Bis[4-(dimethyl-amino)pyridinium] tetra-bromidodiphenyl-plumbate(IV).

The Pb(IV) atom of the anion of the title salt, (C(7)H(11)N(2))(2)[PbBr(4)(C(6)H(5))(2)], is situated on a crystallographic center of inversion and exhibits a tetra-gonally compressed octa-hedral coordination. One of the two independent Br atoms acts as a hydrogen-bond acceptor towards the NH group of the cation.

Related literature

For the structure of isostructural bis­(4-dimethyl­amino­pyridinium) tetra­bromidodiphenyl­stannate, see: Yap et al. (2008 ▶).

Experimental

Crystal data

(C7H11N2)2[PbBr4(C6H5)2]

M = 927.39

Monoclinic,

a = 9.4994 (8) Å

b = 13.882 (1) Å

c = 10.991 (1) Å

β = 92.998 (1)°

V = 1447.3 (2) Å3

Z = 2

Mo Kα radiation

μ = 11.37 mm−1

T = 100 (2) K

0.22 × 0.08 × 0.06 mm

Data collection

Bruker SMART APEX diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.246, T max = 0.549 (expected range = 0.226–0.505)

8227 measured reflections

3309 independent reflections

2879 reflections with I > 2σ(I)

R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.029

wR(F 2) = 0.074

S = 1.03

3309 reflections

162 parameters

H-atom parameters constrained

Δρmax = 1.21 e Å−3

Δρmin = −1.70 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, 2008 ▶).

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808027530/im2080sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808027530/im2080Isup2.hkl

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

(C7H11N2)2[PbBr4(C6H5)2]	F(000) = 876
Mr = 927.39	Dx = 2.128 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3449 reflections
a = 9.4994 (8) Å	θ = 2.3–28.3°
b = 13.882 (1) Å	µ = 11.37 mm−1
c = 10.991 (1) Å	T = 100 K
β = 92.998 (1)°	Prism, colorless
V = 1447.3 (2) Å3	0.22 × 0.08 × 0.06 mm
Z = 2

Bruker SMART APEX diffractometer	3309 independent reflections
Radiation source: fine-focus sealed tube	2879 reflections with I > 2σ(I)
graphite	Rint = 0.029
ω scans	θmax = 27.5°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→12
Tmin = 0.246, Tmax = 0.549	k = −17→18
8227 measured reflections	l = −14→14

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)] = 0.029	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.074	H-atom parameters constrained
S = 1.03	w = 1/[σ2(Fo2) + (0.0374P)2 + 3.9748P] where P = (Fo2 + 2Fc2)/3
3309 reflections	(Δ/σ)max = 0.001
162 parameters	Δρmax = 1.21 e Å−3
0 restraints	Δρmin = −1.70 e Å−3

	x	y	z	Uiso*/Ueq
Pb1	0.5000	0.5000	0.5000	0.00948 (8)
Br1	0.55832 (5)	0.61261 (3)	0.29156 (5)	0.01773 (12)
Br2	0.76243 (5)	0.40245 (3)	0.46044 (4)	0.01405 (11)
N1	1.1998 (4)	0.5912 (3)	−0.0112 (4)	0.0149 (8)
N2	0.8888 (4)	0.5868 (3)	0.2341 (4)	0.0195 (9)
H2n	0.8188	0.5819	0.2831	0.023*
C1	0.6145 (5)	0.6028 (3)	0.6196 (4)	0.0122 (9)
C2	0.5516 (5)	0.6319 (3)	0.7245 (4)	0.0138 (9)
H2	0.4624	0.6071	0.7443	0.017*
C3	0.6230 (5)	0.6988 (3)	0.8006 (4)	0.0171 (10)
H3	0.5821	0.7202	0.8728	0.021*
C4	0.7539 (5)	0.7339 (3)	0.7703 (4)	0.0163 (10)
H4	0.8019	0.7795	0.8219	0.020*
C5	0.8145 (5)	0.7028 (3)	0.6654 (4)	0.0161 (10)
H5	0.9041	0.7269	0.6455	0.019*
C6	0.7450 (5)	0.6367 (3)	0.5894 (4)	0.0136 (9)
H6	0.7864	0.6150	0.5175	0.016*
C7	0.8774 (5)	0.6473 (4)	0.1383 (5)	0.0209 (11)
H7	0.7961	0.6869	0.1276	0.025*
C8	0.9792 (5)	0.6529 (3)	0.0567 (5)	0.0162 (10)
H8	0.9691	0.6961	−0.0102	0.019*
C9	1.1018 (5)	0.5936 (3)	0.0715 (4)	0.0115 (9)
C10	1.1123 (5)	0.5358 (4)	0.1782 (4)	0.0164 (10)
H10	1.1945	0.4981	0.1952	0.020*
C11	1.0064 (5)	0.5337 (4)	0.2559 (5)	0.0189 (10)
H11	1.0150	0.4944	0.3266	0.023*
C12	1.1934 (6)	0.6536 (4)	−0.1184 (5)	0.0235 (12)
H12A	1.0949	0.6696	−0.1405	0.035*
H12B	1.2346	0.6201	−0.1865	0.035*
H12C	1.2463	0.7129	−0.1001	0.035*
C13	1.3293 (5)	0.5345 (4)	0.0087 (5)	0.0195 (10)
H13A	1.3939	0.5682	0.0667	0.029*
H13B	1.3744	0.5264	−0.0688	0.029*
H13C	1.3061	0.4712	0.0416	0.029*

	U11	U22	U33	U12	U13	U23
Pb1	0.01089 (12)	0.01025 (12)	0.00716 (12)	−0.00156 (9)	−0.00091 (8)	−0.00108 (9)
Br1	0.0182 (2)	0.0185 (2)	0.0164 (2)	0.00011 (18)	0.00039 (19)	0.00211 (19)
Br2	0.0142 (2)	0.0158 (2)	0.0120 (2)	0.00186 (17)	−0.00032 (18)	−0.00038 (17)
N1	0.018 (2)	0.0146 (19)	0.012 (2)	0.0033 (16)	0.0018 (17)	0.0019 (16)
N2	0.018 (2)	0.025 (2)	0.016 (2)	−0.0001 (18)	0.0063 (18)	−0.0024 (18)
C1	0.014 (2)	0.011 (2)	0.011 (2)	−0.0021 (17)	−0.0035 (18)	0.0002 (17)
C2	0.015 (2)	0.013 (2)	0.014 (2)	0.0022 (18)	0.0000 (19)	0.0002 (18)
C3	0.022 (2)	0.018 (2)	0.011 (2)	0.003 (2)	−0.003 (2)	−0.0025 (19)
C4	0.023 (3)	0.009 (2)	0.016 (3)	−0.0022 (19)	−0.008 (2)	−0.0004 (18)
C5	0.016 (2)	0.016 (2)	0.016 (2)	−0.0037 (19)	−0.004 (2)	0.0035 (19)
C6	0.020 (2)	0.015 (2)	0.005 (2)	−0.0030 (19)	−0.0028 (18)	0.0005 (18)
C7	0.016 (2)	0.021 (3)	0.025 (3)	0.006 (2)	−0.005 (2)	−0.005 (2)
C8	0.019 (2)	0.016 (2)	0.013 (2)	0.0049 (19)	−0.002 (2)	0.0004 (19)
C9	0.013 (2)	0.011 (2)	0.011 (2)	−0.0004 (17)	−0.0021 (18)	−0.0026 (17)
C10	0.018 (2)	0.019 (2)	0.012 (2)	−0.001 (2)	−0.003 (2)	0.000 (2)
C11	0.019 (2)	0.023 (2)	0.015 (3)	−0.001 (2)	−0.001 (2)	−0.001 (2)
C12	0.030 (3)	0.023 (3)	0.018 (3)	0.004 (2)	0.003 (2)	0.008 (2)
C13	0.013 (2)	0.027 (3)	0.018 (3)	0.005 (2)	0.000 (2)	−0.003 (2)

Pb1—C1	2.190 (5)	C4—H4	0.9500
Pb1—C1i	2.190 (5)	C5—C6	1.385 (6)
Pb1—Br1	2.8516 (5)	C5—H5	0.9500
Pb1—Br1i	2.8516 (5)	C6—H6	0.9500
Pb1—Br2i	2.8897 (5)	C7—C8	1.356 (7)
Pb1—Br2	2.8897 (5)	C7—H7	0.9500
N1—C9	1.335 (6)	C8—C9	1.428 (6)
N1—C13	1.467 (6)	C8—H8	0.9500
N1—C12	1.461 (6)	C9—C10	1.420 (7)
N2—C7	1.347 (7)	C10—C11	1.353 (7)
N2—C11	1.349 (7)	C10—H10	0.9500
N2—H2n	0.8800	C11—H11	0.9500
C1—C6	1.383 (6)	C12—H12A	0.9800
C1—C2	1.386 (6)	C12—H12B	0.9800
C2—C3	1.401 (7)	C12—H12C	0.9800
C2—H2	0.9500	C13—H13A	0.9800
C3—C4	1.392 (7)	C13—H13B	0.9800
C3—H3	0.9500	C13—H13C	0.9800
C4—C5	1.384 (7)
C1—Pb1—C1i	180.00 (17)	C6—C5—C4	120.2 (4)
C1—Pb1—Br1	90.79 (12)	C6—C5—H5	119.9
C1i—Pb1—Br1	89.21 (12)	C4—C5—H5	119.9
C1—Pb1—Br1i	89.21 (12)	C1—C6—C5	119.1 (4)
C1i—Pb1—Br1i	90.79 (12)	C1—C6—H6	120.4
Br1—Pb1—Br1i	180.000 (16)	C5—C6—H6	120.4
C1—Pb1—Br2i	90.55 (12)	C8—C7—N2	121.5 (5)
C1i—Pb1—Br2i	89.45 (12)	C8—C7—H7	119.3
Br1—Pb1—Br2i	93.978 (14)	N2—C7—H7	119.3
Br1i—Pb1—Br2i	86.022 (14)	C7—C8—C9	119.8 (5)
C1—Pb1—Br2	89.45 (12)	C7—C8—H8	120.1
C1i—Pb1—Br2	90.55 (12)	C9—C8—H8	120.1
Br1—Pb1—Br2	86.022 (14)	N1—C9—C10	121.8 (4)
Br1i—Pb1—Br2	93.978 (14)	N1—C9—C8	122.0 (4)
Br2i—Pb1—Br2	180.0	C10—C9—C8	116.2 (4)
C9—N1—C13	121.4 (4)	C11—C10—C9	120.7 (5)
C9—N1—C12	122.2 (4)	C11—C10—H10	119.7
C13—N1—C12	115.9 (4)	C9—C10—H10	119.7
C7—N2—C11	120.7 (4)	C10—C11—N2	120.8 (5)
C7—N2—H2n	119.6	C10—C11—H11	119.6
C11—N2—H2n	119.6	N2—C11—H11	119.6
C6—C1—C2	122.1 (4)	N1—C12—H12A	109.5
C6—C1—Pb1	120.1 (3)	N1—C12—H12B	109.5
C2—C1—Pb1	117.8 (3)	H12A—C12—H12B	109.5
C1—C2—C3	118.2 (4)	N1—C12—H12C	109.5
C1—C2—H2	120.9	H12A—C12—H12C	109.5
C3—C2—H2	120.9	H12B—C12—H12C	109.5
C4—C3—C2	120.0 (4)	N1—C13—H13A	109.5
C4—C3—H3	120.0	N1—C13—H13B	109.5
C2—C3—H3	120.0	H13A—C13—H13B	109.5
C5—C4—C3	120.4 (4)	N1—C13—H13C	109.5
C5—C4—H4	119.8	H13A—C13—H13C	109.5
C3—C4—H4	119.8	H13B—C13—H13C	109.5
Br1—Pb1—C1—C6	−46.0 (4)	Pb1—C1—C6—C5	179.0 (3)
Br1i—Pb1—C1—C6	134.0 (4)	C4—C5—C6—C1	0.2 (7)
Br2i—Pb1—C1—C6	−140.0 (4)	C11—N2—C7—C8	3.9 (8)
Br2—Pb1—C1—C6	40.0 (4)	N2—C7—C8—C9	0.1 (8)
Br1—Pb1—C1—C2	133.8 (3)	C13—N1—C9—C10	−5.1 (7)
Br1i—Pb1—C1—C2	−46.2 (3)	C12—N1—C9—C10	−177.1 (5)
Br2i—Pb1—C1—C2	39.9 (3)	C13—N1—C9—C8	176.2 (4)
Br2—Pb1—C1—C2	−140.1 (3)	C12—N1—C9—C8	4.2 (7)
C6—C1—C2—C3	0.9 (7)	C7—C8—C9—N1	174.8 (5)
Pb1—C1—C2—C3	−179.0 (3)	C7—C8—C9—C10	−3.9 (7)
C1—C2—C3—C4	−0.3 (7)	N1—C9—C10—C11	−174.7 (5)
C2—C3—C4—C5	−0.2 (7)	C8—C9—C10—C11	4.0 (7)
C3—C4—C5—C6	0.3 (7)	C9—C10—C11—N2	−0.3 (8)
C2—C1—C6—C5	−0.8 (7)	C7—N2—C11—C10	−3.8 (8)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2n···Br1	0.88	2.52	3.254 (4)	142

Table 1

Selected bond lengths (Å)

Pb1—C1	2.190 (5)
Pb1—Br1	2.8516 (5)
Pb1—Br2	2.8897 (5)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2n⋯Br1	0.88	2.52	3.254 (4)	142