1,4-Diazo­niabicyclo­[2.2.2]octane tetra­chloroiodate(III) chloride

Chen, L.-Z.

doi:10.1107/S1600536810007865

Volume 66
Part 4
Page o788
April 2010

Received 22 January 2010
Accepted 2 March 2010
Online 10 March 2010

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.004 Å
Disorder in main residue
R = 0.019
wR = 0.045
Data-to-parameter ratio = 18.9
Details

1,4-Diazoniabicyclo[2.2.2]octane tetrachloroiodate(III) chloride

Li-Zhuang Chen ^a ^*

^aSchool of Material Science and Engineering, Jiangsu University of Science and Technology, Zhenjiang 212003, People's Republic of China
Correspondence e-mail: clz1977@sina.com

In the title compound, C₆H₁₄N₂²⁺·Cl₄I^-·Cl^-, the dication and the anions lie on special positions. The dication has mm2 symmetry with two bonded C atoms and the two N atoms located on a crystallographic mirror plane parallel to bc, and with a mirror plane parallel to ab passing through the mid points of the three C-C bonds. In the square-planar Cl₄I^- anion, two Cl atoms and the I atom are located on the mm2 axis; the other two Cl atoms are disordered over two postions of equal occupancy (0.25) across the mirror parallel to the ab plane. The Cl^- anion is located on the mm2 axis. The crystal structure is stabilized by intermolecular N-HCl hydrogen bonds.

Related literature

For ferroelectric materials, see: Scott (2007); Katrusiak & Szafranski (2006).

Experimental

Crystal data

C₆H₁₄N₂²⁺·Cl₄I^-·Cl^-
M_r = 418.34
Orthorhombic, C m c m
a = 8.1496 (16) Å
b = 21.904 (4) Å
c = 7.7184 (15) Å
V = 1377.8 (5) Å³
Z = 4
Mo K radiation
= 3.26 mm^-1
T = 293 K
0.28 × 0.25 × 0.20 mm

Data collection

Rigaku SCXmini diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005) T_min = 0.85, T_max = 0.90
7175 measured reflections
908 independent reflections
882 reflections with I > 2(I)
R_int = 0.028

Refinement

R[F² > 2(F²)] = 0.019
wR(F²) = 0.045
S = 1.25
908 reflections
48 parameters
H-atom parameters constrained
_max = 0.44 e Å^-3
_min = -0.41 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1Cl4ⁱ	0.91	2.29	3.028 (2)	138
Symmetry code: (i) x, y, z+1.

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: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: PV2257 ).

Acknowledgements

This work was supported by a start-up grant from Jiangsu University of Science and Technology

References

Katrusiak, A. & Szafranski, M. (2006). J. Am. Chem. Soc. 128, 15775-15785
Rigaku (2005). CrystalClear. Rigaku Corporation, Tokyo, Japan.
Scott, J. F. (2007). Science, 315, 954-959.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

organic compounds