Bis(oxonium) tetra­kis(o-toluidinium) cyclo­hexa­phosphate

Marouani, H.; Rzaigui, M.; Al-Deyab, S.S.

doi:10.1107/S1600536810006537

Volume 66
Part 3
Page o702
March 2010

Received 16 February 2010
Accepted 19 February 2010
Online 27 February 2010

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.005 Å
R = 0.052
wR = 0.114
Data-to-parameter ratio = 20.8
Details

Bis(oxonium) tetrakis(o-toluidinium) cyclohexaphosphate

Houda Marouani,^a ^* Mohamed Rzaigui ^a and Salem S. Al-Deyab ^b

^aLaboratoire de Chimie des Matériaux, Faculté des Sciences de Bizerte, 7021 Zarzouna Bizerte, Tunisia, and ^bPetrochemical Research Chair, College of Science, King Saud University, Riyadh, Saudi Arabia
Correspondence e-mail: houda.marouani@fsb.rnu.tn

In the title compound, 4C₇H₁₀N⁺·2H₃O⁺·P₆O₁₈^6-, the complete cyclohexaphosphate anion is generated by crystallographic inversion symmetry. In the crystal, the H₃O⁺ ions and the [P₆O₁₈]^6- anions are linked by O-HO hydrogen bonds, generating infinite layers lying parallel to the ab plane at z = 1/2. These layers are interconnected by the organic cations, which establish N-HO hydrogen bonds with the [P₆O₁₈]^6- anions.

Related literature

For further synthetic details, see: Schülke & Kayser (1985). For related structures, see: Amri et al. (2008); Larafa et al. (1997); Akriche & Rzaigui (2000); Selmi et al. (2009); Khemiri et al. (2009). For a discussion on hydrogen bonding, see: Brown (1976); Blessing (1986). For tetrahedral distortions, see: Baur (1974).

Experimental

Crystal data

4C₇H₁₀N⁺·2H₃O⁺·P₆O₁₈^6-
M_r = 944.51
Triclinic, $[P \overline 1]$
a = 9.344 (3) Å
b = 10.360 (2) Å
c = 11.537 (2) Å
= 95.35 (4)°
= 92.23 (3)°
= 116.00 (5)°
V = 995.4 (4) Å³
Z = 1
Mo K radiation
= 0.36 mm^-1
T = 293 K
0.25 × 0.20 × 0.15 mm

Data collection

Enraf-Nonius CAD-4 diffractometer
6038 measured reflections
5773 independent reflections
3061 reflections with I > 2(I)
R_int = 0.025
2 standard reflections every 120 min intensity decay: 10%

Refinement

R[F² > 2(F²)] = 0.052
wR(F²) = 0.114
S = 1.01
5773 reflections
278 parameters
6 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.33 e Å^-3
_min = -0.38 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O10-H110O9	0.86 (1)	1.62 (1)	2.469 (3)	170 (3)
O10-H210O2ⁱ	0.86 (1)	1.69 (1)	2.550 (3)	177 (3)
O10-H310O6ⁱⁱ	0.86 (1)	1.67 (1)	2.524 (3)	171 (3)
N1-H1AO8ⁱⁱⁱ	0.89	1.86	2.753 (3)	177
N1-H1BO2ⁱ	0.89	1.98	2.853 (3)	168
N1-H1CO5ⁱⁱⁱ	0.89	1.92	2.800 (3)	169
N2-H2AO6^iv	0.89	2.35	3.085 (4)	140
N2-H2BO5ⁱⁱ	0.89	2.02	2.904 (3)	176
N2-H2CO1^v	0.89	1.83	2.710 (3)	170
Symmetry codes: (i) -x+1, -y, -z+1; (ii) x+1, y+1, z; (iii) x+1, y, z; (iv) -x, -y, -z+1; (v) x, y+1, z.

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1996); program(s) used to solve structure: SHELXS86 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); 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: HB5337 ).

References

Akriche, S. & Rzaigui, M. (2000). Solid State Sci. 2, 397-403.
Amri, O., Abid, S. & Rzaigui, M. (2008). Phosphorus Sulfur Silicon Relat. Elem. 183, 1996-2005.
Baur, W. H. (1974). Acta Cryst. B30, 1195-1215.
Blessing, R. H. (1986). Acta Cryst. B42, 613-621.
Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal impact GbR, Bonn, Germany.
Brown, I. D. (1976). Acta Cryst. A32, 24-31.
Enraf-Nonius (1994). CAD-4 EXPRESS. Enraf-Nonius, Delft, The Netherlands.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
Harms, K. & Wocadlo, S. (1996). XCAD4. University of Marburg, Germany.
Khemiri, H., Akriche, S. & Rzaigui, M. (2009). Acta Cryst. E65, o1152.
Larafa, K., Mahjoub, A., Rzaigui, M. & Durif, A. (1997). Eur. J. Solid State Inorg. Chem. 34, 481-494.
Schülke, U. & Kayser, R. (1985). Z. Anorg. Allg. Chem. 531, 167-175.
Selmi, A., Akriche, S. & Rzaigui, M. (2009). Acta Cryst. E65, m1487.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

organic compounds