1-Amino-pyridinium triiodidoplumbate(II).

The title complex, (C(5)H(7)N(2))[PbI(3)], consists of a 1-amino-pyridinium cation, disordered about a mirror plane, and a [PbI(3)](-) anion. The Pb(2+) ion (site symmetry ) is surrounded by six I atoms in a slightly distorted octa-hedral coordination. The PbI(6) octa-hedra share faces, building up (∞) (1)[PbI(6/2)] chains running along [010]. The cations are situated between the chains. Coulombic attractions and van der Waals inter-actions between the inorganic and organic components are mainly responsible for the cohesion of the structure.

Related literature

For background to hybrid materials, see: Rogow et al. (2010 ▶); Thirumurugan & Rao (2008 ▶). For structures with lead halide building blocks, see: Li et al. (2008 ▶); Zhang et al. (2008 ▶).

Experimental

Crystal data

(C5H7N2)[PbI3]

M = 683.03

Orthorhombic,

a = 15.0417 (19) Å

b = 8.1316 (10) Å

c = 10.5625 (14) Å

V = 1291.9 (3) Å3

Z = 4

Mo Kα radiation

μ = 20.18 mm−1

T = 296 K

0.6 × 0.2 × 0.1 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.011, T max = 0.133

10792 measured reflections

1607 independent reflections

1263 reflections with I > 2σ(I)

R int = 0.036

Refinement

R[F 2 > 2σ(F 2)] = 0.025

wR(F 2) = 0.056

S = 1.11

1607 reflections

61 parameters

1 restraint

H-atom parameters constrained

Δρmax = 0.86 e Å−3

Δρmin = −1.05 e Å−3

Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810036263/wm2395sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810036263/wm2395Isup2.hkl

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

(C5H7N2)[PbI3]	Z = 4
Mr = 683.03	F(000) = 1168
Orthorhombic, Pnma	Dx = 3.512 Mg m−3
Hall symbol: -P 2ac 2n	Mo Kα radiation, λ = 0.71073 Å
a = 15.0417 (19) Å	µ = 20.18 mm−1
b = 8.1316 (10) Å	T = 296 K
c = 10.5625 (14) Å	Needle, orange
V = 1291.9 (3) Å3	0.6 × 0.2 × 0.1 mm

Bruker SMART CCD area-detector diffractometer	1607 independent reflections
Radiation source: fine-focus sealed tube	1263 reflections with I > 2σ(I)
graphite	Rint = 0.036
phi and ω scans	θmax = 27.6°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −19→19
Tmin = 0.011, Tmax = 0.133	k = −10→10
10792 measured reflections	l = −13→13

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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.056	H-atom parameters constrained
S = 1.11	w = 1/[σ2(Fo2) + (0.016P)2 + 2.8133P] where P = (Fo2 + 2Fc2)/3
1607 reflections	(Δ/σ)max = 0.001
61 parameters	Δρmax = 0.86 e Å−3
1 restraint	Δρmin = −1.05 e Å−3

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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	Occ. (<1)
Pb1	0.5000	0.5000	0.5000	0.05028 (11)
I1	0.66188 (4)	0.2500	0.44218 (7)	0.06995 (19)
I2	0.45861 (4)	0.2500	0.73162 (5)	0.05961 (16)
I3	0.38187 (5)	0.2500	0.33215 (6)	0.06837 (19)
C1	0.0996 (6)	0.1682 (10)	0.4247 (8)	0.100 (3)
H1	0.0708	0.1100	0.3609	0.120*
C2	0.1419 (7)	0.0883 (12)	0.5186 (9)	0.103 (3)
H2	0.1424	−0.0261	0.5197	0.123*
C3	0.1824 (5)	0.1708 (11)	0.6087 (7)	0.100 (3)	0.50
H3	0.2114	0.1142	0.6731	0.120*	0.50
N1	0.1824 (5)	0.1708 (11)	0.6087 (7)	0.100 (3)	0.50
N2	0.2230 (10)	0.132 (2)	0.7177 (16)	0.121 (5)	0.50
H2A	0.2415	0.2091	0.7672	0.146*	0.50
H2B	0.2307	0.0310	0.7382	0.146*	0.50

	U11	U22	U33	U12	U13	U23
Pb1	0.0585 (2)	0.03787 (16)	0.05448 (19)	0.00017 (13)	0.00130 (15)	−0.00097 (14)
I1	0.0549 (3)	0.0611 (4)	0.0938 (5)	0.000	0.0189 (3)	0.000
I2	0.0727 (4)	0.0575 (3)	0.0486 (3)	0.000	0.0023 (3)	0.000
I3	0.0753 (4)	0.0603 (4)	0.0696 (4)	0.000	−0.0268 (3)	0.000
C1	0.120 (7)	0.100 (6)	0.081 (5)	−0.001 (5)	−0.015 (5)	−0.010 (5)
C2	0.104 (7)	0.089 (6)	0.114 (8)	−0.005 (5)	0.008 (6)	0.004 (6)
C3	0.064 (4)	0.162 (9)	0.074 (5)	0.010 (4)	0.010 (3)	0.026 (5)
N1	0.064 (4)	0.162 (9)	0.074 (5)	0.010 (4)	0.010 (3)	0.026 (5)
N2	0.111 (11)	0.121 (12)	0.133 (13)	0.004 (10)	−0.004 (11)	0.029 (11)

Pb1—I3i	3.2301 (5)	C1—C1iii	1.331 (16)
Pb1—I3	3.2301 (5)	C1—C2	1.345 (12)
Pb1—I1	3.2303 (5)	C1—H1	0.9300
Pb1—I1i	3.2303 (5)	C2—C3	1.315 (11)
Pb1—I2	3.2412 (5)	C2—H2	0.9300
Pb1—I2i	3.2412 (5)	C3—C3iii	1.288 (18)
I1—Pb1ii	3.2303 (5)	C3—H3	0.9300
I2—Pb1ii	3.2412 (5)	N2—H2A	0.8600
I3—Pb1ii	3.2301 (5)	N2—H2B	0.8600
I3i—Pb1—I3	180.0	I2—Pb1—I2i	180.0
I3i—Pb1—I1	94.886 (17)	Pb1ii—I1—Pb1	78.000 (17)
I3—Pb1—I1	85.114 (17)	Pb1ii—I2—Pb1	77.688 (16)
I3i—Pb1—I1i	85.114 (17)	Pb1—I3—Pb1ii	78.007 (16)
I3—Pb1—I1i	94.886 (17)	C1iii—C1—C2	118.9 (6)
I1—Pb1—I1i	180.0	C1iii—C1—H1	120.6
I3i—Pb1—I2	94.940 (16)	C2—C1—H1	120.6
I3—Pb1—I2	85.060 (16)	C3—C2—C1	120.4 (9)
I1—Pb1—I2	83.844 (15)	C3—C2—H2	119.8
I1i—Pb1—I2	96.156 (15)	C1—C2—H2	119.8
I3i—Pb1—I2i	85.060 (16)	C3iii—C3—C2	120.7 (6)
I3—Pb1—I2i	94.940 (16)	C3iii—C3—H3	119.7
I1—Pb1—I2i	96.156 (15)	C2—C3—H3	119.7
I1i—Pb1—I2i	83.844 (15)	H2A—N2—H2B	120.0

Table 1

Selected bond lengths (Å)

Pb1—I3	3.2301 (5)
Pb1—I1	3.2303 (5)
Pb1—I2	3.2412 (5)