The one-dimensional organic-inorganic hybrid: catena-poly[bis-[1-(3-ammonio-prop-yl)-1H-imidazolium] [[iodidoplumbate(II)]-tri-μ-iodido-plumbate(II)-tri-μ-iodido-[iodidoplumbate(II)]-di-μ-iodido]].

The organic-inorganic hybrid, {(C(6)H(13)N(3))(2)[Pb(3)I(10)]}(n), was obtained by the reaction of 1-(3-ammonio-prop-yl)imidazolium triiodide and PbI(2) at room temperature. The structure contains one-dimensional {[Pb(3)I(10)](4-)}(n) polymeric anions spreading parallel to [001], resulting from face-face-edge association of PbI(6) distorted octa-hedra. One of the Pb(II) cations is imposed at an inversion centre, whereas the second occupies a general position. N-H⋯I hydrogen bonds connect the organic cations and inorganic anions.

Related literature

For organic–inorganic hybrid materials, see: Billing & Lemmerer (2004 ▶); Dammak et al. (2009 ▶); Elleuch et al. (2007 ▶, 2010 ▶); Gebauer & Schmid (1999 ▶); Ishihara et al. (1990 ▶); Krautscheid et al. (2001 ▶). For the structures of lead iodide-based complexes, see: Maxcy et al. (2003 ▶); Mitzi et al. (2001 ▶); Mousdis et al. (1998 ▶); Papavassiliou et al. (1999 ▶); Samet Kallel et al. (2008 ▶).

Experimental

Crystal data

(C6H13N3)2[Pb3I10]

M = 2144.99

Triclinic,

a = 8.652 (3) Å

b = 11.728 (5) Å

c = 11.972 (6) Å

α = 117.21 (3)°

β = 98.05 (2)°

γ = 107.17 (3)°

V = 976.7 (9) Å3

Z = 1

Mo Kα radiation

μ = 20.81 mm−1

T = 293 K

0.40 × 0.20 × 0.02 mm

Data collection

Enraf–Nonius CAD-4 diffractometer

Absorption correction: ψ scan (North et al., 1968 ▶) T min = 0.139, T max = 0.624

4950 measured reflections

3796 independent reflections

2749 reflections with I > 2σ(I)

R int = 0.024

2 standard reflections every 120 min intensity decay: 6%

Refinement

R[F 2 > 2σ(F 2)] = 0.036

wR(F 2) = 0.110

S = 1.02

3796 reflections

143 parameters

H-atom parameters constrained

Δρmax = 2.17 e Å−3

Δρmin = −2.09 e Å−3

Data collection: CAD-4 EXPRESS (Duisenberg, 1992 ▶); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681100941X/yk2002sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053681100941X/yk2002Isup2.hkl

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

(C6H13N3)2[Pb3I10]	Z = 1
Mr = 2144.99	F(000) = 916
Triclinic, P1	Dx = 3.647 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.652 (3) Å	Cell parameters from 25 reflections
b = 11.728 (5) Å	θ = 9–15°
c = 11.972 (6) Å	µ = 20.81 mm−1
α = 117.21 (3)°	T = 293 K
β = 98.05 (2)°	Flat, yellow
γ = 107.17 (3)°	0.4 × 0.2 × 0.02 mm
V = 976.7 (9) Å3

Enraf–Nonius CAD-4 diffractometer	2749 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.024
graphite	θmax = 26.0°, θmin = 2.0°
non–profiled ω/2θ scans	h = −10→2
Absorption correction: ψ scan (North et al., 1968)	k = −14→14
Tmin = 0.139, Tmax = 0.624	l = −14→14
4950 measured reflections	2 standard reflections every 120 min
3796 independent reflections	intensity decay: 6%

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)] = 0.036	H-atom parameters constrained
wR(F2) = 0.110	w = 1/[σ2(Fo2) + (0.063P)2] where P = (Fo2 + 2Fc2)/3
S = 1.01	(Δ/σ)max = 0.001
3796 reflections	Δρmax = 2.17 e Å−3
143 parameters	Δρmin = −2.09 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: 0.00169 (17)

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
Pb1	0.45091 (5)	0.90517 (4)	0.62320 (4)	0.03669 (15)
Pb2	0.5000	1.0000	1.0000	0.03708 (18)
I1	0.76440 (9)	0.98779 (8)	0.52450 (7)	0.0436 (2)
I2	0.14853 (9)	0.82298 (7)	0.74775 (7)	0.0436 (2)
I3	0.67368 (10)	0.82982 (8)	0.79737 (7)	0.0432 (2)
I4	0.59957 (11)	1.21598 (7)	0.90100 (8)	0.0505 (2)
I5	0.30697 (11)	0.59287 (8)	0.38118 (8)	0.0501 (2)
N9	0.2562 (18)	0.3757 (14)	0.5290 (12)	0.073 (4)
H9A	0.2959	0.4198	0.4885	0.109*
H9B	0.1595	0.3006	0.4732	0.109*
H9C	0.3332	0.3487	0.5545	0.109*
C8	0.223 (2)	0.4705 (14)	0.6451 (14)	0.060 (4)
H8A	0.1398	0.5000	0.6172	0.073*
H8B	0.3281	0.5534	0.7047	0.073*
C7	0.1565 (18)	0.3985 (15)	0.7187 (14)	0.057 (3)
H7A	0.1032	0.4516	0.7762	0.069*
H7B	0.0682	0.3058	0.6536	0.069*
C6	0.2864 (16)	0.3825 (13)	0.8013 (12)	0.050 (3)
H6A	0.3363	0.3245	0.7449	0.060*
H6B	0.3773	0.4739	0.8663	0.060*
N1	0.2042 (13)	0.3173 (9)	0.8694 (9)	0.045 (2)
C2	0.1429 (17)	0.1818 (12)	0.8230 (12)	0.050 (3)
H2	0.1488	0.1127	0.7458	0.060*
N3	0.0710 (14)	0.1625 (10)	0.9077 (11)	0.054 (3)
H3	0.0212	0.0825	0.8993	0.065*
C4	0.0878 (19)	0.2879 (14)	1.0096 (14)	0.058 (3)
H4	0.0471	0.3025	1.0808	0.069*
C5	0.1731 (18)	0.3842 (14)	0.9870 (13)	0.057 (3)
H5	0.2065	0.4805	1.0411	0.069*

	U11	U22	U33	U12	U13	U23
Pb1	0.0386 (3)	0.0395 (2)	0.0362 (2)	0.01781 (19)	0.01491 (18)	0.02124 (19)
Pb2	0.0412 (3)	0.0372 (3)	0.0332 (3)	0.0167 (3)	0.0139 (2)	0.0179 (2)
I1	0.0373 (4)	0.0564 (4)	0.0468 (4)	0.0216 (4)	0.0182 (3)	0.0318 (4)
I2	0.0343 (4)	0.0428 (4)	0.0479 (4)	0.0126 (3)	0.0151 (3)	0.0210 (3)
I3	0.0473 (4)	0.0506 (4)	0.0447 (4)	0.0300 (4)	0.0203 (3)	0.0272 (3)
I4	0.0590 (5)	0.0321 (4)	0.0514 (4)	0.0121 (4)	0.0103 (4)	0.0213 (3)
I5	0.0543 (5)	0.0409 (4)	0.0411 (4)	0.0177 (4)	0.0087 (4)	0.0140 (3)
N9	0.090 (10)	0.089 (9)	0.074 (8)	0.051 (8)	0.035 (7)	0.057 (7)
C8	0.085 (11)	0.058 (8)	0.062 (8)	0.034 (8)	0.029 (7)	0.045 (7)
C7	0.063 (9)	0.065 (8)	0.062 (8)	0.030 (7)	0.026 (7)	0.042 (7)
C6	0.045 (7)	0.053 (7)	0.055 (7)	0.021 (6)	0.019 (6)	0.030 (6)
N1	0.044 (6)	0.038 (5)	0.042 (5)	0.015 (4)	0.006 (4)	0.017 (4)
C2	0.055 (8)	0.038 (6)	0.041 (6)	0.021 (6)	0.005 (6)	0.012 (5)
N3	0.056 (7)	0.041 (5)	0.058 (6)	0.007 (5)	0.009 (5)	0.030 (5)
C4	0.068 (9)	0.061 (8)	0.058 (8)	0.026 (7)	0.038 (7)	0.037 (7)
C5	0.064 (9)	0.045 (7)	0.051 (7)	0.020 (7)	0.018 (7)	0.018 (6)

Pb1—I5	3.155 (2)	C8—H8A	0.9700
Pb1—I1	3.1757 (13)	C8—H8B	0.9700
Pb1—I3	3.2264 (14)	C7—C6	1.502 (18)
Pb1—I1i	3.2652 (13)	C7—H7A	0.9700
Pb1—I2	3.3039 (14)	C7—H7B	0.9700
Pb1—I4	3.309 (2)	C6—N1	1.473 (16)
Pb2—I4	3.2105 (15)	C6—H6A	0.9700
Pb2—I4ii	3.2105 (14)	C6—H6B	0.9700
Pb2—I3	3.2388 (14)	N1—C2	1.315 (15)
Pb2—I3ii	3.2388 (14)	N1—C5	1.375 (16)
Pb2—I2ii	3.263 (2)	C2—N3	1.331 (17)
Pb2—I2	3.263 (2)	C2—H2	0.9300
I1—Pb1i	3.2653 (13)	N3—C4	1.362 (16)
N9—C8	1.460 (17)	N3—H3	0.8600
N9—H9A	0.8900	C4—C5	1.318 (19)
N9—H9B	0.8900	C4—H4	0.9300
N9—H9C	0.8900	C5—H5	0.9300
C8—C7	1.536 (19)
I5—Pb1—I1	90.09 (5)	C8—N9—H9C	109.5
I5—Pb1—I3	89.89 (5)	H9A—N9—H9C	109.5
I1—Pb1—I3	88.94 (4)	H9B—N9—H9C	109.5
I5—Pb1—I1i	95.96 (5)	N9—C8—C7	111.1 (11)
I1—Pb1—I1i	92.18 (4)	N9—C8—H8A	109.4
I3—Pb1—I1i	174.05 (2)	C7—C8—H8A	109.4
I5—Pb1—I2	91.62 (5)	N9—C8—H8B	109.4
I1—Pb1—I2	175.04 (2)	C7—C8—H8B	109.4
I3—Pb1—I2	86.41 (4)	H8A—C8—H8B	108.0
I1i—Pb1—I2	92.27 (4)	C6—C7—C8	116.4 (12)
I5—Pb1—I4	172.82 (3)	C6—C7—H7A	108.2
I1—Pb1—I4	94.09 (5)	C8—C7—H7A	108.2
I3—Pb1—I4	84.36 (5)	C6—C7—H7B	108.2
I1i—Pb1—I4	89.73 (5)	C8—C7—H7B	108.2
I2—Pb1—I4	83.75 (5)	H7A—C7—H7B	107.3
I4—Pb2—I4ii	180.0	N1—C6—C7	109.8 (10)
I4—Pb2—I3	85.76 (4)	N1—C6—H6A	109.7
I4ii—Pb2—I3	94.24 (4)	C7—C6—H6A	109.7
I3—Pb2—I3ii	180.0	N1—C6—H6B	109.7
I4ii—Pb2—I2	94.02 (5)	C7—C6—H6B	109.7
I4—Pb2—I2	85.98 (5)	H6A—C6—H6B	108.2
I3ii—Pb2—I2	93.10 (5)	C2—N1—C5	108.9 (12)
I3—Pb2—I2	86.90 (5)	C2—N1—C6	124.3 (10)
I2ii—Pb2—I2	180.0	C5—N1—C6	126.8 (10)
I3ii—Pb2—I2ii	86.90 (5)	N1—C2—N3	106.8 (10)
I3—Pb2—I2ii	93.10 (5)	N1—C2—H2	126.6
I4ii—Pb2—I2ii	85.98 (5)	N3—C2—H2	126.6
I4—Pb2—I2ii	94.02 (5)	C2—N3—C4	110.1 (10)
I4—Pb2—I3ii	94.24 (4)	C2—N3—H3	124.9
I4ii—Pb2—I3ii	85.76 (4)	C4—N3—H3	124.9
Pb1—I1—Pb1i	87.82 (4)	C5—C4—N3	106.2 (11)
Pb2—I2—Pb1	76.05 (4)	C5—C4—H4	126.9
Pb1—I3—Pb2	77.46 (4)	N3—C4—H4	126.9
Pb2—I4—Pb1	76.68 (5)	C4—C5—N1	108.0 (12)
C8—N9—H9A	109.5	C4—C5—H5	126.0
C8—N9—H9B	109.5	N1—C5—H5	126.0
H9A—N9—H9B	109.5

D—H···A	D—H	H···A	D···A	D—H···A
N9—H9A···I5	0.89	2.84	3.67 (2)	156
N9—H9B···I2iii	0.89	2.90	3.68 (2)	147
N9—H9C···I5iv	0.89	2.89	3.64 (2)	143

Table 1

Selected geometric parameters (Å, °)

Pb1—I5	3.155 (2)
Pb1—I1	3.1757 (13)
Pb1—I3	3.2264 (14)
Pb1—I1i	3.2652 (13)
Pb1—I2	3.3039 (14)
Pb1—I4	3.309 (2)
Pb2—I4	3.2105 (15)
Pb2—I3	3.2388 (14)
Pb2—I2	3.263 (2)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N9—H9A⋯I5	0.89	2.84	3.67 (2)	156
N9—H9B⋯I2iii	0.89	2.90	3.68 (2)	147
N9—H9C⋯I5iv	0.89	2.89	3.64 (2)	143

Symmetry codes: (iii) ; (iv) .