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Volume 69 
Part 8 
Pages m452-m453  
August 2013  

Received 12 April 2013
Accepted 5 July 2013
Online 13 July 2013

Key indicators
Single-crystal X-ray study
T = 293 K
Mean [sigma](C-C) = 0.002 Å
Disorder in solvent or counterion
R = 0.030
wR = 0.080
Data-to-parameter ratio = 19.0
Details
Open access

catena-Poly[[[tetraaquamagnesium]-trans-[mu]-[(piperazine-1,4-diium-1,4-diyl)bis(methylene)]diphosphonato] hemihydrate]

aInstitut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Max-Eyth-Strasse 2, 24118 Kiel, Germany
Correspondence e-mail: stock@ac.uni-kiel.de

The structure of the title polymer, }[Mg(C6H14N2O6P2)(H2O)4]·0.5H2O}n, is based on centrosymmetric MgO6 octahedra, which are linked by [(piperazine-1,4-diium-1,4-diyl)bis(methylene)]diphosphonate ligands, forming chains parallel to [1-1-1]. These chains are connected via hydrogen bonds primarily formed between the phosphonate groups and water molecules. The latter constitute four of the corners of the MgO6 polyhedra and bind to the O atoms of the phosphonate groups of neighbouring chains. The lattice water molecule is disordered around an inversion centre, exhibiting an occupancy of 0.25.

Related literature

For related magnesium structures, see: Wharmby et al. (2012[Wharmby, M. T., Pearce, G. M., Mowat, J. P. S., Griffin, J. M., Ashbrook, S. E., Wright, P. A., Schilling, L.-H., Lieb, A., Stock, N., Chavan, S., Bordiga, S., Garcia, E., Pirngruber, G. D., Vreeke, M. & Gora, L. (2012). Microporous Mesoporous Mater. 157, 3-17.]). For related N,N'-piperaziniumbis(methylenephosphonates), see: Choi et al. (1994[Choi, N., Khan, I., Matthews, R. W., McPartlin, M. & Murphy, B. P. (1994). Polyhedron, 13, 847-850.]); Groves et al. (2005a[Groves, J. A., Wright, P. A. & Lightfoot, P. (2005a). Dalton Trans. pp. 2007-2010.],b[Groves, J. A., Wright, P. A. & Lightfoot, P. (2005b). Inorg. Chem. 44, 1736-1739.]); Groves, Stephens et al. (2006[Groves, J. A., Stephens, N. F., Wright, P. A. & Lightfoot, P. (2006). Solid State Sci. 8, 397-403.]); Groves, Miller et al. (2006[Groves, J. A., Miller, S. R., Warrender, S. J., Mellot-Draznieks, C., Lightfoot, P. & Wright, P. A. (2006). Chem. Commun. pp. 3305-3307.]); LaDuca et al. (1996[LaDuca, R., Rose, D., DeBord, J. R. D., Haushalter, R. C., O'Connor, C. J. & Zubieta, J. (1996). J. Solid State Chem. 123, 408-412.]); Serre et al. (2006[Serre, C., Groves, J. A., Lightfoot, P., Slawin, A. M. Z., Wright, P. A., Stock, N., Bein, T., Haouas, M., Taulelle, F. & Férey, G. R. (2006). Chem. Mater. 18, 1451-1457.]); Soghomonian et al. (1995[Soghomonian, V., Diaz, R., Haushalter, R. C., O'Connor, C. J. & Zubieta, J. (1995). Inorg. Chem. 34, 4460-4466.]); Wang et al. (2004[Wang, Y., Bao, S.-S., Xu, W., Chen, J., Gao, S. & Zheng, L.-M. (2004). J. Solid State Chem. 177, 1297-1301.]); Wharmby et al. (2012[Wharmby, M. T., Pearce, G. M., Mowat, J. P. S., Griffin, J. M., Ashbrook, S. E., Wright, P. A., Schilling, L.-H., Lieb, A., Stock, N., Chavan, S., Bordiga, S., Garcia, E., Pirngruber, G. D., Vreeke, M. & Gora, L. (2012). Microporous Mesoporous Mater. 157, 3-17.]). As a result of their flexible coordination behaviour, organic linker molecules containing phosphonate groups allow the synthesis of a multitude of inorganic-organic hybrid materials, see: Gagnon et al. (2012[Gagnon, K. J., Perry, H. P. & Clearfield, A. (2012). Chem. Rev. 112, 1034-1054.]).

[Scheme 1]

Experimental

Crystal data
  • [Mg(C6H14N2O6P2)(H2O)4]·0.5H2O

  • Mr = 377.51

  • Triclinic, [P \overline 1]

  • a = 6.6296 (5) Å

  • b = 6.8074 (6) Å

  • c = 8.7962 (7) Å

  • [alpha] = 94.579 (6)°

  • [beta] = 103.326 (6)°

  • [gamma] = 106.552 (6)°

  • V = 365.75 (5) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 0.40 mm-1

  • T = 293 K

  • 0.21 × 0.12 × 0.04 mm

Data collection
  • Stoe IPSD-2 diffractometer

  • Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008[Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.]) Tmin = 0.886, Tmax = 0.974

  • 6973 measured reflections

  • 1957 independent reflections

  • 1727 reflections with I > 2[sigma](I)

  • Rint = 0.036

Refinement
  • R[F2 > 2[sigma](F2)] = 0.030

  • wR(F2) = 0.080

  • S = 1.01

  • 1957 reflections

  • 103 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.43 e Å-3

  • [Delta][rho]min = -0.43 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1N1...O3i 0.86 1.84 2.6187 (16) 150
O4-H1O4...O3ii 0.82 1.99 2.7956 (15) 166
O4-H2O4...O2 0.82 1.88 2.6733 (17) 164
O5-H1O5...O2iii 0.82 1.89 2.7032 (17) 172
O5-H2O5...O2iv 0.82 1.99 2.7667 (18) 158
Symmetry codes: (i) -x+1, -y+2, -z+2; (ii) -x+1, -y+2, -z+1; (iii) x, y-1, z; (iv) -x, -y+1, -z+1.

Data collection: X-AREA (Stoe & Cie, 2008[Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (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: XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) and DIAMOND Brandenburg (2011[Brandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: XCIF in SHELXTL.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CQ2003 ).


Acknowledgements

We gratefully acknowledge financial support by the DFG (project No. STO-643/2-3) and the State of Schleswig-Holstein.

References

Brandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Choi, N., Khan, I., Matthews, R. W., McPartlin, M. & Murphy, B. P. (1994). Polyhedron, 13, 847-850.  [CrossRef] [ChemPort] [Web of Science]
Gagnon, K. J., Perry, H. P. & Clearfield, A. (2012). Chem. Rev. 112, 1034-1054.  [Web of Science] [CrossRef] [ChemPort] [PubMed]
Groves, J. A., Miller, S. R., Warrender, S. J., Mellot-Draznieks, C., Lightfoot, P. & Wright, P. A. (2006). Chem. Commun. pp. 3305-3307.  [CSD] [CrossRef]
Groves, J. A., Stephens, N. F., Wright, P. A. & Lightfoot, P. (2006). Solid State Sci. 8, 397-403.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Groves, J. A., Wright, P. A. & Lightfoot, P. (2005a). Dalton Trans. pp. 2007-2010.  [CSD] [CrossRef] [PubMed]
Groves, J. A., Wright, P. A. & Lightfoot, P. (2005b). Inorg. Chem. 44, 1736-1739.  [Web of Science] [CSD] [CrossRef] [PubMed] [ChemPort]
LaDuca, R., Rose, D., DeBord, J. R. D., Haushalter, R. C., O'Connor, C. J. & Zubieta, J. (1996). J. Solid State Chem. 123, 408-412.  [CrossRef] [ChemPort] [Web of Science]
Serre, C., Groves, J. A., Lightfoot, P., Slawin, A. M. Z., Wright, P. A., Stock, N., Bein, T., Haouas, M., Taulelle, F. & Férey, G. R. (2006). Chem. Mater. 18, 1451-1457.  [Web of Science] [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Soghomonian, V., Diaz, R., Haushalter, R. C., O'Connor, C. J. & Zubieta, J. (1995). Inorg. Chem. 34, 4460-4466.  [CrossRef] [ChemPort] [Web of Science]
Stoe & Cie (2008). X-AREA, X-RED32 and X-SHAPE. Stoe & Cie, Darmstadt, Germany.
Wang, Y., Bao, S.-S., Xu, W., Chen, J., Gao, S. & Zheng, L.-M. (2004). J. Solid State Chem. 177, 1297-1301.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Wharmby, M. T., Pearce, G. M., Mowat, J. P. S., Griffin, J. M., Ashbrook, S. E., Wright, P. A., Schilling, L.-H., Lieb, A., Stock, N., Chavan, S., Bordiga, S., Garcia, E., Pirngruber, G. D., Vreeke, M. & Gora, L. (2012). Microporous Mesoporous Mater. 157, 3-17.  [Web of Science] [CSD] [CrossRef] [ChemPort]


Acta Cryst (2013). E69, m452-m453   [ doi:10.1107/S1600536813018722 ]

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