Bis(4,4′-bipyridinium) di-μ-hydroxido-bis­[dihydroxido(pyridine-2,6-dicarboxyl­ato)anti­monate(III,V)] octa­hydrate

Soleimannejad, J.; Aghabozorg, H.; Golenji, Y.M.A.; Attar Gharamaleki, J.; Adams, H.

doi:10.1107/S1600536808001372

Volume 64
Part 2
Pages m387-m388
February 2008

Received 29 November 2007
Accepted 14 January 2008
Online 23 January 2008

Key indicators
Single-crystal X-ray study
T = 150 K
Mean (C-C) = 0.003 Å
R = 0.023
wR = 0.060
Data-to-parameter ratio = 16.6
Details

Bis(4,4'-bipyridinium) di--hydroxido-bis[dihydroxido(pyridine-2,6-dicarboxylato)antimonate(III,V)] octahydrate

Janet Soleimannejad,^a ^* Hossein Aghabozorg,^b Yaghoub Mohammadzadeh Azar Golenji,^a Jafar Attar Gharamaleki ^b and Harry Adams ^c

^aDepartment of Chemistry, Ilam University, Ilam, Iran,^bDepartment of Chemistry, Teacher Training University, 49 Mofateh Avenue 15614, Tehran, Iran, and ^cDepartment of Chemistry, Sheffield University, Sheffield S3 7HF, England
Correspondence e-mail: janet_soleimannejad@yahoo.com

The reaction of antimony(III) chloride, 4,4'-bipyridine (4,4'-bipy) and pyridine-2,6-dicarboxylic acid (pydcH₂), in a 1:2:2 molar ratio in an aqueous solution, resulted in the formation of the title centrosymmetric disordered mixed-valence Sb^III/Sb^V compound, (C₁₀H₉N₂)₂[Sb₂(C₇H₃NO₄)₂(OH)₆]·8H₂O or (4,4'-bipyH)₂[Sb(pydc)(OH)₂( [mu] -OH)]₂·8H₂O. The seven donor atoms of the (pydc)^2- groups and the hydroxido ligands form a distorted pentagonal-bipyramidal arrangement around the Sb^III/Sb^V centers. C-H [pi] stacking interactions between CH groups of the complex dianion and the aromatic rings of the (4,4'-bipyH)⁺ cations, with a distance of 2.89 Å, are observed. In the crystal structure, a wide range of noncovalent interactions, consisting of O-HO, N-HO and C-HO hydrogen bonds [DA ranging from 2.722 (2) to 3.137 (3) Å], ion pairing, [pi] - [pi] stacking [centroid-centroid distance of 3.4363 (13) Å] and C-H [pi] interactions, connect the various components into a supramolecular structure.

Related literature

For related literature, see: Aghabozorg, Attar Gharamaleki, Ghadermazi et al. (2007); Aghabozorg, Attar Gharamaleki, Ghasemikhah et al. (2007); Aghabozorg, Daneshvar et al. (2007).

Experimental

Crystal data

(C₁₀H₉N₂)₂[Sb₂(C₇H₃NO₄)₂(OH)₆]·8H₂O
M_r = 1134.27
Triclinic, $[P \overline 1]$
a = 10.0149 (11) Å
b = 10.4826 (12) Å
c = 11.0974 (12) Å
= 92.816 (2)°
= 97.813 (2)°
= 114.046 (2)°
V = 1047.0 (2) Å³
Z = 1
Mo K radiation
= 1.38 mm^-1
T = 150 (2) K
0.43 × 0.41 × 0.39 mm

Data collection

Bruker SMART 1000 diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2004) T_min = 0.588, T_max = 0.614 (expected range = 0.557-0.583)
12026 measured reflections
4790 independent reflections
4536 reflections with I > 2(I)
R_int = 0.022

Refinement

R[F² > 2(F²)] = 0.023
wR(F²) = 0.060
S = 1.07
4790 reflections
289 parameters
H-atom parameters constrained
_max = 0.91 e Å^-3
_min = -0.70 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O5-H5AO10ⁱ	0.85	2.13	2.949 (2)	161
O6-H6AO10ⁱⁱ	0.85	1.94	2.783 (2)	172
O7-H7AO8ⁱⁱⁱ	0.85	1.91	2.760 (2)	174
O8-H8BO11^iv	0.85	2.22	2.997 (2)	151
O8-H8BO3^iv	0.85	2.61	3.067 (2)	115
O8-H8AN2	0.85	1.93	2.751 (2)	161
O9-H9AO1^v	0.85	1.91	2.749 (2)	170
O9-H9BO6	0.85	1.88	2.731 (2)	177
O10-H10AO11^vi	0.85	2.03	2.867 (2)	168
O10-H10BO9	0.85	1.87	2.722 (2)	178
O11-H11AO4	0.85	1.95	2.793 (2)	174
O11-H11BO8	0.85	1.99	2.830 (2)	169
N3-H3AO6^vii	0.85	1.91	2.760 (2)	173
C13-H13O1^viii	0.95	2.30	3.205 (3)	160
C15-H15O5	0.95	2.23	3.107 (3)	153
C17-H17O5^ix	0.95	2.23	3.137 (3)	159
C5-H5Cg1(N2/C11-C15)^x	0.95	2.89	3.596 (2)	132
Symmetry codes: (i) x-1, y, z; (ii) -x+1, -y, -z; (iii) x, y, z-1; (iv) -x, -y, -z+1; (v) -x+1, -y+1, -z; (vi) -x+1, -y, -z+1; (vii) x, y+1, z; (viii) x, y, z+1; (ix) -x, -y+1, -z; (x) -x+1, -y+1, -z+1.

Data collection: SMART (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2034 ).

Acknowledgements

Financial support from Ilam University and the Teacher Training University is gratefully acknowledged.

References

Aghabozorg, H., Attar Gharamaleki, J., Ghadermazi, M., Ghasemikhah, P. & Soleimannejad, J. (2007). Acta Cryst. E63, m1803-m1804.
Aghabozorg, H., Attar Gharamaleki, J., Ghasemikhah, P., Ghadermazi, M. & Soleimannejad, J. (2007). Acta Cryst. E63, m1710-m1711.
Aghabozorg, H., Daneshvar, S., Motyeian, E., Ghadermazi, M. & Attar Gharamaleki, J. (2007). Acta Cryst. E63, m2468-m2469.
Bruker (2004). SADABS. Version 1. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2005). SMART (Version 5.059) and SAINT (Version 7.23A). Bruker AXS Inc., Madison, Wisconsin, USA.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds