Bis(homopiperazine-1,4-diium) cyclo­tetra­phosphate–telluric acid (1/2)

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

doi:10.1107/S1600536810038225

Volume 66
Part 11
Page o2712
November 2010

Received 13 August 2010
Accepted 24 September 2010
Online 2 October 2010

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.004 Å
R = 0.033
wR = 0.084
Data-to-parameter ratio = 28.5
Details

Bis(homopiperazine-1,4-diium) cyclotetraphosphate-telluric acid (1/2)

Hanène Hemissi,^a ^* Mohammed 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: hanene.hemissi@fsb.rnu.tn

The title compound, 2C₅H₁₄N₂²⁺·P₄O₁₂^4-·2Te(OH)₆, involves doubly protonated homopiperazinium cations, cyclotetraphosphate anions and telluric acid molecules. The framework possesses very large channels wherein the organic cations reside. A network of O-HO, N-HO and C-HO hydrogen bonds consolidates the crystal packing.

Related literature

For the properties of materials containing telluric acid, see: Chabchoub et al. (2006); Khemakhem, (1999). For related structures containing phosphate rings and telluric acid, see: Averbuch-Pouchot & Durif (1987a,b); Durif et al. (1982). For hydrogen bonding, see: Blessing (1986); Brown (1976). For deviations in four-membered phosphate rings having the same $[\overline{1}]$ internal symmetry, see: Durif (1995); A similar conformation for the same organic molecule was observed in (C₅H₁₄N₂)(H₂AsO₄)₂, see: Wilkinson & Harrison (2006). For the synthesis, see: Ondik (1964).

Experimental

Crystal data

C₅H₁₄N₂²⁺·0.5P₄O₁₂^4-·Te(OH)₆
M_r = 489.77
Monoclinic, C 2/c
a = 20.826 (3) Å
b = 8.3600 (13) Å
c = 17.030 (8) Å
= 101.65 (3)°
V = 2903.9 (14) Å³
Z = 8
Ag K radiation
= 0.56083 Å
= 1.24 mm^-1
T = 293 K
0.2 × 0.18 × 0.16 mm

Data collection

Enraf-Nonius CAD-4 diffractometer
8219 measured reflections
6346 independent reflections
4847 reflections with I > 2(I)
R_int = 0.027
2 standard reflections every 120 min intensity decay: 5%

Refinement

R[F² > 2(F²)] = 0.033
wR(F²) = 0.084
S = 1.01
6346 reflections
223 parameters
12 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 1.99 e Å^-3
_min = -1.19 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O1-H1O12ⁱ	0.86 (2)	1.85 (2)	2.686 (3)	165 (2)
N1-H1BO4ⁱⁱ	0.90	2.15	2.898 (3)	140
N1-H1BO9ⁱⁱⁱ	0.90	2.42	3.002 (3)	123
N1-H1AO2^iv	0.90	1.89	2.763 (3)	162
O2-H2O9^v	0.86 (2)	1.83 (2)	2.688 (3)	172 (3)
N2-H2AO12	0.90	1.89	2.769 (3)	167
N2-H2BO11^vi	0.90	1.85	2.739 (3)	172
O3-H3O8^v	0.84 (3)	2.05 (3)	2.881 (3)	170 (4)
O4-H4O1^vii	0.85 (3)	1.85 (3)	2.695 (3)	175 (3)
O5-H5O8^viii	0.87 (3)	1.85 (3)	2.719 (3)	172 (3)
O6-H6O9^ix	0.83 (3)	1.90 (2)	2.722 (3)	171 (3)
C2-H2CO1^x	0.97	2.60	3.162 (3)	117
C4-H4BO5ⁱ	0.97	2.43	3.256 (4)	142
C5-H5BO11^xi	0.97	2.31	3.265 (4)	168
Symmetry codes: (i) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1]$ ; (ii) -x, -y+1, -z+1; (iii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iv) x, y, z+1; (v) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (vi) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (vii) $[-x, y, -z+{\script{1\over 2}}]$ ; (viii) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ix) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (x) $[x, -y, z+{\script{1\over 2}}]$ ; (xi) $[x, -y+1, z+{\script{1\over 2}}]$ .

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: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (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: BV2159 ).

References

Averbuch-Pouchot, M. T. & Durif, A. (1987a). Acta Cryst. C43, 1245-1247.
Averbuch-Pouchot, M. T. & Durif, A. (1987b). C. R. Acad. Sci. Ser. 2, 304, 269-271.
Blessing, R. H. (1986). Acta Cryst. B42, 613-621.
Brown, I. D. (1976). Acta Cryst. A32, 24-31.
Chabchoub, N., Darriet, J. & Khemakhem, H. (2006). J. Solid State Chem. 1792, 164-2173.
Durif, A. (1995). In Crystal Chemistry of Condensed Phosphates. New York: Plenum Press.
Durif, A., Averbuch-Pouchot, M. T. & Guitel, J. C. (1982). J. Solid State Chem. 41, 153-159.
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.
Khemakhem, H. (1999). Ferroelectrics, 234, 47-59.
Ondik, H. M. (1964). Acta Cryst. 17, 1139-1145.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Wilkinson, H. S. & Harrison, W. T. A. (2006). Acta Cryst. E62, m1397-m1399.

organic compounds