Tetra­kis(4-chloro­anilinium) hexa­chlorido­stannate(IV) dichloride

Benhua Zhou; Hongxia Liu

doi:10.1107/S1600536812021666

. 2012 May 19;68(Pt 6):m782. doi: 10.1107/S1600536812021666

Tetrakis(4-chloroanilinium) hexachloridostannate(IV) dichloride

Benhua Zhou ^a,^*, Hongxia Liu ^a

PMCID: PMC3379112 PMID: 22719333

Abstract

The asymmetric unit of the title compound, (C₆H₇ClN)₄[SnCl₆]Cl₂, comprises two 4-chloroanilinium cations, half of an [SnCl₆]²⁻ anion and a Cl⁻ anion. The Sn^IV atom, located on a special position on a twofold rotation axis, exhibits an octahedral environment. In the crystal, molecules are linked by N—H⋯Cl hydrogen bonds between the 4-chloroanilinium cations, [SnCl₆]²⁻ anions and Cl⁻ anions.

Related literature

For general background to ferroelectric metal-organic frameworks, see: Ye et al. (2009 ▶); Fu et al. (2007 ▶). For phase transitions in ferroelectric materials, see: Zhang et al. (2008 ▶); Zhao et al. (2008 ▶); Ye et al. (2006 ▶). graphic file with name e-68-0m782-scheme1.jpg

Experimental

Crystal data

(C₆H₇ClN)₄[SnCl₆]Cl₂
M _r = 916.59
Monoclinic,
a = 27.855 (6) Å
b = 7.2061 (14) Å
c = 21.895 (4) Å
β = 125.03 (3)°
V = 3598.8 (18) Å³
Z = 4
Mo Kα radiation
μ = 1.63 mm⁻¹
T = 293 K
0.20 × 0.20 × 0.20 mm

Data collection

Rigaku SCXmini diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2005 ▶) T _min = 0.715, T _max = 0.730
17870 measured reflections
4122 independent reflections
3581 reflections with I > 2σ(I)
R _int = 0.031

Refinement

R[F ² > 2σ(F ²)] = 0.030
wR(F ²) = 0.067
S = 1.10
4122 reflections
188 parameters
H-atom parameters constrained
Δρ_max = 0.44 e Å⁻³
Δρ_min = −0.46 e Å⁻³

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: DIAMOND (Brandenburg & Putz, 2005 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812021666/kp2409sup1.cif

e-68-0m782-sup1.cif^{(17.9KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812021666/kp2409Isup2.hkl

e-68-0m782-Isup2.hkl^{(202.1KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Selected bond lengths (Å).

Cl3—Sn1	2.4205 (11)
Cl4—Sn1	2.4076 (7)
Cl5—Sn1	2.4356 (7)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯Cl5ⁱ	0.89	2.64	3.522 (2)	172
N1—H1A⋯Cl3ⁱ	0.89	2.98	3.424 (2)	112
N1—H1B⋯Cl6ⁱⁱ	0.89	2.25	3.123 (3)	165
N1—H1C⋯Cl6ⁱⁱⁱ	0.89	2.26	3.120 (3)	162
N2—H2A⋯Cl3^iv	0.89	2.75	3.455 (2)	137
N2—H2A⋯Cl4^v	0.89	2.79	3.567 (2)	147
N2—H2A⋯Cl4^iv	0.89	2.92	3.344 (3)	111
N2—H2B⋯Cl6^vi	0.89	2.20	3.085 (3)	175
N2—H2C⋯Cl5^vii	0.89	2.61	3.424 (3)	153

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) .

Acknowledgments

The authors are grateful to the starter fund of Southeast University, Nanjing, People’s Republic of China.

supplementary crystallographic information

Comment

The study of ferroelectric materials has received much attention; some of them have predominantly dielectric–ferroelectric performance (Ye et al., 2006; Fu et al., 2007; Zhao et al. 2008; Zhang et al., 2008; Ye et al., 2009). As a part of our work to obtain potential ferroelectric phase-transition material, we report herein on the crystal structure of title compound. Unluckily, the title compound has no dielectric anomalies in the temperature range 93–453 K, suggesting that it might be only a paraelectric.

The asymmetric unit of the title compound is shown in Fig. 1 and Sn-Cl bonds are listed in Table 1. The crystal packing (Fig. 2) is stabilised by intermolecular N—H···Cl hydrogen bonds between the [C₆H₇ClN]⁺cations and SnCl₆^2–anions and Cl^- anions (Table 2).

Experimental

For the preparation of the title compound, the water solution of the hydrochloric acid (10 mmol) was added to the ethanol solution of the 4-chlorobenzenamine(10 mmol), then the water solution of the SnCl₄(5 mmol) was added into a reaction mixture. The resulting precipitate was filtered. Colourless crystals suitable for X-ray analysis were formed after several weeks by slow evaporation of the solvent at room temperature.