Bis(4-ethoxy­anilinium) sulfate trihydrate

Fu, X.

doi:10.1107/S1600536809036290

Volume 65
Part 10
Page o2520
October 2009

Received 7 September 2009
Accepted 8 September 2009
Online 26 September 2009

Key indicators
Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.003 Å
R = 0.054
wR = 0.143
Data-to-parameter ratio = 17.1
Details

Bis(4-ethoxyanilinium) sulfate trihydrate

Xue-qun Fu ^a ^*

^aOrdered Matter Science Research Center, Southeast University, Nanjing 210096, People's Republic of China
Correspondence e-mail: fuxuequn222@163.com

The structure of the title compound, 2C₈H₁₂NO⁺·SO₄^2-·3H₂O, consists of organic layers, water molecules and SO₄^2- anions which lie within the organic layers. In the crystal, intermolecular N-HO, N-HS O-HO and O-HS hydrogen bonds, some of which are bifurcated, stabilize the structure.

Related literature

For background to this study, see: Hang et al. (2009); Li et al. (2008).

Experimental

Crystal data

2C₈H₁₂NO⁺·SO₄^2-·3H₂O
M_r = 426.48
Triclinic, $[P \overline 1]$
a = 7.0455 (14) Å
b = 10.969 (2) Å
c = 13.787 (3) Å
= 101.40 (3)°
= 94.53 (3)°
= 90.18 (3)°
V = 1041.0 (4) Å³
Z = 2
Mo K radiation
= 0.21 mm^-1
T = 298 K
0.20 × 0.20 × 0.20 mm

Data collection

Rigaku SCXmini diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005) T_min = 0.96, T_max = 0.96
10835 measured reflections
4748 independent reflections
3947 reflections with I > 2(I)
R_int = 0.041

Refinement

R[F² > 2(F²)] = 0.054
wR(F²) = 0.143
S = 1.10
4748 reflections
277 parameters
H atoms treated by a mixture of independent and constrained refinement
_max = 0.30 e Å^-3
_min = -0.62 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N2-H2CO1ⁱ	0.89	2.05	2.870 (2)	153
N2-H2CS1ⁱ	0.89	2.77	3.649 (2)	172
N2-H2DO2ⁱⁱ	0.89	2.07	2.788 (2)	137
N2-H2EO7Wⁱⁱⁱ	0.89	1.94	2.819 (3)	169
N1-H1DO8Wⁱⁱⁱ	0.89	2.14	2.823 (2)	133
N1-H1DO9Wⁱⁱ	0.89	2.46	3.166 (3)	136
N1-H1EO3ⁱⁱ	0.89	1.93	2.785 (2)	162
N1-H1FO1^iv	0.89	2.03	2.849 (2)	152
O7W-H7DO4^v	0.81 (4)	2.11 (4)	2.893 (3)	163 (3)
O8W-H8DO4^vi	0.75 (3)	2.12 (3)	2.864 (3)	172 (3)
O9W-H9EO1^vii	0.92 (4)	2.07 (4)	2.991 (3)	175 (4)
O9W-H9ES1^vii	0.92 (4)	2.98 (4)	3.791 (2)	147 (3)
O7W-H7CO2	0.83 (4)	2.05 (4)	2.851 (3)	164 (3)
O8W-H8CO3	0.90 (4)	1.94 (4)	2.815 (3)	164 (3)
O8W-H8CS1	0.90 (4)	3.02 (4)	3.852 (2)	154 (3)
O9W-H9DO4	1.03 (5)	2.00 (5)	2.981 (3)	158 (4)
O9W-H9DS1	1.03 (5)	2.81 (5)	3.547 (2)	129 (3)
Symmetry codes: (i) x-1, y, z-1; (ii) -x+1, -y+1, -z+1; (iii) -x+2, -y+1, -z+1; (iv) x-1, y-1, z-1; (v) -x+2, -y+1, -z+2; (vi) -x+2, -y+2, -z+2; (vii) x-1, y, z.

Data collection: CrystalClear (Rigaku, 2005); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: PRPKAPPA (Ferguson, 1999).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: JH2104 ).

Acknowledgements

The author is grateful to the starter fund of Southeast University for financial support to buy the X-ray diffractometer.

References

Ferguson, G. (1999). PRPKAPPA. University of Guelph, Canada.
Hang, T., Fu, D. W., Ye, Q. & Xiong, R. G. (2009). Cryst. Growth Des. 5, 2026-2029.
Li, X. Z., Qu, Z. R. & Xiong, R. G. (2008). Chin. J. Chem. 11, 1959-1962.
Rigaku (2005). CrystalClear. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

organic compounds