[Journal logo]

Volume 69 
Part 6 
Pages m305-m306  
June 2013  

Received 9 April 2013
Accepted 29 April 2013
Online 11 May 2013

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](C-C) = 0.003 Å
R = 0.050
wR = 0.128
Data-to-parameter ratio = 32.0
Details
Open access

Poly[bis(piperazine-1,4-diium) [([mu]4-cyclo-hexaphosphato)dilithium] tetrahydrate]

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: sonia.abid@fsb.rnu.tn

In the title compound, {(C4H12N2)2[Li2(P6O18)]·4H2O}n, the phosphate ring anion, located around an inversion center, adopts a chair conformation. Adjacent P6O18 rings are linked via corner-sharing by LiO4 tetrahedra, generating anionic porous {[Li2(P6O18)]4-}n layers parallel to (101). The piperazine-1,4-diium cations occupy the pores and develop hydrogen bonds with the inorganic framework. An extensive network of N-H...O and O-H...O hydrogen-bonding interactions link the components into a three-dimensional network and additional stabilization is provided by weak C-H...O hydrogen bonds.

Related literature

For applications of compounds with open-framework structures, see: Assani et al. (2012[Assani, A., Saadi, M., Zriouil, M. & El Ammari, L. (2012). Acta Cryst. E68, i30.]); Mahesh et al. (2002[Mahesh, S., Green, M. A. & Natarajan, S. (2002). J. Solid State Chem. 165, 334-342.]); Natarajan (2000[Natarajan, S. (2000). Proc. Indian Acad. Sci. Chem. Sci. 112, 249-272.]). For related structures with cyclohexaphosphate rings, see: Abid et al. (2011[Abid, S., Al-Deyab, S. S. & Rzaigui, M. (2011). Acta Cryst. E67, m1549-m1550.]), Amri et al. (2009[Amri, O., Abid, S. & Rzaigui, M. (2009). Acta Cryst. E65, o654.]); Marouani et al. (2010[Marouani, H., Rzaigui, M. & Al-Deyab, S. S. (2010). Acta Cryst. E66, o702.]); For related structures with piperazine rings, see: Essid et al. (2010[Essid, M., Marouani, H., Rzaigui, M. & Al-Deyab, S. S. (2010). Acta Cryst. E66, o2244-o2245.]), Xu et al. (2007[Xu, H., Dong, P., Liu, L., Wang, J.-G., Deng, F. & Dong, J.-X. (2007). J. Porous Mater. 14, 97-101.]). For the synthesis of the precursor, see: Schülke & Kayser (1985[Schülke, U. & Kayser, R. (1985). Z. Anorg. Allg. Chem. 531, 167-175.]).

[Scheme 1]

Experimental

Crystal data
  • (C4H12N2)2[Li2(P6O18)]·4H2O

  • Mr = 736.08

  • Monoclinic, P 21 /c

  • a = 10.245 (3) Å

  • b = 12.966 (4) Å

  • c = 10.910 (4) Å

  • [beta] = 111.00 (3)°

  • V = 1352.8 (7) Å3

  • Z = 2

  • Ag K[alpha] radiation

  • [lambda] = 0.56085 Å

  • [mu] = 0.26 mm-1

  • T = 293 K

  • 0.50 × 0.40 × 0.30 mm

Data collection
  • Enraf-Nonius CAD-4 diffractometer

  • 7884 measured reflections

  • 6469 independent reflections

  • 3904 reflections with I > 2[sigma](I)

  • Rint = 0.038

  • 2 standard reflections every 120 min intensity decay: 1%

Refinement
  • R[F2 > 2[sigma](F2)] = 0.050

  • wR(F2) = 0.128

  • S = 1.00

  • 6469 reflections

  • 202 parameters

  • 6 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.57 e Å-3

  • [Delta][rho]min = -0.47 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H2A...O8 0.90 1.99 2.792 (3) 147
N1-H2B...O7i 0.90 1.88 2.763 (3) 166
N2-H3A...O11 0.90 1.83 2.707 (4) 165
N2-H3B...O4ii 0.90 1.91 2.802 (2) 168
O10-H110...O1iii 0.84 (4) 1.99 (4) 2.792 (4) 159 (5)
O11-H111...O5iii 0.84 (3) 2.49 (4) 3.001 (3) 120 (3)
O11-H111...O8iii 0.84 (3) 2.07 (3) 2.826 (3) 150 (4)
O10-H210...O5i 0.82 (4) 1.95 (4) 2.764 (3) 170 (4)
O11-H211...O10iii 0.86 (4) 1.87 (4) 2.720 (4) 170 (4)
C1-H1A...O6iv 0.97 2.51 3.273 (4) 135
C4-H1D...O10 0.97 2.56 3.227 (4) 126
C2-H2C...O2v 0.97 2.29 3.078 (3) 137
C3-H4B...O5iii 0.97 2.46 3.324 (4) 148
Symmetry codes: (i) [x, -y+{\script{5\over 2}}, z-{\script{1\over 2}}]; (ii) x, y, z-1; (iii) -x+2, -y+2, -z; (iv) -x+1, -y+2, -z; (v) [x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}].

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994[Enraf-Nonius (1994). CAD-4 EXPRESS. Enraf-Nonius, Delft, The Netherlands.]); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995[Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.]); program(s) used to solve structure: SHELXS86 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: PK2476 ).


Acknowledgements

This work was supported by the Tunisian Ministry of HEScR and the Deanship of Scientific Research at King Saud University (research group project No. RGP-VPP-089).

References

Abid, S., Al-Deyab, S. S. & Rzaigui, M. (2011). Acta Cryst. E67, m1549-m1550.  [CSD] [CrossRef] [ChemPort] [details]
Amri, O., Abid, S. & Rzaigui, M. (2009). Acta Cryst. E65, o654.  [CSD] [CrossRef] [details]
Assani, A., Saadi, M., Zriouil, M. & El Ammari, L. (2012). Acta Cryst. E68, i30.  [CrossRef] [details]
Enraf-Nonius (1994). CAD-4 EXPRESS. Enraf-Nonius, Delft, The Netherlands.
Essid, M., Marouani, H., Rzaigui, M. & Al-Deyab, S. S. (2010). Acta Cryst. E66, o2244-o2245.  [CSD] [CrossRef] [ChemPort] [details]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.
Mahesh, S., Green, M. A. & Natarajan, S. (2002). J. Solid State Chem. 165, 334-342.  [ISI] [CrossRef] [ChemPort]
Marouani, H., Rzaigui, M. & Al-Deyab, S. S. (2010). Acta Cryst. E66, o702.  [CSD] [CrossRef] [details]
Natarajan, S. (2000). Proc. Indian Acad. Sci. Chem. Sci. 112, 249-272.  [CrossRef] [ChemPort]
Schülke, U. & Kayser, R. (1985). Z. Anorg. Allg. Chem. 531, 167-175.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]
Xu, H., Dong, P., Liu, L., Wang, J.-G., Deng, F. & Dong, J.-X. (2007). J. Porous Mater. 14, 97-101.  [ISI] [CrossRef] [ChemPort]


Acta Cryst (2013). E69, m305-m306   [ doi:10.1107/S1600536813011756 ]

This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.