Bis(4-acetyl­anilinium) hexa­chlorido­stannate(IV)

Xian-Wang Song; Rui-Ting Xue; Shou-Gang Chen; Yan-Sheng Yin

doi:10.1107/S1600536811015546

. 2011 Apr 29;67(Pt 5):m653. doi: 10.1107/S1600536811015546

Bis(4-acetylanilinium) hexachloridostannate(IV)

Xian-Wang Song ^a, Rui-Ting Xue ^a, Shou-Gang Chen ^a,^*, Yan-Sheng Yin ^a

PMCID: PMC3089185 PMID: 21754357

Abstract

In the title compound, (C₈H₁₀NO)₂[SnCl₆], the Sn^IV atom exists in an octahedral coordination environment. In the crystal, intermolecular N—H⋯O and N—H⋯Cl hydrogen bonds link the cations and anions into a three-dimensional framework.

Related literature

For general background to inorganic–organic hybrid compounds, see: Antonietti & Ozin (2004 ▶); Cong & Yu (2009 ▶); Descazo et al. (2006 ▶); Li et al. (2007 ▶); Sanchez et al. (2005 ▶).

Experimental

Crystal data

(C₈H₁₀NO)₂[SnCl₆]
M _r = 603.73
Monoclinic,
a = 7.2540 (8) Å
b = 12.6481 (13) Å
c = 24.438 (2) Å
β = 93.991 (1)°
V = 2236.7 (4) Å³
Z = 4
Mo Kα radiation
μ = 1.87 mm⁻¹
T = 298 K
0.48 × 0.44 × 0.43 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.467, T _max = 0.500
10422 measured reflections
3929 independent reflections
2996 reflections with I > 2σ(I)
R _int = 0.058

Refinement

R[F ² > 2σ(F ²)] = 0.044
wR(F ²) = 0.112
S = 1.00
3929 reflections
248 parameters
H-atom parameters constrained
Δρ_max = 0.84 e Å⁻³
Δρ_min = −0.83 e Å⁻³

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811015546/ci5184sup1.cif

e-67-0m653-sup1.cif^{(18.4KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811015546/ci5184Isup2.hkl

e-67-0m653-Isup2.hkl^{(192.6KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2A⋯O1ⁱ	0.89	2.06	2.939 (7)	170
N1—H1B⋯O2ⁱⁱ	0.89	2.01	2.884 (6)	168
N1—H1A⋯Cl1ⁱⁱⁱ	0.89	2.49	3.322 (6)	156
N2—H2B⋯Cl2ⁱ	0.89	2.59	3.350 (6)	144
N2—H2C⋯Cl3^iv	0.89	2.69	3.321 (5)	129
N1—H1C⋯Cl5^v	0.89	2.55	3.367 (5)	153
N2—H2C⋯Cl6^iv	0.89	2.64	3.442 (5)	151

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

Acknowledgments

The authors acknowledge the National Science Foundation of China for financial support of this project (grant Nos. 51072188 and 50702053).

supplementary crystallographic information

Comment

Inorganic-organic hybrid materials have received much attention due to their potential applications in many areas such as gas storage, separation, catalysis, magnetism, optics as well as in electrical conductivity (Descazo et al., 2006; Li et al., 2007; Sanchez et al., 2005). Recently, we have prepared the title compound and here its crystal structure is reported.

This title compound contains SnC1₆ inorganic anions and organic cations. The SnCl₆ inorganic anion adopts a regular octahedral geometry, with average Sn—Cl distance of 2.4102 Å. In the organic cations, the diangle between the methyl ketone and the phenyl ring is 14.9 (3)° or 3.1 (2)°.

In the crystal structure, intermolecular N—H···O and N—H···Cl hydrogen bonds link cations and anions into a three-dimensioal framework.

Experimental

p-Aminoacetophenone (10 mmol) was dissolved in methanol (10 ml). Ten minutes later, a methanol solution (10 ml) of tin tetrachloride (5 mmol) was added with stirring. The reaction mixture was stirred for 4 h. The solution was held at room temperature for about two weeks, whereupon yellow crystals suitable for X-ray diffraction analysis were obtained.