(IUCr) Rb2Sb4O11

Volume 65
Part 6
Page i41
June 2009

Received 22 April 2009
Accepted 29 April 2009
Online 7 May 2009

Key indicators
Single-crystal X-ray study
T = 120 K
Mean (Sb-O) = 0.004 Å
R = 0.028
wR = 0.072
Data-to-parameter ratio = 14.4
Details

Rb₂Sb₄O₁₁

Govindaraasan Kalpana ^a ^* and Mark T. Weller ^a

^aSchool of Chemistry, University of Southampton, Highfield Campus, Southamtpon SO17 1BJ, England
Correspondence e-mail: kg1t07@soton.ac.uk

The title compound, dirubidium tetraantimonate(V), Rb₂Sb₄O₁₁, has been synthesized by flux reaction. It is isotypic with known A₂Sb₄O₁₁ (A = K, Cs) structures and consists of an (Sb₄O₁₁)^2- skeleton and two Rb atoms as charge-compensating cations. Distorted SbO₆ octahedra share edges and corners, resulting in a layered assembly. Alternate stacking of the layers along the c axis leads to the formation of tunnels. The Rb⁺ ions, surrounded by nine and ten O atoms, respectively, are located in these tunnels. Some atoms in the structure are on special positions of m symmetry (two Sb atoms, both Rb atoms and four O atoms) and 2 symmetry (one O atom).

Related literature

Isotypic structures have been reported by Hong (1974) [K₂Sb₄O₁₁] and by Hirschle et al. (2001) [Cs₂Sb₄O₁₁]. For Rb-O distances in the crystal structure of Rb₃Ti₂(TiO)(PO₄)₃P₂O₇, see: Duhlev (1994).

Experimental

Crystal data

Rb₂Sb₄O₁₁
M_r = 833.94
Monoclinic, C 2/m
a = 19.5045 (11) Å
b = 7.5681 (4) Å
c = 7.2115 (4) Å
= 95.203 (3)°
V = 1060.12 (10) Å³
Z = 4
Mo K radiation
= 19.26 mm^-1
T = 120 K
0.12 × 0.12 × 0.11 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2007) T_min = 0.110, T_max = 0.120
7605 measured reflections
1312 independent reflections
1234 reflections with I > 2(I)
R_int = 0.038

Refinement

R[F² > 2(F²)] = 0.028
wR(F²) = 0.072
S = 1.41
1312 reflections
91 parameters
18 restraints
_max = 1.89 e Å^-3
_min = -1.91 e Å^-3

Table 1
Selected bond lengths (Å)

Sb1-O4	1.940 (4)
Sb1-O3ⁱ	1.956 (5)
Sb1-O1ⁱⁱ	1.986 (3)
Sb1-O2	2.089 (5)
Sb2-O3ⁱⁱⁱ	1.903 (5)
Sb2-O6^iv	1.970 (3)
Sb2-O2^v	1.977 (5)
Sb2-O5ⁱⁱⁱ	1.993 (5)
Sb2-O2ⁱⁱⁱ	2.129 (5)
Sb3-O8	1.9281 (15)
Sb3-O4	1.959 (4)
Sb3-O7^vi	1.978 (4)
Sb3-O7	1.979 (4)
Sb3-O6	2.005 (4)
Sb3-O5	2.0261 (14)
Symmetry codes: (i) x, y, z+1; (ii) x+1, y, z+1; (iii) -x+1, -y, -z+1; (iv) -x+1, y, -z+1; (v) x-1, y, z; (vi) $[-x+{\script{3\over 2}}, -y-{\script{1\over 2}}, -z+1]$ .

Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997) and COLLECT; data reduction: DENZO nd COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: WinGX (Farrugia, 1999).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2230 ).

Acknowledgements

The authors thank the EPSRC for funding, the EPSRC National Crystallography Service for the use of the KappaCCD diffractometer and Dr Mark E. Light for useful discussions.

References

Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Duhlev, R. (1994). Acta Cryst. C50, 1523-1525.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
Hirschle, C. J. R., Emmerling, F. & Röhr, C. (2001). Z. Naturforsch. Teil B, 56, 169-178.
Hong, H. Y.-P. (1974). Acta Cryst. B30, 945-952.
Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press.
Sheldrick, G. M. (2007). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

inorganic compounds

Rb2Sb4O11