Filled skutterudite structure of europium ruthenium polyphosphide, EuRu(4)P(12).

The crystal structure of EuRu(4)P(12) is isotypic with filled skutterudite structures of rare earth transition metal poly-phosphides: RFe(4)P(12) (R = Ce, Pr, Nd, Sm and Eu), RRu(4)P(12) (R = La, Ce, Pr and Nd) and ROs(4)P(12) (R = La, Ce, Pr and Nd). The Ru cation is coordinated by six P anions in a distorted octa-hedral manner. The partially occupied Eu position (site occupancy 0.97) is enclosed by a cage formed by the corner-shared framework of the eight RuP(6) octa-hedra.

Related literature

The title compound is isotypic with the Im form of LaFe4P12, see: Jeitschko & Braun (1977 ▶). For the single-crystal preparation and magnetic and electrical properties of EuRu4P12, see: Sekine et al. (2000 ▶). For hyperfine inter­action in EuRu4P12, see: Grandjean et al. (1983 ▶); Indoh et al. (2002 ▶). For the method used to avoid multiple diffraction, see: Takenaka et al. (2008 ▶).

Experimental

Crystal data

Eu0.97Ru4P12

M = 923.37

Cubic,

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

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

Eu0.97Ru4P12	Dx = 5.925 Mg m−3
Mr = 923.37	Mo Kα radiation, λ = 0.71073 Å
Cubic, Im3	Cell parameters from 37 reflections
Hall symbol: -I 2 2 3	θ = 36.0–37.7°
a = 8.04163 (10) Å	µ = 13.37 mm−1
V = 520.04 (1) Å3	T = 100 K
Z = 2	Sphere, black
F(000) = 828.4	0.04 mm (radius)

MacScience M06XHF22 four-circle diffractometer	769 independent reflections
Radiation source: fine-focus rotating anode	625 reflections with F > 3σ(F)
graphite	Rint = 0.016
Detector resolution: 1.25 x 1.25° pixels mm-1	θmax = 74.2°, θmin = 3.6°
ω/2θ scans	h = −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 = 0.526	l = −18→20
1564 measured reflections

Refinement on F	Weighting scheme based on measured s.u.'s
Least-squares matrix: full	(Δ/σ)max = 0.018
R[F2 > 2σ(F2)] = 0.020	Δρmax = 2.08 e Å−3
wR(F2) = 0.024	Δρmin = −1.14 e Å−3
S = 1.54	Extinction correction: B–C type 1 Gaussian isotropic (Becker & Coppens, 1975)
1304 reflections	Extinction coefficient: 0.068 (6)
30 parameters

	x	y	z	Uiso*/Ueq	Occ. (<1)
Eu1	0.000000	0.000000	0.000000	0.00270 (2)	0.970 (4)
Ru1	0.250000	0.250000	0.250000	0.001840 (15)
P1	0.000000	0.359329	0.143386	0.00283 (4)

	U11	U22	U33	U12	U13	U23
Eu1	0.00271 (3)	0.00271 (3)	0.00271 (3)	0	0	0
Ru1	0.00185 (3)	0.00185 (3)	0.00185 (3)	0.000108 (17)	0.000108 (17)	0.000108 (17)
P1	0.00268 (10)	0.00301 (10)	0.00285 (10)	0	0	−0.00009 (7)

Eu1—P1	3.1112 (3)	Ru1—P1i	2.3558 (1)
Eu1—Ru1	3.4821 (1)	P1—P1ii	2.3061 (1)
Ru1—P1	2.3558 (1)	P1—P1i	3.0829 (1)
Eu1—P1—Ru1	77.78	Ru1—P1—P1i	49.13
Eu1—P1—P1ii	68.25	P1—Ru1—P1i	81.74
Eu1—P1—P1i	109.77	P1ii—P1—P1i	89.59
Ru1—P1—P1ii	111.34

Table 1

Selected bond lengths (Å)

Eu1—P1	3.1112 (3)
Eu1—Ru1	3.4821 (1)
Ru1—P1	2.3558 (1)
P1—P1i	2.3061 (1)
P1—P1ii	3.0829 (1)

Symmetry codes: (i) ; (ii) .