(IUCr) Bis(4-chlorobenzylammonium) tetrakis(2,6-diethylanilinium) cyclohexaphosphate tetrahydrate

Volume 65
Part 3
Page o654
March 2009

Received 21 February 2009
Accepted 23 February 2009
Online 28 February 2009

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.005 Å
R = 0.053
wR = 0.144
Data-to-parameter ratio = 20.3
Details

Bis(4-chlorobenzylammonium) tetrakis(2,6-diethylanilinium) cyclohexaphosphate tetrahydrate

Olfa Amri,^a Sonia Abid ^a ^* and Mohamed Rzaigui ^a

^aLaboratoire de Chimie des Matériaux, Faculté des Sciences de Bizerte, 7021 Zarzouna Bizerte, Tunisia
Correspondence e-mail: sonia.abid@fsb.rnu.tn

In the crystal of the title hydrated molecular salt, 2C₇H₉ClN⁺·4C₁₀H₁₆N⁺·P₆O₁₈^6-·4H₂O, the packing consists of a three-dimensional O-HO and N-HO hydrogen-bonded network resulting from the association of anionic layers built up from centrosymmetric cyclohexaphosphate ions and water molecules and the two types of organic cations.

Related literature

For related structures, see: Amri et al. (2007, 2008); Marouani & Rzaigui (2002). For background, see: Kresge et al. (1992); Katsoulis (1998).

Experimental

Crystal data

2C₇H₉ClN⁺·4C₁₀H₁₆N⁺·P₆O₁₈^6-·4H₂O
M_r = 1432.04
Monoclinic, C 2/c
a = 31.437 (2) Å
b = 14.178 (2) Å
c = 16.034 (2) Å
= 99.60 (2)°
V = 7046.5 (14) Å³
Z = 4
Mo K radiation
= 0.30 mm^-1
T = 293 K
0.20 × 0.18 × 0.16 mm

Data collection

Enraf-Nonius TurboCAD-4 diffractometer
Absorption correction: none
11637 measured reflections
8452 independent reflections
5321 reflections with I > 2(I)
R_int = 0.035
2 standard reflections frequency: 120 min intensity decay: 5%

Refinement

R[F² > 2(F²)] = 0.053
wR(F²) = 0.144
S = 1.02
8452 reflections
417 parameters
H-atom parameters not refined
_max = 0.57 e Å^-3
_min = -0.44 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1AO9ⁱ	0.89	1.80	2.685 (3)	171
N1-H1BO2	0.89	2.03	2.758 (3)	138
N1-H1CO4	0.89	2.13	2.935 (3)	151
N2-H2AO4ⁱⁱ	0.89	1.94	2.827 (3)	172
N2-H2BO1	0.89	2.05	2.887 (3)	156
N2-H2CO7	0.89	1.94	2.809 (3)	166
N3-H3AO5ⁱⁱⁱ	0.89	1.89	2.762 (3)	165
N3-H3BO9	0.89	1.93	2.799 (3)	164
N3-H3CO10	0.89	1.99	2.800 (5)	151
O10-H1O11	0.85	2.22	2.923 (6)	140
O10-H2O11^iv	0.86	2.25	2.831 (5)	125
O11-H6O2^v	0.85	2.23	2.740 (4)	118
O11-H7O5ⁱⁱⁱ	0.85	2.17	2.781 (4)	129
Symmetry codes: (i) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1]$ ; (iii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iv) $[-x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1]$ ; (v) x, y+1, z.

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); 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: HB2918 ).

References

Amri, O., Abid, S. & Rzaigui, M. (2007). Cryst. Res. Technol. 42, 930-936.
Amri, O., Abid, S. & Rzaigui, M. (2008). Phosphorus Sulfur Silicon Relat. Elem. 183, 1984-1993.
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. (1995). XCAD4. University of Marburg, Germany.
Katsoulis, D. E. (1998). Chem. Rev. 98, 359-387.
Kresge, C. T., Leonowicz, M. E., Roth, W. J., Vartuli, J. C. & Beck, J. S. (1992). Nature (London), 359, 710-712.
Marouani, H. & Rzaigui, M. (2002). Z. Kristallogr. New Cryst. Struct. 217, 277-278.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

organic compounds