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

Benslimane, M.; Merazig, H.; Daran, J.-C.; Zeghouan, O.

doi:10.1107/S1600536812041724

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 (C-C) = 0.007 Å
Disorder in solvent or counterion
R = 0.029
wR = 0.068
Data-to-parameter ratio = 21.7
Details

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

Meriem Benslimane,^a ^* Hocine Merazig,^a Jean-Claude Daran ^b and Ouahida Zeghouan ^a

^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-HCl 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-HO and O-HCl hydrogen bonds, forming sheets lying parallel to the bc plane. These sheets are linked via O-HCl hydrogen bonds, forming a three-dimensional network. The 4-(dimethylamino)pyridinium cations are located in the cavities and linked to the framework by C-HCl interactions.

Related literature

For the crystal structures of complexes involving 4-(dimethylamino)pyridinium, see: Chao et al. (1977); Mayr-Stein & Bolte (2000); Lo & Ng (2008, 2009); Koon et al. (2009); Benslimane et al. (2012). For hydrogen-bond motifs, see: Bernstein et al. (1995).

Experimental

Crystal data

(C₇H₁₁N₂)₃[Nd₂Cl₄(H₂O)₁₀]Cl₅·2H₂O
M_r = 1193.26
Triclinic, $[P \overline 1]$
a = 9.5172 (4) Å
b = 10.7739 (5) Å
c = 11.9976 (5) Å
= 74.855 (4)°
= 69.780 (4)°
= 85.075 (4)°
V = 1114.28 (8) Å³
Z = 1
Mo K radiation
= 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) T_min = 0.475, T_max = 0.633
23060 measured reflections
4551 independent reflections
4088 reflections with I > 2(I)
R_int = 0.034

Refinement

R[F² > 2(F²)] = 0.029
wR(F²) = 0.068
S = 1.11
4551 reflections
210 parameters
H-atom parameters constrained
_max = 0.95 e Å^-3
_min = -1.76 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O11-H111Cl4ⁱ	0.85	2.16	3.010 (3)	177
O11-H112Cl11ⁱⁱ	0.85	2.30	3.149 (4)	173
O12-H121Cl6ⁱⁱⁱ	0.85	2.24	3.080 (3)	168
O12-H122Cl3^iv	0.85	2.25	3.089 (3)	171
O13-H131O11	0.85	2.19	2.738 (6)	122
O13-H131Cl4ⁱ	0.85	2.99	3.631 (6)	134
O13-H132Cl4	0.85	2.16	3.005 (4)	172
O14-H142Cl4^iv	0.85	2.46	3.159 (4)	140
O14-H142Cl11	0.85	2.73	3.210 (4)	118
O15-H151O1W	0.85	1.84	2.683 (4)	172
O15-H152Cl3	0.85	2.26	3.109 (3)	175
N12-H12Cl11^v	0.88	2.65	3.358 (5)	138
N12-H12Cl11	0.88	2.78	3.451 (5)	134
O1W-H11WCl3^vi	0.85	2.35	3.197 (3)	179
O1W-H12WCl6	0.85	2.52	3.349 (3)	167
N32-H32ACl4	0.88	2.26	3.0808 (16)	156
C34-H34Cl1ⁱ	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); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 2012); 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.
Benslimane, M., Merazig, H., Daran, J.-C. & Zeghouan, O. (2012). Acta Cryst. E68, m1321-m1322.
Bernstein, J., Davis, R. E., Shimoni, L. & Chang, N.-L. (1995). Angew. Chem. Int. Ed. Engl. 34, 1555-1573.
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.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
Koon, Y. C., Lo, K. M. & Ng, S. W. (2009). Acta Cryst. E65, m663.
Lo, K. M. & Ng, S. W. (2008). Acta Cryst. E64, m800.
Lo, K. M. & Ng, S. W. (2009). Acta Cryst. E65, m13.
Mayr-Stein, R. & Bolte, M. (2000). Acta Cryst. C56, e19-e20.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.