Tris(3-methylanilinium) pentachloridoantimonate(III) chloride

In the title compound, (C7H10N)3[SbCl5]Cl, the SbIII cation is coordinated by five Cl− anions in a distorted square-pyramidal geometry, in which the longest Sb—Cl distance of 3.0319 (14) Å indicates a weak coordination bond. In the crystal, the 3-methylanilinium cations link with the complex antimonate anions and Cl− anions via N—H⋯Cl hydrogen bonds.

In the title compound, (C 7 H 10 N) 3 [SbCl 5 ]Cl, the Sb III cation is coordinated by five Cl À anions in a distorted square-pyramidal geometry, in which the longest Sb-Cl distance of 3.0319 (14) Å indicates a weak coordination bond. In the crystal, the 3-methylanilinium cations link with the complex antimonate anions and Cl À anions via N-HÁ Á ÁCl hydrogen bonds.
The author thanks an anonymous advisor from the Ordered Matter Science Research Centre, Southeast University, for great help with the revision of this paper.
The title compound, [(C 7 H 10 N) 3 SbCl 5 ] + .Cl -, has an asymmetric unit that consists of three C 7 H 10 N cations, one antimony(III) pentachloride anion and one chloride anion all in general positions (Fig 1). The non-hydrgen atoms of C 7 H 10 N cation are nearly coplanar, the antimony(III) atom is coordinated by five chlorine atoms, forming a distorted square-pyramid, the Sb-Cl bond distances range from 2.4043 (13) to 3.0319 (14) Å (  Chen et al., 2009b). The existence of N-H···Cl hydrogen-bonding interactions gives rise a three-dimensional structure (Fig. 2).
Experimental 3.21 g (0.03 mol) of 3-methylbenzenamine was firstly dissolved in 30 ml ethanol, to which 1.1 g (0.03 mol) of hydrochloric acid was then added to afford the solution, then the 2.28 g (0.01 mol) antimony chloride was dissolved in 20 ml ethanol which was added hydrochloric acid, at last, mixed the above solution without any precipitation under stirring at the ambient temperature. Single crystals suitable for X-ray structure analysis were obtained by the slow evaporation of the above solution after 4 days in air.
The dielectric constant of the compound as a function of temperature indicates that the permittivity is basically temperature-independent (ε = C/(T-T 0 )), suggesting that this compound is not ferroelectric or there may be no distinct phase transition occurring within the measured temperature within the measured temperature (below the melting point).

Special details
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.
Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > 2sigma(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.