)
  46. Crystal structure of 2-methoxy-4-(methoxy-carbonyl)phenyl 2-chloro-4-fluorobenzoate, C16H12ClFO5
  47. Crystal structure of catena-poly[bis(μ2-dicyanamide-κ2 N:N′)-bis(4-vinylpyridine-κN)-copper(II)], C18H14CuN8
  48. The crystal structure of iguratimod-dimethylformamide (1/1), C17H14N2O6S·C3H7NO
  49. Synthesis and crystal structure of 1-((3R,10S,13S,17S)-10,13-dimethyl-3-(m-tolylamino)hexadecahydro-1H-cyclopenta[α]phenanthren-17-yl)ethan-1-one, C28H41NO
  50. The crystal structure of diaqua-bis(4-bromo-2-formylphenoxy)zinc(II), C14H12Br2O6Zn
  51. The crystal structure of tetra(1-ethylimidazole-κ 1 N)-[μ 4-imidazole-4,5-dicarboxylato-κ 4 O, N, O′, N′]-trioxido-divanadium, C25H33N10O7V2
  52. The crystal structure of (E)-N′-(1-(4-fluorophenyl)propylidene)-2-hydroxybenzohydrazide, C16H15FN2O2
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