Redetermination of the perovskite-type compound YRh(3)B revealing a Rh deficiency.

In contrast with previous structural studies of ytterbium trirhodium boride, YbRh(3)B, that suggest a boron deficiency, the current redetermination of the crystal structure of YbRh(3)B revealed instead a rhodium deficiency with a refined composition of YbRh(2.67 (2))B. In the ABX(3) perovskite-type structure, Yb, B and Rh are located on the A, B and X positions, respectively, with site symmetries of mm for the A and B sites, and 4/mm.m for the X site.

Related literature

For a previous powder diffraction study of YbRh3B, see: Takei & Shishido (1984 ▶). For general background, see: Becker & Coppens (1975 ▶); Libermann et al. (1971 ▶); Mann (1968 ▶).

Experimental

Crystal data

YbRh2.67B

M = 458.61

Cubic,

a = 4.12992 (7) Å

V = 70.44 (1) Å3

Z = 1

Mo Kα radiation

μ = 47.90 mm−1

T = 109 (1) K

Radius: 0.041 mm

Data collection

MacScience M06XHF22 four-circle diffractometer

Absorption correction: for a sphere [transmission coefficients for spheres tabulated in International Tables for X-ray Crystallography (Vol. II, 1972, Table 5.3.6B) were interpolated with Lagrange’s method (four point interpolation; Yamauchi et al., 1965 ▶)] T min = 0.069, T max = 0.169

953 measured reflections

193 independent reflections

193 reflections with F > 3σ(F)

R int = 0.018

Refinement

R[F 2 > 2σ(F 2)] = 0.014

wR(F 2) = 0.029

S = 1.15

193 reflections

11 parameters

3 restraints

Δρmax = 1.86 e Å−3

Δρmin = −1.98 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 & Ōnuki, 2002 ▶; 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/S1600536808030754/wm2195sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808030754/wm2195Isup2.hkl

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

YbRh2.67B	Dx = 10.81 Mg m−3
Mr = 458.61	Mo Kα radiation, λ = 0.71073 Å
Cubic, Pm3m	Cell parameters from 30 reflections
Hall symbol: -P 4 2 3	θ = 36.5–38.3°
a = 4.12992 (7) Å	µ = 47.90 mm−1
V = 70.44 (1) Å3	T = 109 K
Z = 1	Sphere, black
F(000) = 195.14	0.08 × 0.08 × 0.08 × 0.04 (radius) mm

MacScience M06XHF22 four-circle diffractometer	193 independent reflections
Radiation source: fine-focus rotating anode	193 reflections with F > 3σ(F)
graphite	Rint = 0.019
Detector resolution: 1.25 x 1.25° pixels mm-1	θmax = 74.9°, θmin = 4.9°
ω/2θ scans	h = −7→9
Absorption correction: for a sphere [transmission coefficients for spheres tabulated in International Tables for X-ray Crystallography (Vol. II, 1972, Table 5.3.6B) were interpolated with Lagrange's method (four point interpolation; Yamauchi et al., 1965)]	k = −11→11
Tmin = 0.069, Tmax = 0.169	l = −11→11
953 measured reflections

Refinement on F	3 restraints
Least-squares matrix: full	Weighting scheme based on measured s.u.'s
R[F2 > 2σ(F2)] = 0.014	(Δ/σ)max = 0.0001
wR(F2) = 0.029	Δρmax = 1.86 e Å−3
S = 1.15	Δρmin = −1.98 e Å−3
193 reflections	Extinction correction: B-C type 1 Gaussian anisotropic (Becker & Coppens, 1975)
11 parameters	Extinction coefficient: 0.052 (2) times 104

Experimental. Multiple diffraction was avoided by using ψ-scans. Intensities was measured at the equi-temperature region of combinaion of angles ω and χ of a four-circle diffractometer.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Yb	0.5000	0.5000	0.5000	0.212 (1)
Rh	0.0000	0.0000	0.5000	0.143 (2)	0.891 (6)
B	0.0000	0.0000	0.0000	0.291 (6)

	U11	U22	U33	U12	U13	U23
Yb	0.00269 (4)	0.00269 (4)	0.00269 (4)	0	0	0
Rh	0.00202 (6)	0.00202 (6)	0.00139 (6)	0	0	0
B	0.0037 (2)	0.0037 (2)	0.0037 (2)	0	0	0

Rhi—Rhii	2.92029 (7)	Bi—Yb	3.57662 (7)
Bi—Rhi	2.06496 (7)	Rhi—Yb	2.92029 (7)
?···?	?
Rhi—Bi—Rhii	90.000	Rhi—Yb—Bi	35.264
Rhi—Yb—Rhii	60.000	Yb—Bi—Rhii	54.736

Table 1

Selected bond lengths (Å)

Rhi—Rhii	2.92029 (7)
Bi—Rhi	2.06496 (7)
Bi—Yb	3.57662 (7)
Rhi—Yb	2.92029 (7)

Symmetry codes: (i) ; (ii) .