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Volume 68 
Part 11 
Pages m1321-m1322  
November 2012  

Received 25 September 2012
Accepted 28 September 2012
Online 3 October 2012

Key indicators
Single-crystal X-ray study
T = 180 K
Mean [sigma](C-C) = 0.004 Å
R = 0.023
wR = 0.056
Data-to-parameter ratio = 22.7
Details
Open access

Bis[4-(dimethylamino)pyridinium] octaaquachloridolanthanum(III) tetrachloride trihydrate

aUnité de Recherche de Chimie de l'Environnement et Moléculaire Structurale, Faculté des Sciences Exactes, Département de Chimie, Université Mentouri de Constantine, 25000 Constantine, Algeria, and bLaboratoire de Chimie de Coordination, UPR-CNRS 8241, 205 route de Narbonne, 31077 Toulouse Cedex 4, France
Correspondence e-mail: b_meriem80@yahoo.fr

The title organic-inorganic salt, (C7H11N2)2[LaCl(H2O)8]Cl4·3H2O, consists of two 4-(dimethylamino)pyridinium and one [La(H2O)8Cl]2+ cations, four chloride anions and three solvent water molecules. In the crystal, the various units are connected by N-H...Cl, O-H...Cl, O-H...O and N-H...O hydrogen bonds, forming a network of alternating organic and inorganic layers. The 4-(dimethylamino)pyridinium cations stack along the c axis, while the inorganic layers lie parallel to the ac plane. The chloride anions are located between these entities, forming hydrogen bonds with the NH atom of the pyridinium ions and the water molecules. There are also C-H...Cl hydrogen bonds present involving one of the 4-(dimethylamino)pyridinium cations, resulting in the formation of a three-dimensional supramolecular architecture.

Related literature

For common applications of organic-inorganic hybrid materials, see: Cui et al. (2000[Cui, Y., Ren, J., Chen, G., Yu, W.-C. & Qian, Y. (2000). Acta Cryst. C56, e552-e553.]); Lacroix et al. (1994[Lacroix, P. G., Clement, R., Nakatani, K., Zyss, J. & Ledoux, I. (1994). Science, 263, 658-660.]); Chakravarthy & Guloy (1997[Chakravarthy, V. & Guloy, A. M. (1997). Chem. Commun. pp. 697-698.]). For the crystal structures of compounds involving 4-(dimethylamino)pyridinium, see: Chao et al. (1977[Chao, M., Schempp, E. & Rosenstein, D. (1977). Acta Cryst. B33, 1820-1823.]); Mayr-Stein & Bolte (2000[Mayr-Stein, R. & Bolte, M. (2000). Acta Cryst. C56, e19-e20.]); Lo & Ng (2008[Lo, K. M. & Ng, S. W. (2008). Acta Cryst. E64, m800.], 2009[Lo, K. M. & Ng, S. W. (2009). Acta Cryst. E65, m13.]); Koon et al. (2009[Koon, Y. C., Lo, K. M. & Ng, S. W. (2009). Acta Cryst. E65, m663.]). For hydrogen-bond motifs, see: Bernstein et al. (1995[Bernstein, J., Davis, R. E., Shimoni, L. & Chang, N.-L. (1995). Angew. Chem. Int. Ed. Engl. 34, 1555-1573.]).

[Scheme 1]

Experimental

Crystal data
  • (C7H11N2)2[LaCl(H2O)8]Cl4·3H2O

  • Mr = 760.69

  • Triclinic, [P \overline 1]

  • a = 9.6741 (4) Å

  • b = 12.6695 (7) Å

  • c = 14.3601 (7) Å

  • [alpha] = 68.354 (5)°

  • [beta] = 75.273 (4)°

  • [gamma] = 84.264 (4)°

  • V = 1582.16 (15) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 1.82 mm-1

  • T = 180 K

  • 0.43 × 0.28 × 0.08 mm

Data collection
  • Oxford Xcalibur Sapphire1 diffractometer

  • Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011[Agilent (2011). CrysAlis PRO. Agilent Technologies Ltd, Yarnton, England.]) Tmin = 0.548, Tmax = 0.864

  • 33782 measured reflections

  • 7144 independent reflections

  • 6518 reflections with I > 2[sigma](I)

  • Rint = 0.038

Refinement
  • R[F2 > 2[sigma](F2)] = 0.023

  • wR(F2) = 0.056

  • S = 1.11

  • 7144 reflections

  • 320 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.76 e Å-3

  • [Delta][rho]min = -1.03 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N2-H2A...Cl5i 0.86 2.71 3.314 (3) 129
N2-H2A...O1Wii 0.86 2.24 2.909 (3) 134
N4-H4A...Cl4iii 0.86 2.51 3.213 (2) 140
N4-H4A...Cl4iv 0.86 2.77 3.418 (3) 133
O1-H11...Cl2v 0.79 2.46 3.2316 (19) 165
O1-H12...O1Wvi 0.78 2.01 2.784 (2) 167
O2W-H12W...Cl3iii 0.85 2.38 3.222 (2) 169
O3W-H13W...Cl2vii 0.85 2.51 3.293 (2) 153
O2-H21...Cl3viii 0.85 2.32 3.1537 (17) 166
O1W-H21W...Cl1 0.85 2.31 3.1538 (19) 173
O2-H22...Cl4 0.85 2.27 3.1023 (17) 168
O2W-H22W...Cl2 0.85 2.37 3.213 (2) 172
O3W-H23W...Cl2v 0.85 2.34 3.193 (2) 176
O3-H31...Cl4viii 0.84 2.34 3.1471 (17) 160
O3-H32...Cl1vi 0.84 2.36 3.1413 (16) 157
O4-H41...Cl3viii 0.84 2.31 3.1459 (17) 173
O4-H42...O2W 0.85 1.95 2.791 (3) 178
O5-H51...Cl1 0.84 2.38 3.1707 (19) 158
O5-H52...Cl2 0.85 2.43 3.241 (2) 160
O6-H61...Cl4 0.84 2.35 3.1708 (17) 164
O6-H62...Cl1 0.85 2.32 3.1250 (16) 158
O7-H71...Cl5v 0.84 2.46 3.1402 (17) 139
O7-H72...Cl1 0.84 2.41 3.2287 (18) 162
O8-H81...O3W 0.85 1.94 2.786 (3) 172
O8-H82...Cl3 0.84 2.48 3.2711 (19) 156
C11-H11A...Cl3iii 0.93 2.80 3.612 (3) 147
C14-H14B...Cl1 0.96 2.75 3.639 (4) 154
Symmetry codes: (i) x-1, y+1, z; (ii) -x+1, -y+2, -z+1; (iii) x, y-1, z; (iv) -x+1, -y, -z+2; (v) -x+2, -y+1, -z+1; (vi) x+1, y, z; (vii) x, y+1, z; (viii) -x+2, -y+1, -z+2.

Data collection: CrysAlis PRO (Agilent, 2011[Agilent (2011). CrysAlis PRO. Agilent Technologies Ltd, Yarnton, England.]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SIR92 (Altomare et al., 1993[Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEPIII (Burnett & Johnson, 1996[Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.]) and ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: SHELXL97.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2504 ).


Acknowledgements

Technical support (X-ray measurements) from the Laboratory of Coordination Chemistry, UPR-CNRS 8241, Toulouse, is gratefully acknowledged.

References

Agilent (2011). CrysAlis PRO. Agilent Technologies Ltd, Yarnton, England.
Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350.  [CrossRef] [ISI] [details]
Bernstein, J., Davis, R. E., Shimoni, L. & Chang, N.-L. (1995). Angew. Chem. Int. Ed. Engl. 34, 1555-1573.  [CrossRef] [ChemPort] [ISI]
Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.
Chakravarthy, V. & Guloy, A. M. (1997). Chem. Commun. pp. 697-698.  [CSD] [CrossRef]
Chao, M., Schempp, E. & Rosenstein, D. (1977). Acta Cryst. B33, 1820-1823.  [CrossRef] [details] [ISI]
Cui, Y., Ren, J., Chen, G., Yu, W.-C. & Qian, Y. (2000). Acta Cryst. C56, e552-e553.  [CrossRef] [details]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Koon, Y. C., Lo, K. M. & Ng, S. W. (2009). Acta Cryst. E65, m663.  [CSD] [CrossRef] [details]
Lacroix, P. G., Clement, R., Nakatani, K., Zyss, J. & Ledoux, I. (1994). Science, 263, 658-660.  [CrossRef] [PubMed] [ChemPort] [ISI]
Lo, K. M. & Ng, S. W. (2008). Acta Cryst. E64, m800.  [CSD] [CrossRef] [details]
Lo, K. M. & Ng, S. W. (2009). Acta Cryst. E65, m13.  [CSD] [CrossRef] [details]
Mayr-Stein, R. & Bolte, M. (2000). Acta Cryst. C56, e19-e20.  [CSD] [CrossRef] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]


Acta Cryst (2012). E68, m1321-m1322   [ doi:10.1107/S1600536812040901 ]

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