Bis[4-(dimethyl-amino)pyridinium] penta-bromidochloridostannate(IV).

In the title compound, (C(7)H(11)N(2))(2)[SnBr(5)Cl], there is Br/Cl disorder in 0.6561 (12):0.3439 (12) and 0.8438 (12):0.1561 (12) ratios over two of three halide sites in the centrosymmetric anion, such that an overall formulation of [SnBr(5)Cl](2-) arises. In the crystal, associations of two cations and one anion linked by N-H⋯Br hydrogen bonds occur.

Related literature

For related 4-dimethyl­amino­pyridinium halogenoorgano­stannates, see: Lo & Ng (2008 ▶); Norhafiza et al. (2008 ▶); Yau et al. (2008 ▶).

Experimental

Crystal data

(C7H11N2)2[SnBr5Cl]

M = 800.05

Monoclinic,

a = 8.4424 (1) Å

b = 11.8821 (2) Å

c = 11.8868 (2) Å

β = 107.123 (1)°

V = 1139.55 (3) Å3

Z = 2

Mo Kα radiation

μ = 10.01 mm−1

T = 100 K

0.30 × 0.10 × 0.10 mm

Data collection

Bruker SMART APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.152, T max = 0.434 (expected range = 0.129–0.367)

9261 measured reflections

2613 independent reflections

2408 reflections with I > 2σ(I)

R int = 0.022

Refinement

R[F 2 > 2σ(F 2)] = 0.021

wR(F 2) = 0.053

S = 1.01

2613 reflections

121 parameters

4 restraints

H-atom parameters constrained

Δρmax = 0.91 e Å−3

Δρmin = −0.95 e Å−3

Data collection: APEX2 software (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/S160053680901705X/hb2965sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053680901705X/hb2965Isup2.hkl

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

(C7H11N2)2[SnBr5Cl]	F(000) = 752
Mr = 800.05	Dx = 2.332 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5777 reflections
a = 8.4424 (1) Å	θ = 2.5–28.3°
b = 11.8821 (2) Å	µ = 10.01 mm−1
c = 11.8868 (2) Å	T = 100 K
β = 107.123 (1)°	Block, colourless
V = 1139.55 (3) Å3	0.30 × 0.10 × 0.10 mm
Z = 2

Bruker SMART APEX CCD diffractometer	2613 independent reflections
Radiation source: fine-focus sealed tube	2408 reflections with I > 2σ(I)
graphite	Rint = 0.022
ω scans	θmax = 27.5°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→10
Tmin = 0.152, Tmax = 0.434	k = −15→15
9261 measured reflections	l = −15→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)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.053	H-atom parameters constrained
S = 1.01	w = 1/[σ2(Fo2) + (0.0276P)2 + 1.7721P] where P = (Fo2 + 2Fc2)/3
2613 reflections	(Δ/σ)max = 0.001
121 parameters	Δρmax = 0.91 e Å−3
4 restraints	Δρmin = −0.95 e Å−3

	x	y	z	Uiso*/Ueq	Occ. (<1)
Sn1	0.5000	0.5000	0.5000	0.01035 (7)
Br1	0.50979 (5)	0.63602 (3)	0.66902 (3)	0.02104 (10)	0.6561 (12)
Br2	0.58402 (4)	0.33881 (2)	0.64884 (3)	0.02209 (9)	0.8438 (12)
Br3	0.80725 (3)	0.53820 (3)	0.52248 (3)	0.02568 (8)
Cl1	0.50979 (5)	0.63602 (3)	0.66902 (3)	0.02104 (10)	0.3439 (12)
Cl2	0.58402 (4)	0.33881 (2)	0.64884 (3)	0.02209 (9)	0.1561 (12)
N1	0.6520 (3)	0.8746 (2)	0.5886 (3)	0.0271 (6)
H1	0.5999	0.8123	0.5962	0.032*
N2	0.9139 (3)	1.15682 (19)	0.5545 (2)	0.0186 (5)
C1	0.8253 (3)	1.0669 (2)	0.5659 (2)	0.0154 (5)
C2	0.7373 (4)	1.0025 (2)	0.4666 (3)	0.0194 (5)
H2	0.7358	1.0257	0.3898	0.023*
C3	0.6551 (4)	0.9077 (2)	0.4809 (3)	0.0245 (6)
H3	0.5991	0.8642	0.4139	0.029*
C4	0.7277 (4)	0.9358 (3)	0.6848 (3)	0.0251 (6)
H4	0.7203	0.9125	0.7595	0.030*
C5	0.8137 (4)	1.0296 (2)	0.6768 (3)	0.0211 (6)
H5	0.8670	1.0711	0.7459	0.025*
C6	0.9127 (4)	1.1990 (3)	0.4393 (3)	0.0249 (6)
H6A	0.9488	1.1393	0.3955	0.037*
H6B	0.9883	1.2633	0.4490	0.037*
H6C	0.8002	1.2229	0.3958	0.037*
C7	1.0105 (4)	1.2208 (3)	0.6571 (3)	0.0291 (7)
H7A	0.9353	1.2650	0.6887	0.044*
H7B	1.0866	1.2715	0.6336	0.044*
H7C	1.0740	1.1687	0.7175	0.044*

	U11	U22	U33	U12	U13	U23
Sn1	0.00978 (11)	0.01195 (11)	0.00936 (12)	−0.00163 (8)	0.00287 (9)	−0.00006 (8)
Br1	0.0306 (2)	0.01735 (16)	0.01761 (19)	−0.00301 (13)	0.01094 (15)	−0.00399 (12)
Br2	0.03025 (18)	0.01759 (15)	0.01582 (17)	−0.00058 (12)	0.00271 (13)	0.00430 (11)
Br3	0.01302 (14)	0.03789 (17)	0.02652 (17)	−0.00656 (11)	0.00643 (12)	−0.00107 (12)
Cl1	0.0306 (2)	0.01735 (16)	0.01761 (19)	−0.00301 (13)	0.01094 (15)	−0.00399 (12)
Cl2	0.03025 (18)	0.01759 (15)	0.01582 (17)	−0.00058 (12)	0.00271 (13)	0.00430 (11)
N1	0.0210 (12)	0.0210 (12)	0.0407 (17)	−0.0003 (10)	0.0115 (11)	0.0092 (11)
N2	0.0175 (11)	0.0195 (11)	0.0167 (12)	−0.0033 (9)	0.0019 (9)	−0.0018 (9)
C1	0.0123 (12)	0.0183 (12)	0.0145 (13)	0.0038 (9)	0.0025 (10)	0.0005 (10)
C2	0.0183 (13)	0.0212 (13)	0.0170 (14)	0.0007 (10)	0.0024 (11)	−0.0009 (11)
C3	0.0208 (14)	0.0230 (14)	0.0265 (16)	−0.0016 (11)	0.0019 (12)	−0.0023 (12)
C4	0.0214 (14)	0.0320 (15)	0.0256 (16)	0.0108 (12)	0.0130 (12)	0.0122 (13)
C5	0.0207 (14)	0.0283 (14)	0.0141 (14)	0.0061 (11)	0.0049 (11)	0.0018 (11)
C6	0.0240 (14)	0.0240 (14)	0.0251 (16)	−0.0053 (11)	0.0047 (12)	0.0069 (12)
C7	0.0290 (16)	0.0304 (16)	0.0233 (17)	−0.0097 (12)	0.0007 (13)	−0.0110 (13)

Sn1—Br1	2.5608 (3)	C1—C2	1.419 (4)
Sn1—Cl1i	2.5608 (3)	C1—C5	1.421 (4)
Sn1—Br1i	2.5608 (3)	C2—C3	1.360 (4)
Sn1—Br2	2.5618 (3)	C2—H2	0.9500
Sn1—Cl2i	2.5618 (3)	C3—H3	0.9500
Sn1—Br2i	2.5618 (3)	C4—C5	1.348 (4)
Sn1—Br3i	2.5687 (3)	C4—H4	0.9500
Sn1—Br3	2.5687 (3)	C5—H5	0.9500
N1—C4	1.347 (4)	C6—H6A	0.9800
N1—C3	1.347 (4)	C6—H6B	0.9800
N1—H1	0.8800	C6—H6C	0.9800
N2—C1	1.334 (3)	C7—H7A	0.9800
N2—C6	1.456 (4)	C7—H7B	0.9800
N2—C7	1.464 (4)	C7—H7C	0.9800
Br1—Sn1—Cl1i	180.0	C1—N2—C6	121.5 (2)
Br1—Sn1—Br1i	180.0	C1—N2—C7	121.6 (2)
Cl1i—Sn1—Br1i	0.000 (11)	C6—N2—C7	116.9 (2)
Br1—Sn1—Br2	89.520 (11)	N2—C1—C2	121.3 (3)
Cl1i—Sn1—Br2	90.480 (11)	N2—C1—C5	122.5 (3)
Br1i—Sn1—Br2	90.480 (11)	C2—C1—C5	116.2 (3)
Br1—Sn1—Cl2i	90.480 (11)	C3—C2—C1	120.3 (3)
Cl1i—Sn1—Cl2i	89.520 (11)	C3—C2—H2	119.8
Br1i—Sn1—Cl2i	89.520 (11)	C1—C2—H2	119.8
Br2—Sn1—Cl2i	180.000 (12)	N1—C3—C2	120.9 (3)
Br1—Sn1—Br2i	90.480 (11)	N1—C3—H3	119.6
Cl1i—Sn1—Br2i	89.520 (11)	C2—C3—H3	119.6
Br1i—Sn1—Br2i	89.520 (11)	N1—C4—C5	121.1 (3)
Br2—Sn1—Br2i	180.000 (12)	N1—C4—H4	119.4
Cl2i—Sn1—Br2i	0.00 (2)	C5—C4—H4	119.4
Br1—Sn1—Br3i	89.512 (11)	C4—C5—C1	120.6 (3)
Cl1i—Sn1—Br3i	90.488 (11)	C4—C5—H5	119.7
Br1i—Sn1—Br3i	90.488 (11)	C1—C5—H5	119.7
Br2—Sn1—Br3i	90.316 (10)	N2—C6—H6A	109.5
Cl2i—Sn1—Br3i	89.684 (10)	N2—C6—H6B	109.5
Br2i—Sn1—Br3i	89.684 (10)	H6A—C6—H6B	109.5
Br1—Sn1—Br3	90.488 (11)	N2—C6—H6C	109.5
Cl1i—Sn1—Br3	89.512 (11)	H6A—C6—H6C	109.5
Br1i—Sn1—Br3	89.512 (11)	H6B—C6—H6C	109.5
Br2—Sn1—Br3	89.684 (10)	N2—C7—H7A	109.5
Cl2i—Sn1—Br3	90.316 (10)	N2—C7—H7B	109.5
Br2i—Sn1—Br3	90.316 (10)	H7A—C7—H7B	109.5
Br3i—Sn1—Br3	180.0	N2—C7—H7C	109.5
C4—N1—C3	120.8 (3)	H7A—C7—H7C	109.5
C4—N1—H1	119.6	H7B—C7—H7C	109.5
C3—N1—H1	119.6
C6—N2—C1—C2	5.6 (4)	C4—N1—C3—C2	1.3 (4)
C7—N2—C1—C2	−177.4 (3)	C1—C2—C3—N1	1.7 (4)
C6—N2—C1—C5	−174.8 (3)	C3—N1—C4—C5	−2.4 (4)
C7—N2—C1—C5	2.2 (4)	N1—C4—C5—C1	0.6 (4)
N2—C1—C2—C3	176.4 (3)	N2—C1—C5—C4	−177.5 (3)
C5—C1—C2—C3	−3.3 (4)	C2—C1—C5—C4	2.2 (4)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···Br1	0.88	2.47	3.327 (2)	165

Table 1

Selected bond lengths (Å). X = (Br, Cl)

Sn1—X1	2.5608 (3)
Sn1—X2	2.5618 (3)
Sn1—X3	2.5687 (3)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1⋯Br1	0.88	2.47	3.327 (2)	165