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Acta Crystallogr Sect E Struct Rep Online. 2010 February 1; 66(Pt 2): i6.
Published online 2010 January 13. doi:  10.1107/S1600536810000589
PMCID: PMC2979920

Filled skutterudite structure of europium ruthenium polyphosphide, EuRu4P12

Abstract

The crystal structure of EuRu4P12 is isotypic with filled skutterudite structures of rare earth transition metal poly­phosphides: RFe4P12 (R = Ce, Pr, Nd, Sm and Eu), RRu4P12 (R = La, Ce, Pr and Nd) and ROs4P12 (R = La, Ce, Pr and Nd). The Ru cation is coordinated by six P anions in a distorted octa­hedral manner. The partially occupied Eu position (site occupancy 0.97) is enclosed by a cage formed by the corner-shared framework of the eight RuP6 octa­hedra.

Related literature

The title compound is isotypic with the Im An external file that holds a picture, illustration, etc.
Object name is e-66-000i6-efi1.jpg form of LaFe4P12, see: Jeitschko & Braun (1977 [triangle]). For the single-crystal preparation and magnetic and electrical properties of EuRu4P12, see: Sekine et al. (2000 [triangle]). For hyperfine inter­action in EuRu4P12, see: Grandjean et al. (1983 [triangle]); Indoh et al. (2002 [triangle]). For the method used to avoid multiple diffraction, see: Takenaka et al. (2008 [triangle]).

Experimental

Crystal data

  • Eu0.97Ru4P12
  • M r = 923.37
  • Cubic, An external file that holds a picture, illustration, etc.
Object name is e-66-000i6-efi2.jpg
  • a = 8.04163 (10) Å
  • V = 520.04 (1) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 13.37 mm−1
  • T = 100 K
  • 0.04 mm (radius)

Data collection

  • MacScience M06XHF22 four-circle diffractometer
  • Absorption correction: for a sphere [transmission coefficients for spheres tabulated in International Tables Vol. C (1992), Table 6.3.3.3, were interpolated with Lagrange’s method (four-point interpolation; Yamauchi et al., 1965 [triangle])] T min = 0.486, T max = 0.526
  • 1564 measured reflections
  • 769 independent reflections
  • 625 reflections with F > 3σ(F)
  • R int = 0.016

Refinement

  • R[F 2 > 2σ(F 2)] = 0.020
  • wR(F 2) = 0.024
  • S = 1.54
  • 1304 reflections
  • 30 parameters
  • Δρmax = 2.08 e Å−3
  • Δρmin = −1.14 e Å−3

Data collection: MXCSYS (MacScience, 1995 [triangle]) and IUANGLE (Tanaka et al., 1994 [triangle]); cell refinement: RSLC-3 UNICS system (Sakurai & Kobayashi, 1979 [triangle]); data reduction: RDEDIT (Tanaka, 2008 [triangle]); program(s) used to solve structure: QNTAO (Tanaka et al., 2008 [triangle]); program(s) used to refine structure: QNTAO; molecular graphics: ATOMS for Windows (Dowty, 2000 [triangle]); software used to prepare material for publication: RDEDIT.

Table 1
Selected bond lengths (Å)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810000589/br2130sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810000589/br2130Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

Part of this study was supported by the Inter­national Training Programme (ITP) from the Japan Society for the Promotion of Science (JSPS).

supplementary crystallographic information

Refinement

Multiple diffraction was avoided by using ψ-scans (Takenaka et al., 2008). Intensities were measured at the equi-temperature region of combination of angles ω and χ of a four-circle diffractometer. The intensities have not been included for the refinement if the multiple diffraction cannot be avoided. In addition, the crystal was cooled to 100 K with an Oxford cryostream cooler installed on a four-circle diffractometer. Since the temperature of the sample depends on the ω and χ-angle and the X-ray diffraction measurement was carried out in the equi-temperature area, the ω and χ-angle had the limitation. Thus completeness of the independent reflection was less than 85%.

Figures

Fig. 1.
The structure of EuRu4P12 at 100 K. Small yellow and large red spheres, respectively, represent P and Eu atoms. Green distorted octahedron represent RuO6 units.
Fig. 2.
Bonding of Ru4 and P12 around an Eu ion with displacement ellipsoids at the 90% probability level. Red, blue and yellow ellipsoids represent Eu, Ru and P atoms, in Fig. 1.

Crystal data

Eu0.97Ru4P12Dx = 5.925 Mg m3
Mr = 923.37Mo Kα radiation, λ = 0.71073 Å
Cubic, Im3Cell parameters from 37 reflections
Hall symbol: -I 2 2 3θ = 36.0–37.7°
a = 8.04163 (10) ŵ = 13.37 mm1
V = 520.04 (1) Å3T = 100 K
Z = 2Sphere, black
F(000) = 828.40.04 mm (radius)

Data collection

MacScience M06XHF22 four-circle diffractometer769 independent reflections
Radiation source: fine-focus rotating anode625 reflections with F > 3σ(F)
graphiteRint = 0.016
Detector resolution: 1.25 x 1.25° pixels mm-1θmax = 74.2°, θmin = 3.6°
ω/2θ scansh = −18→20
Absorption correction: for a sphere [transmission coefficients for spheres tabulated in International Tables Vol. C (1992), Table 6.3.3.3, were interpolated with Lagrange's method (four-point interpolation; Yamauchi et al., 1965)]k = −21→21
Tmin = 0.486, Tmax = 0.526l = −18→20
1564 measured reflections

Refinement

Refinement on FWeighting scheme based on measured s.u.'s
Least-squares matrix: full(Δ/σ)max = 0.018
R[F2 > 2σ(F2)] = 0.020Δρmax = 2.08 e Å3
wR(F2) = 0.024Δρmin = −1.14 e Å3
S = 1.54Extinction correction: B–C type 1 Gaussian isotropic (Becker & Coppens, 1975)
1304 reflectionsExtinction coefficient: 0.068 (6)
30 parameters

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

xyzUiso*/UeqOcc. (<1)
Eu10.0000000.0000000.0000000.00270 (2)0.970 (4)
Ru10.2500000.2500000.2500000.001840 (15)
P10.0000000.3593290.1433860.00283 (4)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Eu10.00271 (3)0.00271 (3)0.00271 (3)000
Ru10.00185 (3)0.00185 (3)0.00185 (3)0.000108 (17)0.000108 (17)0.000108 (17)
P10.00268 (10)0.00301 (10)0.00285 (10)00−0.00009 (7)

Geometric parameters (Å, °)

Eu1—P13.1112 (3)Ru1—P1i2.3558 (1)
Eu1—Ru13.4821 (1)P1—P1ii2.3061 (1)
Ru1—P12.3558 (1)P1—P1i3.0829 (1)
Eu1—P1—Ru177.78Ru1—P1—P1i49.13
Eu1—P1—P1ii68.25P1—Ru1—P1i81.74
Eu1—P1—P1i109.77P1ii—P1—P1i89.59
Ru1—P1—P1ii111.34

Symmetry codes: (i) −z+1/2, x+1/2, −y+1/2; (ii) −x, y, −z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BR2130).

References

  • Dowty, E. (2000). ATOMS for Windows Shape Software, Kingsport, Tennessee, USA.
  • Grandjean, F., Gerard, A., Hodges, J., Braun, D. J. & Jeitschko, W. (1983). Hyperfine Interact.15–16, 765–765.
  • Indoh, K., Onodera, H., Sekine, C., Shirotani, I. & Yamaguchi, Y. (2002). J. Phys. Soc. Jpn, 71 (Suppl.), 243–245.
  • Jeitschko, W. & Braun, D. (1977). Acta Cryst. B33, 3401–3406.
  • MacScience (1995). MXCSYS Bruker AXS Inc., Tsukuba, Ibaraki, Japan.
  • Sakurai, T. & Kobayashi, K. (1979). Rikagaku Kenkyusho Hokoku (Rep. Inst. Phys. Chem. Res.), 55, 69–77.
  • Sekine, C., Inoue, M., Inaba, T. & Shirotani, I. (2000). Physica B, 281–282, 308–310.
  • Takenaka, Y., Sakakura, T., Tanaka, K. & Kishimoto, S. (2008). Acta Cryst. A64, C566.
  • Tanaka, K. (2008). RDEDIT Unpublished.
  • Tanaka, K., Kumazawa, S., Tsubokawa, M., Maruno, S. & Shirotani, I. (1994). Acta Cryst. A50, 246–252.
  • Tanaka, K., Makita, R., Funahashi, S., Komori, T. & Zaw Win (2008). Acta Cryst. A64, 437–449. [PubMed]
  • Yamauchi, J., Moriguchi, S. & Ichimatsu, S. (1965). Numerical Calculation Method for Computer Tokyo: Baifukan.

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography