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

Trigui, A.; Boughzala, H.; Driss, A.; Abid, Y.

doi:10.1107/S160053681100941X

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 67| Part 4| April 2011| Pages m458-m459

doi:10.1107/S160053681100941X

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

A. Trigui,^a H. Boughzala,^b ^* A. Driss ^b and Y. Abid ^a

^aLaboratoire de Physique Appliquée (LPA), Faculté des Sciences de Sfax, 3018, BP 802, Tunisia, and ^bLaboratoire de Cristallochimie et des Matériaux, Faculté des Sciences de Tunis, Tunisia
^*Correspondence e-mail: habib.boughzala@ipein.rnu.tn

(Received 19 February 2011; accepted 11 March 2011; online 15 March 2011)

The organic–inorganic hybrid, {(C₆H₁₃N₃)₂[Pb₃I₁₀]}_n, was obtained by the reaction of 1-(3-ammoniopropyl)imidazolium triiodide and PbI₂ at room temperature. The structure contains one-dimensional {[Pb₃I₁₀]⁴⁻}_n polymeric anions spreading parallel to [001], resulting from face–face–edge association of PbI₆ distorted octahedra. 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_r = 2144.99
Triclinic, $[P \overline 1]$
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[F² > 2σ(F²)] = 0.036
wR(F²) = 0.110
S = 1.02
3796 reflections
143 parameters
H-atom parameters constrained
Δρ_max = 2.17 e Å⁻³
Δρ_min = −2.09 e Å⁻³

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) -x+1, -y+2, -z+1.

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⋯I5^iv	0.89	2.89	3.64 (2)	143
Symmetry codes: (iii) -x, -y+1, -z+1; (iv) -x+1, -y+1, -z+1.

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 ).

Supporting information

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

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

checkCIF report

Comment top

Recently, self-assembling organic–inorganic hybrid compounds have been the focus of a great number of investigations owing to their unique structural, magnetic, optical nonlinear and optoelectronic functionality (Papavassiliou et al., 1999; Ishihara et al., 1990; Mitzi et al., 2001). In particular, the lead iodide-based hybrid materials have been extensively studied (Gebauer & Schmid, 1999; Dammak et al., 2009; Elleuch et al., 2010) since they show strong room temperature excitonic optical features with large exciton binding energy and oscillator strengths. These low dimensional complexes include zero dimensional (0D), one dimensional (1D), and two dimensional (2D) lead iodide networks with organic groups as spacers. Among them, 1D-hybrids are more attractive in nanoscaled applications since they form a variety of crystalline structures, which differ in the inorganic chain where the [PbI₆] octahedra can be connected in different ways: face sharing (Elleuch et al., 2007), edge sharing (Samet Kallel et al., 2008), corner sharing (Mousdis et al., 1998) or through several combinations of these various types of sharing (Maxcy et al., 2003; Billing & Lemmerer, 2004; Krautscheid et al., 2001), as in the case of our compound. We present here the structure of the organic–inorganic one dimensional hybrid compound (C₆H₁₃N₃)₂Pb₃I₁₀.

The crystal structure of the title compound consists of (Pb₃I₁₀)_n^4n- chains extending along [001] with the 1-(3-ammoniopropyl)-imidazolium cations as counter-ions (Fig. 1). The inorganic anion, shown in Fig. 1, can be considered as a set of mixed face-shared/edge-shared octahedra. In fact, the unit cell contains three octahedra with two crystallographically independent Pb atoms: Pb1 and Pb2. The central Pb2 octahedron is connected to the Pb1 octahedra by shared faces, while the Pb1 octahedra are linked via edge-sharing at both ends of Pb₃I₁₀^4- to adjacent units.

The coordination octahedron of the central lead ion Pb2 is only slightly distorted since it is located on an inversion centre and is bound to three unique I atoms: I2, I3 and I4, which participate in the face-sharing between the Pb2 and Pb1 octahedra. The bond lengths around Pb2 are very similar (3.2105 (15), 3.2388 (14), 3.263 (2) Å), the bond angles I—Pb2—I deviate slightly from ideal octahedral values, ranging from 83° to 94°. In contrast, Pb1 has a more distorted environement with Pb—I distances ranging from 3.155 (2) to 3.309 (2) Å and with all cis and trans angles different (see Table 1). This Pb atom is bonded to five unique I atoms, where two I1 atoms are responsible for the edge sharing between the neighbouring units to form one-dimensional infinite chains. Atom I5 is the only halide not involved in any bonding with adjacent octahedra and has the shortest Pb—I distance [3.155 (2) Å].

Cations fill channels between the anionic chains (Fig.2). Each terminal ammonium group forms three N—H···I hydrogen bonds to I atoms of three different chains (see Table 2).

Related literature top

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 top

Single crystals of (C₆H₁₃N₃)₂Pb₃I₁₀ were grown by the slow evaporation at room temperature of a solution containing PbI₂ and C₆H₁₃N₃I₃ salts. An aqueous solution of HI was added to the aminopropylimidazole to synthesize C₆H₁₃N₃I₃ precursor. Under ambient conditions, stoechiometric amounts of C₆H₁₃N₃I₃ and PbI₂ with excess HI were sailed in DMF. This mixture was stirred and remained clear without any precipitate. Pale-yellow flatted crystals were obtained few weeks later. Supplementary data for this paper are available from the IUCr electronic archives (Reference: CCDC 782074).

Computing details top

Data collection: CAD-4 EXPRESS (Duisenberg, 1992); cell refinement: CAD-4 EXPRESS (Duisenberg, 1992); 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).

Figures top

	Fig. 1. View of the asymmetric unit of (C₆H₁₃N₃)₂Pb₃I₁₀ with some adjacent atoms showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) 1 - x, 2 - y, 1 - z, (ii) 1 - x, 2 - y, 2 - z]
	Fig. 2. The crystal packing of (C₆H₁₃N₃)₂Pb₃I₁₀ viewed along [001] direction and showing the N—H···I hydrogen bonding (dashed lines).

catena-poly[bis[1-(3-ammoniopropyl)-1H-imidazolium] [[iodidoplumbate(II)]-tri-µ-iodido-plumbate(II)-tri-µ-iodido- [iodidoplumbate(II)]-di-µ-iodido]] top

Crystal data top

(C₆H₁₃N₃)₂[Pb₃I₁₀]	Z = 1
M_r = 2144.99	F(000) = 916
Triclinic, P1	D_x = 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

Data collection top

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

Refinement top

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(F_o²) + (0.063P)²] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.001
3796 reflections	Δρ_max = 2.17 e Å⁻³
143 parameters	Δρ_min = −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)

Crystal data top

(C₆H₁₃N₃)₂[Pb₃I₁₀]	γ = 107.17 (3)°
M_r = 2144.99	V = 976.7 (9) Å³
Triclinic, P1	Z = 1
a = 8.652 (3) Å	Mo Kα radiation
b = 11.728 (5) Å	µ = 20.81 mm⁻¹
c = 11.972 (6) Å	T = 293 K
α = 117.21 (3)°	0.4 × 0.2 × 0.02 mm
β = 98.05 (2)°

Data collection top

Enraf–Nonius CAD-4 diffractometer	2749 reflections with I > 2σ(I)
Absorption correction: ψ scan (North et al., 1968)	R_int = 0.024
T_min = 0.139, T_max = 0.624	2 standard reflections every 120 min
4950 measured reflections	intensity decay: 6%
3796 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	0 restraints
wR(F²) = 0.110	H-atom parameters constrained
S = 1.02	Δρ_max = 2.17 e Å⁻³
3796 reflections	Δρ_min = −2.09 e Å⁻³
143 parameters

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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

Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+1, −y+2, −z+2.

Hydrogen-bond geometry (Å, º) top

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···I5^iv	0.89	2.89	3.64 (2)	143

Symmetry codes: (iii) −x, −y+1, −z+1; (iv) −x+1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	(C₆H₁₃N₃)₂[Pb₃I₁₀]
M_r	2144.99
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	8.652 (3), 11.728 (5), 11.972 (6)
α, β, γ (°)	117.21 (3), 98.05 (2), 107.17 (3)
V (Å³)	976.7 (9)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	20.81
Crystal size (mm)	0.4 × 0.2 × 0.02

Data collection
Diffractometer	Enraf–Nonius CAD-4 diffractometer
Absorption correction	ψ scan (North et al., 1968)
T_min, T_max	0.139, 0.624
No. of measured, independent and observed [I > 2σ(I)] reflections	4950, 3796, 2749
R_int	0.024
(sin θ/λ)_max (Å⁻¹)	0.616

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.110, 1.02
No. of reflections	3796
No. of parameters	143
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	2.17, −2.09

Computer programs: CAD-4 EXPRESS (Duisenberg, 1992), XCAD4 (Harms & Wocadlo, 1995), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2006), publCIF (Westrip, 2010).

Selected geometric parameters (Å, º) top

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

I5—Pb1—I1	90.09 (5)	I1—Pb1—I4	94.09 (5)
I5—Pb1—I3	89.89 (5)	I3—Pb1—I4	84.36 (5)
I1—Pb1—I3	88.94 (4)	I1ⁱ—Pb1—I4	89.73 (5)
I5—Pb1—I1ⁱ	95.96 (5)	I2—Pb1—I4	83.75 (5)
I1—Pb1—I1ⁱ	92.18 (4)	I4ⁱⁱ—Pb2—I3	94.24 (4)
I3—Pb1—I1ⁱ	174.05 (2)	I4—Pb2—I2	85.98 (5)
I5—Pb1—I2	91.62 (5)	I3—Pb2—I2	86.90 (5)
I1—Pb1—I2	175.04 (2)	Pb1—I1—Pb1ⁱ	87.82 (4)
I3—Pb1—I2	86.41 (4)	Pb2—I2—Pb1	76.05 (4)
I1ⁱ—Pb1—I2	92.27 (4)	Pb1—I3—Pb2	77.46 (4)
I5—Pb1—I4	172.82 (3)	Pb2—I4—Pb1	76.68 (5)

Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+1, −y+2, −z+2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N9—H9A···I5	0.89	2.84	3.67 (2)	155.8
N9—H9B···I2ⁱⁱⁱ	0.89	2.90	3.68 (2)	146.5
N9—H9C···I5^iv	0.89	2.89	3.64 (2)	143.2

Symmetry codes: (iii) −x, −y+1, −z+1; (iv) −x+1, −y+1, −z+1.

References

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Volume 67| Part 4| April 2011| Pages m458-m459

doi:10.1107/S160053681100941X

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

References

metal-organic compounds

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