Bis[4-(dimethyl-amino)pyridinium] hexa-kis[bromido/chlorido(0.78/0.22)]stannate(IV).

The Sn atom in the title salt, (C(7)H(11)N(2))(2)[SnBr(4.67)Cl(1.33)], lies on a center of symmetry within an octa-hedron of disordered halogen atoms. The three independent halogen atoms are each a mixture of bromine and chlorine atoms [with site occupancies for bromine of 0.614 (1), 0.831 (1) and 0.888 (1)]. An N-H⋯ hydrogen bond is present.

Related literature

For the isostructural tribromidotrichloridostannate, see: Lo & Ng (2008 ▶); for the isostructural penta­bromido­chlorido­stannate, see: Jang et al. (2009 ▶).

Experimental

Crystal data

(C7H11N2)2[SnBr4.67Cl1.33]

M = 785.15

Monoclinic,

a = 8.4530 (2) Å

b = 11.9036 (2) Å

c = 11.9093 (2) Å

β = 107.109 (1)°

V = 1145.30 (4) Å3

Z = 2

Mo Kα radiation

μ = 9.42 mm−1

T = 100 K

0.30 × 0.25 × 0.20 mm

Data collection

Bruker SMART APEX diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.504, T max = 0.746 (expected range = 0.103–0.152)

10319 measured reflections

2622 independent reflections

2240 reflections with I > 2σ(I)

R int = 0.033

Refinement

R[F 2 > 2σ(F 2)] = 0.023

wR(F 2) = 0.060

S = 0.99

2622 reflections

127 parameters

6 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.80 e Å−3

Δρmin = −0.87 e Å−3

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2009 ▶).

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809019734/tk2458sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809019734/tk2458Isup2.hkl

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

(C7H11N2)2[SnBr4.67Cl1.33]	F(000) = 740
Mr = 785.15	Dx = 2.277 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 4263 reflections
a = 8.4530 (2) Å	θ = 2.5–28.3°
b = 11.9036 (2) Å	µ = 9.42 mm−1
c = 11.9093 (2) Å	T = 100 K
β = 107.109 (1)°	Irregular block, colorless
V = 1145.30 (4) Å3	0.30 × 0.25 × 0.20 mm
Z = 2

Bruker SMART APEX diffractometer	2622 independent reflections
Radiation source: fine-focus sealed tube	2240 reflections with I > 2σ(I)
graphite	Rint = 0.033
ω scans	θmax = 27.5°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→10
Tmin = 0.504, Tmax = 0.746	k = −15→15
10319 measured reflections	l = −14→15

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.060	H atoms treated by a mixture of independent and constrained refinement
S = 0.99	w = 1/[σ2(Fo2) + (0.0343P)2 + 0.6005P] where P = (Fo2 + 2Fc2)/3
2622 reflections	(Δ/σ)max = 0.001
127 parameters	Δρmax = 0.80 e Å−3
6 restraints	Δρmin = −0.87 e Å−3

	x	y	z	Uiso*/Ueq	Occ. (<1)
Sn1	0.5000	0.5000	0.5000	0.01384 (8)
Br1	0.50914 (5)	0.63592 (3)	0.66901 (3)	0.02247 (12)	0.6143 (14)
Br2	0.58481 (5)	0.33875 (3)	0.64866 (3)	0.02405 (12)	0.8309 (9)
Br3	0.80683 (4)	0.53911 (3)	0.52227 (3)	0.02760 (12)	0.8878 (10)
Cl1	0.50914 (5)	0.63592 (3)	0.66901 (3)	0.02247 (12)	0.3858 (14)
Cl2	0.58481 (5)	0.33875 (3)	0.64866 (3)	0.02405 (12)	0.1122 (10)
Cl3	0.80683 (4)	0.53911 (3)	0.52227 (3)	0.02760 (12)	0.1691 (9)
N1	0.6521 (4)	0.8743 (2)	0.5886 (3)	0.0309 (7)
H1	0.598 (5)	0.812 (2)	0.593 (4)	0.061 (14)*
N2	0.9135 (3)	1.1561 (2)	0.5550 (2)	0.0231 (6)
C1	0.7281 (4)	0.9350 (3)	0.6844 (3)	0.0304 (8)
H1A	0.7212	0.9116	0.7590	0.036*
C2	0.8143 (4)	1.0288 (3)	0.6765 (3)	0.0259 (7)
H2	0.8683	1.0696	0.7457	0.031*
C3	0.8251 (4)	1.0670 (3)	0.5661 (3)	0.0190 (6)
C4	0.7363 (4)	1.0019 (3)	0.4663 (3)	0.0228 (7)
H4	0.7345	1.0249	0.3896	0.027*
C5	0.6553 (4)	0.9080 (3)	0.4810 (3)	0.0297 (8)
H5	0.5994	0.8645	0.4142	0.036*
C6	1.0103 (4)	1.2201 (3)	0.6573 (3)	0.0349 (8)
H6A	0.9356	1.2652	0.6883	0.052*
H6B	1.0876	1.2697	0.6340	0.052*
H6C	1.0725	1.1680	0.7182	0.052*
C7	0.9124 (4)	1.1989 (3)	0.4397 (3)	0.0293 (7)
H7A	0.9577	1.1418	0.3985	0.044*
H7B	0.9802	1.2670	0.4496	0.044*
H7C	0.7985	1.2166	0.3937	0.044*

	U11	U22	U33	U12	U13	U23
Sn1	0.01350 (14)	0.01560 (14)	0.01208 (14)	−0.00189 (10)	0.00326 (11)	−0.00020 (11)
Br1	0.0329 (2)	0.0187 (2)	0.0178 (2)	−0.00322 (16)	0.01055 (17)	−0.00423 (15)
Br2	0.0329 (2)	0.01902 (19)	0.01671 (19)	−0.00065 (14)	0.00180 (15)	0.00479 (13)
Br3	0.01394 (18)	0.0409 (2)	0.0279 (2)	−0.00705 (13)	0.00609 (14)	−0.00114 (15)
Cl1	0.0329 (2)	0.0187 (2)	0.0178 (2)	−0.00322 (16)	0.01055 (17)	−0.00423 (15)
Cl2	0.0329 (2)	0.01902 (19)	0.01671 (19)	−0.00065 (14)	0.00180 (15)	0.00479 (13)
Cl3	0.01394 (18)	0.0409 (2)	0.0279 (2)	−0.00705 (13)	0.00609 (14)	−0.00114 (15)
N1	0.0277 (16)	0.0246 (15)	0.0427 (19)	0.0002 (12)	0.0141 (14)	0.0088 (14)
N2	0.0235 (14)	0.0244 (14)	0.0195 (14)	−0.0029 (11)	0.0032 (11)	−0.0017 (11)
C1	0.0298 (19)	0.037 (2)	0.0273 (18)	0.0121 (15)	0.0138 (15)	0.0114 (16)
C2	0.0256 (17)	0.0335 (18)	0.0190 (17)	0.0045 (14)	0.0071 (14)	0.0010 (13)
C3	0.0157 (14)	0.0217 (15)	0.0185 (15)	0.0046 (11)	0.0036 (12)	0.0009 (12)
C4	0.0214 (15)	0.0252 (16)	0.0198 (16)	−0.0003 (13)	0.0030 (13)	−0.0026 (13)
C5	0.0238 (17)	0.0282 (18)	0.033 (2)	−0.0001 (13)	0.0021 (15)	−0.0037 (15)
C6	0.033 (2)	0.035 (2)	0.033 (2)	−0.0101 (15)	0.0035 (16)	−0.0085 (16)
C7	0.0300 (18)	0.0285 (18)	0.0270 (18)	−0.0048 (14)	0.0045 (14)	0.0082 (14)

Sn1—Br1	2.5658 (4)	C1—C2	1.351 (5)
Sn1—Cl1i	2.5658 (4)	C1—H1A	0.9500
Sn1—Br1i	2.5658 (4)	C2—C3	1.419 (4)
Sn1—Br2	2.5663 (3)	C2—H2	0.9500
Sn1—Cl2i	2.5663 (3)	C3—C4	1.433 (4)
Sn1—Br2i	2.5663 (3)	C4—C5	1.349 (5)
Sn1—Cl3i	2.5709 (3)	C4—H4	0.9500
Sn1—Br3i	2.5709 (3)	C5—H5	0.9500
Sn1—Br3	2.5709 (3)	C6—H6A	0.9800
N1—C1	1.343 (5)	C6—H6B	0.9800
N1—C5	1.351 (5)	C6—H6C	0.9800
N1—H1	0.882 (10)	C7—H7A	0.9800
N2—C3	1.327 (4)	C7—H7B	0.9800
N2—C6	1.466 (4)	C7—H7C	0.9800
N2—C7	1.462 (4)
Br1—Sn1—Cl1i	180.0	Br3i—Sn1—Br3	180.000 (17)
Br1—Sn1—Br1i	180.0	C1—N1—C5	120.5 (3)
Cl1i—Sn1—Br1i	0.000 (14)	C1—N1—H1	122 (3)
Br1—Sn1—Br2	89.576 (13)	C5—N1—H1	118 (3)
Cl1i—Sn1—Br2	90.424 (13)	C3—N2—C6	121.7 (3)
Br1i—Sn1—Br2	90.424 (13)	C3—N2—C7	121.6 (3)
Br1—Sn1—Cl2i	90.424 (13)	C6—N2—C7	116.6 (3)
Cl1i—Sn1—Cl2i	89.576 (12)	N1—C1—C2	121.2 (3)
Br1i—Sn1—Cl2i	89.576 (12)	N1—C1—H1A	119.4
Br2—Sn1—Cl2i	180.0	C2—C1—H1A	119.4
Br1—Sn1—Br2i	90.424 (13)	C1—C2—C3	120.8 (3)
Cl1i—Sn1—Br2i	89.576 (12)	C1—C2—H2	119.6
Br1i—Sn1—Br2i	89.576 (12)	C3—C2—H2	119.6
Br2—Sn1—Br2i	180.0	N2—C3—C2	122.7 (3)
Cl2i—Sn1—Br2i	0.00 (2)	N2—C3—C4	121.5 (3)
Br1—Sn1—Cl3i	89.529 (12)	C2—C3—C4	115.7 (3)
Cl1i—Sn1—Cl3i	90.471 (12)	C5—C4—C3	120.2 (3)
Br1i—Sn1—Cl3i	90.471 (12)	C5—C4—H4	119.9
Br2—Sn1—Cl3i	90.248 (12)	C3—C4—H4	119.9
Cl2i—Sn1—Cl3i	89.752 (12)	C4—C5—N1	121.4 (3)
Br2i—Sn1—Cl3i	89.752 (12)	C4—C5—H5	119.3
Br1—Sn1—Br3i	89.529 (12)	N1—C5—H5	119.3
Cl1i—Sn1—Br3i	90.471 (12)	N2—C6—H6A	109.5
Br1i—Sn1—Br3i	90.471 (12)	N2—C6—H6B	109.5
Br2—Sn1—Br3i	90.248 (12)	H6A—C6—H6B	109.5
Cl2i—Sn1—Br3i	89.752 (12)	N2—C6—H6C	109.5
Br2i—Sn1—Br3i	89.752 (12)	H6A—C6—H6C	109.5
Cl3i—Sn1—Br3i	0.00 (2)	H6B—C6—H6C	109.5
Br1—Sn1—Br3	90.471 (12)	N2—C7—H7A	109.5
Cl1i—Sn1—Br3	89.529 (12)	N2—C7—H7B	109.5
Br1i—Sn1—Br3	89.529 (12)	H7A—C7—H7B	109.5
Br2—Sn1—Br3	89.752 (12)	N2—C7—H7C	109.5
Cl2i—Sn1—Br3	90.248 (12)	H7A—C7—H7C	109.5
Br2i—Sn1—Br3	90.248 (12)	H7B—C7—H7C	109.5
Cl3i—Sn1—Br3	180.000 (17)
C5—N1—C1—C2	−2.3 (5)	C1—C2—C3—N2	−177.4 (3)
N1—C1—C2—C3	0.9 (5)	C1—C2—C3—C4	1.5 (5)
C6—N2—C3—C2	1.6 (5)	N2—C3—C4—C5	176.1 (3)
C7—N2—C3—C2	−175.2 (3)	C2—C3—C4—C5	−2.8 (5)
C6—N2—C3—C4	−177.3 (3)	C3—C4—C5—N1	1.6 (5)
C7—N2—C3—C4	5.9 (5)	C1—N1—C5—C4	1.0 (5)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···Br1	0.88 (1)	2.48 (2)	3.334 (3)	162 (4)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1⋯Br1	0.88 (1)	2.484 (18)	3.334 (3)	162 (4)