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Volume 68 
Part 11 
Pages m1342-m1343  
November 2012  

Received 28 September 2012
Accepted 5 October 2012
Online 10 October 2012

Key indicators
Single-crystal X-ray study
T = 180 K
Mean [sigma](C-C) = 0.007 Å
Disorder in solvent or counterion
R = 0.029
wR = 0.068
Data-to-parameter ratio = 21.7
Details
Open access

Tris[4-(dimethylamino)pyridinium][(bis-[mu]-dichlorido)-decaaquadichloridodineodymium(III)] pentachloride dihydrate

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 compound, (C7H11N2)3[Nd2Cl4(H2O)10]Cl5·2H2O, consists of three 4-(dimethylamino)pyridinium cations, one of which is disordered about an inversion center, one [Nd2Cl4(H2O)10]2+ dication possessing inversion symmetry, five chloride anions, one of which is disordered over two inversion centers, and two lattice water molecules. The 4-(dimethylamino)pyridinium cations are protonated at the pyridine N atoms and form N-H...Cl hydrogen bonds with Cl- counter-ions. The dimethylamino groups (C/N/C) lie close to the plane of the pyridinium rings, making dihedral angles of 1.6 (6)° and 6.5 (3)°. In the crystal, the [Nd2Cl4(H2O)10]2+ dications are linked via O-H...O and O-H...Cl hydrogen bonds, forming sheets lying parallel to the bc plane. These sheets are linked via O-H...Cl hydrogen bonds, forming a three-dimensional network. The 4-(dimethylamino)pyridinium cations are located in the cavities and linked to the framework by C-H...Cl interactions.

Related literature

For the crystal structures of complexes 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.]); Benslimane et al. (2012[Benslimane, M., Merazig, H., Daran, J.-C. & Zeghouan, O. (2012). Acta Cryst. E68, m1321-m1322.]). 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)3[Nd2Cl4(H2O)10]Cl5·2H2O

  • Mr = 1193.26

  • Triclinic, [P \overline 1]

  • a = 9.5172 (4) Å

  • b = 10.7739 (5) Å

  • c = 11.9976 (5) Å

  • [alpha] = 74.855 (4)°

  • [beta] = 69.780 (4)°

  • [gamma] = 85.075 (4)°

  • V = 1114.28 (8) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 2.90 mm-1

  • T = 180 K

  • 0.36 × 0.22 × 0.16 mm

Data collection
  • Agilent Xcalibur Sapphire1 diffractometer

  • Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011[Agilent (2011). CrysAlis PRO. Agilent Technologies Ltd, Yarnton, England.]) Tmin = 0.475, Tmax = 0.633

  • 23060 measured reflections

  • 4551 independent reflections

  • 4088 reflections with I > 2[sigma](I)

  • Rint = 0.034

Refinement
  • R[F2 > 2[sigma](F2)] = 0.029

  • wR(F2) = 0.068

  • S = 1.11

  • 4551 reflections

  • 210 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.95 e Å-3

  • [Delta][rho]min = -1.76 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O11-H111...Cl4i 0.85 2.16 3.010 (3) 177
O11-H112...Cl11ii 0.85 2.30 3.149 (4) 173
O12-H121...Cl6iii 0.85 2.24 3.080 (3) 168
O12-H122...Cl3iv 0.85 2.25 3.089 (3) 171
O13-H131...O11 0.85 2.19 2.738 (6) 122
O13-H131...Cl4i 0.85 2.99 3.631 (6) 134
O13-H132...Cl4 0.85 2.16 3.005 (4) 172
O14-H142...Cl4iv 0.85 2.46 3.159 (4) 140
O14-H142...Cl11 0.85 2.73 3.210 (4) 118
O15-H151...O1W 0.85 1.84 2.683 (4) 172
O15-H152...Cl3 0.85 2.26 3.109 (3) 175
N12-H12...Cl11v 0.88 2.65 3.358 (5) 138
N12-H12...Cl11 0.88 2.78 3.451 (5) 134
O1W-H11W...Cl3vi 0.85 2.35 3.197 (3) 179
O1W-H12W...Cl6 0.85 2.52 3.349 (3) 167
N32-H32A...Cl4 0.88 2.26 3.0808 (16) 156
C34-H34...Cl1i 0.95 2.82 3.703 (3) 155
Symmetry codes: (i) -x, -y+1, -z+1; (ii) -x+1, -y+1, -z; (iii) x, y+1, z; (iv) -x+1, -y+1, -z+1; (v) -x+2, -y+1, -z; (vi) -x+1, -y, -z+1.

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: SU2506 ).


Acknowledgements

The authors acknowledge technical support (X-ray measurements) by the Laboratory of Coordination Chemistry, UPR-CNRS 8241,Toulouse.

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]
Benslimane, M., Merazig, H., Daran, J.-C. & Zeghouan, O. (2012). Acta Cryst. E68, m1321-m1322.  [CrossRef] [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.
Chao, M., Schempp, E. & Rosenstein, D. (1977). Acta Cryst. B33, 1820-1823.  [CrossRef] [details] [ISI]
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]
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, m1342-m1343   [ doi:10.1107/S1600536812041724 ]

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