The one-dimensional organic inorganic hybrid compound poly[(diethyl-ene-triamine)tetra-μ-iodido-dilead(II)].

A new organic-inorganic hybrid, [Pb(2)I(4)(C(4)H(13)N(3))](n), was obtained by the reaction of C(4)N(3)H(10) and PbI(2) at room temperature. The structure is a three-dimensional polymer resulting from the association of PbI(6) octa-hedra and a mixed lead organic-inorganic PbI(4)(C(4)N(3)H(13)) coordination polyhedron. Both Pb atoms, two I atoms and one N atom lie on a mirror plane. N-H⋯I hydrogen bonds further connect the organic unit and some I atoms.

Related literature

For related literature, see: Lode & Krautscheild (2001 ▶); Krautscheild et al. (2001 ▶); Papavassiliou et al. (1999 ▶); Wang et al. (1995 ▶); Zhu et al. (2004 ▶).

Experimental

Crystal data

[Pb2I4(C4H13N3)]

M = 1025.15

Orthorhombic,

a = 17.034 (6) Å

b = 9.218 (3) Å

c = 11.092 (4) Å

V = 1741.6 (10) Å3

Z = 4

Mo Kα radiation

μ = 26.38 mm−1

T = 293 (2) K

0.2 × 0.05 × 0.05 mm

Data collection

Enraf–Nonius CAD-4 diffractometer

Absorption correction: ψ scan (North et al., 1968 ▶) T min = 0.095, T max = 0.268

2906 measured reflections

1998 independent reflections

1202 reflections with I > 2σ(I)

R int = 0.045

2 standard reflections frequency: 120 min intensity decay: 5%

Refinement

R[F 2 > 2σ(F 2)] = 0.040

wR(F 2) = 0.099

S = 1.00

1998 reflections

67 parameters

H-atom parameters constrained

Δρmax = 1.57 e Å−3

Δρmin = −1.58 e Å−3

Data collection: CAD-4 EXPRESS (Duisenberg, 1992 ▶; Macíček & Yordanov, 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: PLATOn class="Chemical">N (Spek, 2003 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808013913/dn2346sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808013913/dn2346Isup2.hkl

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

[Pb2I4(C4H13N3)]	F000 = 1736
Mr = 1025.15	Dx = 3.910 Mg m−3
Orthorhombic, Pnma	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 25 reflections
a = 17.034 (6) Å	θ = 10.7–13.8º
b = 9.218 (3) Å	µ = 26.38 mm−1
c = 11.092 (4) Å	T = 293 (2) K
V = 1741.6 (10) Å3	Needle, yellow
Z = 4	0.2 × 0.05 × 0.05 mm

Enraf–Nonius CAD-4 diffractometer	Rint = 0.045
Radiation source: fine-focus sealed tube	θmax = 27.0º
Monochromator: graphite	θmin = 2.2º
T = 293(2) K	h = −1→21
Non–profiled ω/2θ scans	k = −11→3
Absorption correction: ψ scan(North et al., 1968)	l = −1→14
Tmin = 0.095, Tmax = 0.268	2 standard reflections
2906 measured reflections	every 120 min
1998 independent reflections	intensity decay: 5%
1202 reflections with I > 2σ(I)

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)] = 0.040	H-atom parameters constrained
wR(F2) = 0.099	w = 1/[σ2(Fo2) + (0.0394P)2] where P = (Fo2 + 2Fc2)/3
S = 1.00	(Δ/σ)max < 0.001
1998 reflections	Δρmax = 1.57 e Å−3
67 parameters	Δρmin = −1.58 e Å−3
Primary atom site location: structure-invariant direct methods	Extinction correction: none

Experimental. Number of psi-scan sets used was 4 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied (North et al.,1968).

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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	0.49490 (3)	0.2500	0.49379 (7)	0.0376 (2)
Pb2	0.23035 (4)	0.2500	0.86880 (7)	0.0361 (2)
I1	0.32678 (7)	0.2500	0.61874 (12)	0.0482 (4)
I2	0.66724 (7)	0.2500	0.36339 (11)	0.0441 (3)
I3	0.43945 (5)	−0.00127 (10)	0.31479 (9)	0.0458 (3)
N1	0.2835 (7)	−0.0102 (10)	0.8986 (11)	0.049 (3)
H1A	0.2469	−0.0639	0.9365	0.059*
H1B	0.2922	−0.0506	0.8260	0.059*
N2	0.3598 (9)	0.2500	0.9763 (17)	0.055 (5)
H2	0.3467	0.2500	1.0558	0.066*
C2	0.4032 (8)	0.113 (2)	0.9595 (18)	0.079 (6)
H2C	0.4281	0.1143	0.8807	0.094*
H2D	0.4445	0.1075	1.0195	0.094*
C1	0.3559 (10)	−0.0133 (16)	0.9684 (18)	0.076 (6)
H1C	0.3426	−0.0282	1.0525	0.091*
H1D	0.3867	−0.0961	0.9425	0.091*

	U11	U22	U33	U12	U13	U23
Pb1	0.0375 (4)	0.0355 (4)	0.0399 (4)	0.000	0.0008 (3)	0.000
Pb2	0.0285 (3)	0.0402 (4)	0.0397 (4)	0.000	0.0006 (3)	0.000
I1	0.0465 (7)	0.0557 (8)	0.0425 (8)	0.000	0.0098 (7)	0.000
I2	0.0429 (7)	0.0507 (8)	0.0388 (7)	0.000	0.0023 (6)	0.000
I3	0.0484 (5)	0.0472 (6)	0.0419 (5)	−0.0063 (4)	−0.0028 (4)	−0.0008 (5)
N1	0.060 (7)	0.025 (6)	0.062 (9)	0.006 (5)	0.010 (6)	0.001 (6)
N2	0.043 (8)	0.062 (12)	0.059 (12)	0.000	−0.015 (9)	0.000
C2	0.048 (9)	0.084 (14)	0.103 (16)	0.013 (10)	−0.007 (10)	0.011 (13)
C1	0.088 (12)	0.043 (10)	0.096 (16)	0.017 (9)	−0.023 (12)	0.001 (11)

Pb1—I1	3.1816 (17)	N1—H1A	0.9000
Pb1—I3	3.1936 (13)	N1—H1B	0.9000
Pb1—I2	3.2725 (16)	N2—C2	1.476 (18)
Pb1—I3i	3.3190 (13)	N2—H2	0.9100
Pb2—N2	2.506 (15)	C2—C1	1.42 (2)
Pb2—N1	2.585 (10)	C2—H2C	0.9700
Pb2—I2ii	3.1591 (18)	C2—H2D	0.9700
Pb2—I1	3.2236 (17)	C1—H1C	0.9700
Pb2—I3iii	3.7392 (17)	C1—H1D	0.9700
N1—C1	1.457 (19)
I1—Pb1—I3	90.26 (3)	Pb1ix—I3—Pb2viii	74.61 (2)
I3—Pb1—I3iv	92.98 (5)	Pb1—I1—Pb2	146.46 (5)
I1—Pb1—I2	179.59 (4)	Pb2x—I2—Pb1	83.66 (4)
I3—Pb1—I2	89.46 (3)	Pb1—I3—Pb1ix	90.21 (4)
I1—Pb1—I3i	91.41 (3)	C1—N1—Pb2	112.5 (8)
I3—Pb1—I3i	176.76 (3)	C1—N1—H1A	109.1
I3iv—Pb1—I3i	89.79 (4)	Pb2—N1—H1A	109.1
I2—Pb1—I3i	88.88 (3)	C1—N1—H1B	109.1
I3—Pb1—I3v	89.79 (4)	Pb2—N1—H1B	109.1
I3iv—Pb1—I3v	176.76 (3)	H1A—N1—H1B	107.8
I3i—Pb1—I3v	87.39 (4)	C2—N2—C2iv	117.7 (17)
N2—Pb2—N1	68.4 (3)	C2—N2—Pb2	112.4 (9)
N1iv—Pb2—N1	136.3 (5)	C2—N2—H2	104.2
N2—Pb2—I2ii	81.5 (4)	Pb2—N2—H2	104.2
N1—Pb2—I2ii	89.9 (3)	C1—C2—N2	114.1 (12)
N2—Pb2—I1	87.8 (4)	C1—C2—H2C	108.7
N1—Pb2—I1	86.1 (3)	N2—C2—H2C	108.7
I2ii—Pb2—I1	169.26 (4)	C1—C2—H2D	108.7
I3iii—Pb2—N1	73.9 (3)	N2—C2—H2D	108.7
I1—Pb2—I3iii	104.85 (3)	H2C—C2—H2D	107.6
I3iii—Pb2—N2	139.17 (15)	C2—C1—N1	115.4 (13)
I3iii—Pb2—I3vi	75.64 (2)	C2—C1—H1C	108.4
I2vii—Pb2—I3iii	83.54 (3)	N1—C1—H1C	108.4
I3vi—Pb2—N1	149.3 (3)	C2—C1—H1D	108.4
I3vi—Pb2—N1iv	73.8 (3)	N1—C1—H1D	108.4
Pb1—I3—Pb2viii	125.02 (3)	H1C—C1—H1D	107.5
C1—N1—N2—C2	25.1 (14)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···I1xi	0.90	2.93	3.791 (12)	160
N1—H1B···I2v	0.90	2.88	3.746 (12)	163
N2—H2···I2ii	0.91	3.19	3.731 (17)	121

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯I1i	0.90	2.93	3.791 (12)	160
N1—H1B⋯I2ii	0.90	2.88	3.746 (12)	163
N2—H2⋯I2iii	0.91	3.19	3.731 (17)	121

Symmetry codes: (i) ; (ii) ; (iii) .