4-(Dimethyl­amino)­pyridinium octa­aqua­erbium(III) tetra­chloride monohydrate

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

doi:10.1107/S1600536812043048

Volume 68
Part 11
Pages m1388-m1389
November 2012

Received 10 October 2012
Accepted 15 October 2012
Online 20 October 2012

Key indicators
Single-crystal X-ray study
T = 180 K
Mean (C-C) = 0.004 Å
R = 0.015
wR = 0.038
Data-to-parameter ratio = 20.5
Details

4-(Dimethylamino)pyridinium octaaquaerbium(III) tetrachloride monohydrate

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

In the title compound, (C₇H₁₁N₂)[Er(H₂O)₈]Cl₄·H₂O, the asymmetric unit consists of one 4-(dimethylamino)pyridinium and one octaaquaerbium cation balanced by four Cl^- anions, and one water molecule. The 4-(dimethylamino)pyridinium cation is protonated at the pyridine N atom. The dimethylamino group (C/N/C) lies close to the plane of the pyridinium ring, making a dihedral angle of 4.5 (3)°. In the crystal, the [Er(H₂O)₈]³⁺ cations are linked via O-HO and O-HCl hydrogen bonds, forming two-dimensional networks propagating in the ab plane. These networks are linked via O-HO and O-HCl hydrogen bonds, forming a three-dimensional network. The 4-(dimethylamino)pyridinium cations are located in the cavities and are linked to the framework via N-HCl, C-HO and C-HCl hydrogen bonds.

Related literature

For similar structures in this series involving 4-(dimethylamino)pyridinium, see: Benslimane et al. (2012a,b). For details of the Cambridge Structural Database, see: Allen (2002). For hydrogen-bond motifs see: Bernstein et al. (1995).

Experimental

Crystal data

(C₇H₁₁N₂)[Er(H₂O)₈]Cl₄·H₂O
M_r = 594.38
Triclinic, $[P \overline 1]$
a = 7.8775 (3) Å
b = 9.3601 (4) Å
c = 15.2593 (6) Å
= 105.831 (3)°
= 101.498 (3)°
= 90.919 (3)°
V = 1057.77 (8) Å³
Z = 2
Mo K radiation
= 4.51 mm^-1
T = 180 K
0.35 × 0.17 × 0.09 mm

Data collection

Agilent Xcalibur Sapphire1 diffractometer
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011) T_min = 0.415, T_max = 0.666
21843 measured reflections
4315 independent reflections
4110 reflections with I > 2(I)
R_int = 0.031

Refinement

R[F² > 2(F²)] = 0.015
wR(F²) = 0.038
S = 1.12
4315 reflections
210 parameters
H-atom parameters constrained
_max = 0.38 e Å^-3
_min = -0.84 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1Cl1	0.86	2.53	3.229 (2)	139
O1W-H1WCl3ⁱ	0.85	2.44	3.2686 (18)	165
O1W-H2WCl3ⁱⁱ	0.85	2.25	3.0874 (18)	171
O1-H11Cl4ⁱⁱⁱ	0.85	2.29	3.1036 (18)	160
O1-H12Cl1	0.85	2.24	3.0863 (17)	172
O2-H21Cl1	0.85	2.25	3.0708 (17)	164
O2-H22Cl2	0.84	2.31	3.1372 (17)	167
O3-H31O1W	0.85	1.82	2.671 (2)	177
O3-H32Cl3	0.84	2.37	3.1826 (17)	162
O4-H41Cl4	0.85	2.25	3.0925 (17)	169
O4-H42Cl2	0.85	2.23	3.0685 (16)	168
O5-H51Cl4	0.85	2.33	3.1469 (18)	160
O5-H52Cl2^iv	0.85	2.27	3.0819 (18)	161
O6-H61Cl4^v	0.85	2.27	3.1164 (17)	171
O6-H62Cl1^vi	0.85	2.25	3.0858 (17)	169
O7-H71Cl3	0.84	2.19	3.0304 (18)	173
O7-H72Cl1^iv	0.85	2.30	3.1132 (18)	159
O8-H81Cl4^vii	0.85	2.29	3.1377 (17)	173
O8-H82Cl2^vii	0.85	2.31	3.1464 (17)	166
C2-H2Cl3^viii	0.93	2.77	3.683 (3)	169
C3-H3O1Wⁱⁱⁱ	0.93	2.51	3.332 (3)	148
C6-H6BO4ⁱⁱ	0.96	2.47	3.379 (3)	158
Symmetry codes: (i) x-1, y, z; (ii) -x+2, -y+1, -z+1; (iii) x, y-1, z; (iv) x+1, y, z; (v) -x+2, -y+1, -z; (vi) -x+1, -y, -z; (vii) -x+1, -y+1, -z; (viii) -x+2, -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: SU2511 ).

Acknowledgements

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

References

Agilent (2011). CrysAlis PRO. Agilent Technologies Ltd, Yarnton, England.
Allen, F. H. (2002). Acta Cryst. B58, 380-388.
Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350.
Benslimane, M., Merazig, H., Daran, J.-C. & Zeghouan, O. (2012a). Acta Cryst. E68, m1321-m1322.
Benslimane, M., Merazig, H., Daran, J.-C. & Zeghouan, O. (2012b). Acta Cryst. E68, m1342-m1343.
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.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds