Bis(diisopropyl-ammonium) hexa-chlorido-stannate(IV).

The title compound, (C(6)H(16)N)(2)[SnCl(6)], crystallizes with one diisopropyl-ammonium cation lying on a general position and the hexa-chloridostannate(IV) anion about a centre of inversion. The [SnCl(6)](2-) anion undergoes a slight distortion from octa-hedral symmetry as the result of the formation of four unforked charge-supported N-H⋯Cl hydrogen bonds. The hydrogen bonds between the cations and anions form layers perpendicular to [101]. These layers are built by 24-membered rings which can be classified with an R(8) (8)(24) graph-set descriptor. According to this hydrogen-bonding motif, the title compound is isostructural with (C(6)H(16)N)(2)[IrCl(6)].

Related literature

For related diisopropyl­ammonium salts, see: Fu et al. (2011 ▶); Reiss (1998 ▶, 2002 ▶, 2012 ▶); Reiss & Helmbrecht (2012 ▶); Reiss & Meyer (2011 ▶). For layered structures, see: Cameron et al. (1983 ▶); Holl & Thewalt (1986 ▶); Rademeyer et al. (2007 ▶). For potassium hexa­halogenidometalates, see: Abrahams et al. (1989 ▶); Amilius et al. (1969 ▶); Boysen & Hewat (1978 ▶); Coll et al. (1987 ▶); Hinz et al. (2000 ▶). For spectroscopy of hexa­chloridostannate(IV) salts, see: Brown et al. (1970 ▶); Ouasri et al. (2001 ▶). For graph-set theory and its applications, see: Etter et al. (1990 ▶); Grell et al. (2002 ▶).

Experimental

Crystal data

(C6H16N)2[SnCl6]

M = 535.81

Monoclinic,

a = 9.54362 (13) Å

b = 11.98179 (19) Å

c = 9.90669 (14) Å

β = 92.9406 (14)°

V = 1131.33 (3) Å3

Z = 2

Mo Kα radiation

μ = 1.83 mm−1

T = 100 K

0.33 × 0.27 × 0.08 mm

Data collection

Oxford Diffraction Xcalibur Eos diffractometer

Absorption correction: numerical (CrysAlis PRO; Oxford Diffraction, 2009 ▶) T min = 0.634, T max = 0.922

11414 measured reflections

4972 independent reflections

4468 reflections with I > 2σ(I)

R int = 0.024

Refinement

R[F 2 > 2σ(F 2)] = 0.021

wR(F 2) = 0.048

S = 1.02

4972 reflections

120 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.53 e Å−3

Δρmin = −0.57 e Å−3

Data collection: CrysAlis PRO (Oxford Diffraction, 2009 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2012 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812043371/mw2089sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812043371/mw2089Isup2.hkl

Click here for additional data file.

Supplementary material file. DOI: 10.1107/S1600536812043371/mw2089Isup3.mol

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

(C6H16N)2[SnCl6]	F(000) = 540
Mr = 535.81	Dx = 1.573 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 8237 reflections
a = 9.54362 (13) Å	θ = 2.9–36.3°
b = 11.98179 (19) Å	µ = 1.83 mm−1
c = 9.90669 (14) Å	T = 100 K
β = 92.9406 (14)°	Plate, colourless
V = 1131.33 (3) Å3	0.33 × 0.27 × 0.08 mm
Z = 2

Oxford Diffraction Xcalibur Eos diffractometer	4972 independent reflections
Radiation source: fine-focus sealed tube	4468 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.024
Detector resolution: 16.2711 pixels mm-1	θmax = 35.0°, θmin = 2.9°
ω scans	h = −15→15
Absorption correction: numerical (CrysAlis PRO; Oxford Diffraction, 2009)	k = −19→19
Tmin = 0.634, Tmax = 0.922	l = −12→15
11414 measured reflections

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.021	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.048	w = 1/[σ2(Fo2) + (0.0186P)2] where P = (Fo2 + 2Fc2)/3
S = 1.02	(Δ/σ)max = 0.001
4972 reflections	Δρmax = 0.53 e Å−3
120 parameters	Δρmin = −0.57 e Å−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0041 (4)

Experimental. Absorption correction: CrysAlisPro (Oxford Diffraction, 2009). Numerical absorption correction based on gaussian integration over a multifaceted crystal model.

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 F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

	x	y	z	Uiso*/Ueq
Sn1	1.0000	0.0000	0.0000	0.01123 (3)
Cl1	0.92766 (3)	0.08742 (2)	0.20722 (2)	0.01631 (6)
Cl2	1.11712 (3)	0.17373 (2)	−0.06094 (3)	0.01646 (6)
Cl3	0.78698 (3)	0.06606 (2)	−0.11335 (3)	0.01563 (5)
N1	0.68736 (10)	0.27997 (8)	0.11589 (10)	0.01418 (17)
H11	0.7445 (17)	0.2227 (14)	0.1090 (15)	0.025 (4)*
H12	0.6727 (16)	0.2895 (13)	0.2005 (15)	0.025 (4)*
C1	0.54865 (11)	0.24787 (9)	0.04603 (11)	0.01420 (19)
H1	0.5701 (16)	0.2361 (12)	−0.0494 (14)	0.017*
C2	0.44162 (12)	0.33988 (10)	0.06181 (12)	0.0186 (2)
H2A	0.4352	0.3571	0.1559	0.025 (2)*
H2B	0.3517	0.3155	0.0251	0.025 (2)*
H2C	0.4702	0.4053	0.0144	0.025 (2)*
C3	0.50358 (13)	0.13875 (10)	0.10779 (13)	0.0213 (2)
H3A	0.5742	0.0831	0.0957	0.025 (2)*
H3B	0.4166	0.1148	0.0642	0.025 (2)*
H3C	0.4914	0.1492	0.2025	0.025 (2)*
C4	0.75609 (12)	0.38701 (10)	0.07441 (12)	0.0171 (2)
H4	0.6925 (16)	0.4433 (13)	0.0962 (14)	0.020*
C5	0.89127 (14)	0.40009 (12)	0.16051 (14)	0.0272 (3)
H5A	0.8715	0.3948	0.2543	0.036 (3)*
H5B	0.9321	0.4716	0.1432	0.036 (3)*
H5C	0.9557	0.3422	0.1384	0.036 (3)*
C6	0.78081 (14)	0.38572 (12)	−0.07562 (12)	0.0238 (2)
H6A	0.8376	0.3224	−0.0961	0.035 (3)*
H6B	0.8281	0.4530	−0.0997	0.035 (3)*
H6C	0.6924	0.3809	−0.1260	0.035 (3)*

	U11	U22	U33	U12	U13	U23
Sn1	0.01016 (5)	0.01241 (5)	0.01133 (5)	0.00038 (3)	0.00261 (3)	0.00032 (3)
Cl1	0.01780 (12)	0.01875 (12)	0.01260 (10)	0.00316 (9)	0.00306 (9)	−0.00157 (9)
Cl2	0.01694 (12)	0.01595 (12)	0.01663 (11)	−0.00356 (9)	0.00218 (9)	0.00126 (9)
Cl3	0.01222 (10)	0.01879 (12)	0.01588 (11)	0.00180 (9)	0.00070 (9)	0.00081 (10)
N1	0.0125 (4)	0.0154 (4)	0.0148 (4)	0.0002 (3)	0.0028 (3)	0.0007 (4)
C1	0.0133 (4)	0.0151 (5)	0.0143 (4)	−0.0012 (4)	0.0026 (4)	−0.0016 (4)
C2	0.0156 (5)	0.0187 (5)	0.0215 (5)	0.0019 (4)	0.0005 (4)	−0.0009 (4)
C3	0.0207 (5)	0.0159 (5)	0.0280 (6)	−0.0038 (4)	0.0079 (5)	0.0012 (5)
C4	0.0151 (5)	0.0135 (5)	0.0231 (5)	−0.0024 (4)	0.0048 (4)	−0.0016 (4)
C5	0.0198 (6)	0.0310 (7)	0.0307 (6)	−0.0091 (5)	0.0012 (5)	−0.0068 (6)
C6	0.0235 (6)	0.0242 (6)	0.0243 (6)	−0.0051 (5)	0.0073 (5)	0.0059 (5)

Sn1—Cl3i	2.4055 (3)	C2—H2B	0.9600
Sn1—Cl3	2.4055 (3)	C2—H2C	0.9600
Sn1—Cl1	2.4359 (3)	C3—H3A	0.9600
Sn1—Cl1i	2.4359 (3)	C3—H3B	0.9600
Sn1—Cl2	2.4527 (3)	C3—H3C	0.9600
Sn1—Cl2i	2.4527 (3)	C4—C6	1.5168 (16)
N1—C4	1.5073 (15)	C4—C5	1.5178 (17)
N1—C1	1.5117 (14)	C4—H4	0.940 (16)
N1—H11	0.881 (16)	C5—H5A	0.9600
N1—H12	0.864 (15)	C5—H5B	0.9600
C1—C3	1.5153 (16)	C5—H5C	0.9600
C1—C2	1.5164 (16)	C6—H6A	0.9600
C1—H1	0.988 (14)	C6—H6B	0.9600
C2—H2A	0.9600	C6—H6C	0.9600
Cl3i—Sn1—Cl3	180.000 (18)	H2A—C2—H2B	109.5
Cl3i—Sn1—Cl1	90.994 (9)	C1—C2—H2C	109.5
Cl3—Sn1—Cl1	89.006 (9)	H2A—C2—H2C	109.5
Cl3i—Sn1—Cl1i	89.006 (9)	H2B—C2—H2C	109.5
Cl3—Sn1—Cl1i	90.994 (9)	C1—C3—H3A	109.5
Cl1—Sn1—Cl1i	180.000 (13)	C1—C3—H3B	109.5
Cl3i—Sn1—Cl2	90.528 (9)	H3A—C3—H3B	109.5
Cl3—Sn1—Cl2	89.472 (9)	C1—C3—H3C	109.5
Cl1—Sn1—Cl2	89.711 (9)	H3A—C3—H3C	109.5
Cl1i—Sn1—Cl2	90.289 (9)	H3B—C3—H3C	109.5
Cl3i—Sn1—Cl2i	89.472 (9)	N1—C4—C6	110.50 (9)
Cl3—Sn1—Cl2i	90.528 (9)	N1—C4—C5	107.69 (10)
Cl1—Sn1—Cl2i	90.289 (9)	C6—C4—C5	112.41 (10)
Cl1i—Sn1—Cl2i	89.711 (9)	N1—C4—H4	104.7 (9)
Cl2—Sn1—Cl2i	180.000 (13)	C6—C4—H4	111.5 (9)
C4—N1—C1	118.34 (9)	C5—C4—H4	109.7 (9)
C4—N1—H11	111.2 (10)	C4—C5—H5A	109.5
C1—N1—H11	107.3 (10)	C4—C5—H5B	109.5
C4—N1—H12	104.2 (11)	H5A—C5—H5B	109.5
C1—N1—H12	107.3 (10)	C4—C5—H5C	109.5
H11—N1—H12	108.0 (14)	H5A—C5—H5C	109.5
N1—C1—C3	107.14 (9)	H5B—C5—H5C	109.5
N1—C1—C2	110.28 (9)	C4—C6—H6A	109.5
C3—C1—C2	112.27 (10)	C4—C6—H6B	109.5
N1—C1—H1	104.8 (9)	H6A—C6—H6B	109.5
C3—C1—H1	109.9 (9)	C4—C6—H6C	109.5
C2—C1—H1	112.1 (9)	H6A—C6—H6C	109.5
C1—C2—H2A	109.5	H6B—C6—H6C	109.5
C1—C2—H2B	109.5
C4—N1—C1—C3	−179.42 (9)	C1—N1—C4—C6	−57.67 (13)
C4—N1—C1—C2	−56.96 (12)	C1—N1—C4—C5	179.20 (10)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H11···Cl1	0.881 (16)	2.541 (16)	3.3449 (10)	152.1 (13)
N1—H12···Cl2ii	0.864 (15)	2.488 (15)	3.3507 (10)	176.0 (14)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H11⋯Cl1	0.881 (16)	2.541 (16)	3.3449 (10)	152.1 (13)
N1—H12⋯Cl2i	0.864 (15)	2.488 (15)	3.3507 (10)	176.0 (14)

Symmetry code: (i) .