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

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

doi:10.1107/S1600536812040901

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 (C-C) = 0.004 Å
R = 0.023
wR = 0.056
Data-to-parameter ratio = 22.7
Details

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

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 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-HCl, O-HCl, O-HO and N-HO 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-HCl 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); Lacroix et al. (1994); Chakravarthy & Guloy (1997). For the crystal structures of compounds involving 4-(dimethylamino)pyridinium, see: Chao et al. (1977); Mayr-Stein & Bolte (2000); Lo & Ng (2008, 2009); Koon et al. (2009). For hydrogen-bond motifs, see: Bernstein et al. (1995).

Experimental

Crystal data

(C₇H₁₁N₂)₂[LaCl(H₂O)₈]Cl₄·3H₂O
M_r = 760.69
Triclinic, $[P \overline 1]$
a = 9.6741 (4) Å
b = 12.6695 (7) Å
c = 14.3601 (7) Å
= 68.354 (5)°
= 75.273 (4)°
= 84.264 (4)°
V = 1582.16 (15) Å³
Z = 2
Mo K radiation
= 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) T_min = 0.548, T_max = 0.864
33782 measured reflections
7144 independent reflections
6518 reflections with I > 2(I)
R_int = 0.038

Refinement

R[F² > 2(F²)] = 0.023
wR(F²) = 0.056
S = 1.11
7144 reflections
320 parameters
H-atom parameters constrained
_max = 0.76 e Å^-3
_min = -1.03 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N2-H2ACl5ⁱ	0.86	2.71	3.314 (3)	129
N2-H2AO1Wⁱⁱ	0.86	2.24	2.909 (3)	134
N4-H4ACl4ⁱⁱⁱ	0.86	2.51	3.213 (2)	140
N4-H4ACl4^iv	0.86	2.77	3.418 (3)	133
O1-H11Cl2^v	0.79	2.46	3.2316 (19)	165
O1-H12O1W^vi	0.78	2.01	2.784 (2)	167
O2W-H12WCl3ⁱⁱⁱ	0.85	2.38	3.222 (2)	169
O3W-H13WCl2^vii	0.85	2.51	3.293 (2)	153
O2-H21Cl3^viii	0.85	2.32	3.1537 (17)	166
O1W-H21WCl1	0.85	2.31	3.1538 (19)	173
O2-H22Cl4	0.85	2.27	3.1023 (17)	168
O2W-H22WCl2	0.85	2.37	3.213 (2)	172
O3W-H23WCl2^v	0.85	2.34	3.193 (2)	176
O3-H31Cl4^viii	0.84	2.34	3.1471 (17)	160
O3-H32Cl1^vi	0.84	2.36	3.1413 (16)	157
O4-H41Cl3^viii	0.84	2.31	3.1459 (17)	173
O4-H42O2W	0.85	1.95	2.791 (3)	178
O5-H51Cl1	0.84	2.38	3.1707 (19)	158
O5-H52Cl2	0.85	2.43	3.241 (2)	160
O6-H61Cl4	0.84	2.35	3.1708 (17)	164
O6-H62Cl1	0.85	2.32	3.1250 (16)	158
O7-H71Cl5^v	0.84	2.46	3.1402 (17)	139
O7-H72Cl1	0.84	2.41	3.2287 (18)	162
O8-H81O3W	0.85	1.94	2.786 (3)	172
O8-H82Cl3	0.84	2.48	3.2711 (19)	156
C11-H11ACl3ⁱⁱⁱ	0.93	2.80	3.612 (3)	147
C14-H14BCl1	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); 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: SU2504 ).

Acknowledgements

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

References

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