Poly[1,4-bis-(ammonio-meth-yl)cyclo-hexane [di-μ-iodido-diiodido-plumbate(II)]].

The title compound, {(C(8)H(20)N(2))[PbI(4)]}(n), is an inorganic-organic hybrid. The structure is composed of alternate layers of two-dimensional corner-sharing PbI(6) octa-hedra ( symmetry) and 1,4-bis-(ammonio-meth-yl)cyclo-hexane cations ( symmetry) extending parallel to the bc plane. The cations inter-act with the inorganic layer via N-H⋯I hydrogen bonding in the right-angled halogen sub-type of the terminal halide hydrogen-bonding motif.

Related literature

For other examples of inorganic–organic hybrid structures encorporating cyclic ammonium cations, see: Billing & Lemmerer (2006 ▶). For hydrogen-bonding nomenclature for inorganic–organic hybrids, see: Mitzi (1999 ▶). For the related chloridoplumbate(II), see: Rayner & Billing (2010a ▶) and for the isotypic bromidoplumbate(II), see: Rayner & Billing (2010b ▶).

Experimental

Crystal data

(C8H20N2)[PbI4]

M = 859.05

Monoclinic,

a = 12.2793 (17) Å

b = 8.7413 (12) Å

c = 8.7829 (13) Å

β = 95.922 (3)°

V = 937.7 (2) Å3

Z = 2

Mo Kα radiation

μ = 15.56 mm−1

T = 173 K

0.36 × 0.26 × 0.08 mm

Data collection

Bruker APEXII CCD area-detector diffractometer

Absorption correction: integration (XPREP; Bruker, 2005 ▶) T min = 0.043, T max = 0.288

5435 measured reflections

2264 independent reflections

2085 reflections with I > 2σ(I)

R int = 0.080

Refinement

R[F 2 > 2σ(F 2)] = 0.033

wR(F 2) = 0.093

S = 1.08

2264 reflections

70 parameters

H-atom parameters constrained

Δρmax = 1.76 e Å−3

Δρmin = −2.79 e Å−3

Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2005 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶) and PLATON (Spek, 2009 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681001682X/wm2340sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053681001682X/wm2340Isup2.hkl

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

(C8H20N2)[PbI4]	F(000) = 752
Mr = 859.05	Dx = 3.043 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 6011 reflections
a = 12.2793 (17) Å	θ = 3.0–28.2°
b = 8.7413 (12) Å	µ = 15.56 mm−1
c = 8.7829 (13) Å	T = 173 K
β = 95.922 (3)°	Plate, orange
V = 937.7 (2) Å3	0.36 × 0.26 × 0.08 mm
Z = 2

Bruker APEXII CCD area-detector diffractometer	2264 independent reflections
Radiation source: fine-focus sealed tube	2085 reflections with I > 2σ(I)
graphite	Rint = 0.080
φ and ω scans	θmax = 28.0°, θmin = 1.7°
Absorption correction: integration (XPREP; Bruker, 2005)	h = −16→16
Tmin = 0.043, Tmax = 0.288	k = −11→10
5435 measured reflections	l = −9→11

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)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.093	H-atom parameters constrained
S = 1.08	w = 1/[σ2(Fo2) + (0.0511P)2 + 1.0393P] where P = (Fo2 + 2Fc2)/3
2264 reflections	(Δ/σ)max = 0.009
70 parameters	Δρmax = 1.76 e Å−3
0 restraints	Δρmin = −2.79 e Å−3

Experimental. Numerical intergration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2005)

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
C1	0.2676 (6)	0.0434 (9)	−0.4667 (9)	0.0333 (15)
H1A	0.2773	0.1355	−0.4011	0.040*
H1B	0.2216	0.0719	−0.5617	0.040*
C2	0.3794 (6)	−0.0123 (8)	−0.5065 (8)	0.0273 (15)
H2	0.3672	−0.0991	−0.5804	0.033*
C3	0.4366 (6)	0.1194 (9)	−0.5867 (8)	0.0306 (14)
H3A	0.3890	0.1529	−0.6785	0.037*
H3B	0.4475	0.2077	−0.5162	0.037*
C4	0.4542 (6)	−0.0685 (9)	−0.3667 (8)	0.0299 (14)
H4A	0.4654	0.0151	−0.2906	0.036*
H4B	0.4187	−0.1550	−0.3183	0.036*
N1	0.2111 (5)	−0.0797 (7)	−0.3841 (6)	0.0274 (12)
H1C	0.1450	−0.0448	−0.3610	0.041*
H1D	0.2531	−0.1050	−0.2962	0.041*
H1E	0.2012	−0.1637	−0.4451	0.041*
I1	−0.26315 (4)	0.02539 (5)	−0.02301 (5)	0.02714 (13)
I2	0.00031 (4)	0.18981 (5)	−0.30914 (4)	0.02605 (14)
Pb1	0.0000	0.0000	0.0000	0.01915 (11)

	U11	U22	U33	U12	U13	U23
C1	0.036 (4)	0.026 (3)	0.039 (4)	0.002 (3)	0.005 (3)	0.004 (3)
C2	0.027 (4)	0.027 (4)	0.028 (3)	−0.003 (3)	0.003 (3)	−0.001 (2)
C3	0.028 (3)	0.030 (3)	0.034 (3)	0.000 (3)	0.001 (3)	0.010 (3)
C4	0.023 (3)	0.035 (4)	0.031 (3)	−0.003 (3)	0.002 (3)	0.008 (3)
N1	0.025 (3)	0.031 (3)	0.026 (3)	−0.004 (2)	0.003 (2)	−0.001 (2)
I1	0.0262 (2)	0.0257 (2)	0.0288 (2)	−0.00327 (17)	−0.00048 (18)	−0.00028 (16)
I2	0.0356 (2)	0.0218 (2)	0.0212 (2)	0.00569 (16)	0.00513 (16)	0.00779 (14)
Pb1	0.02537 (19)	0.01599 (17)	0.01602 (16)	0.00087 (11)	0.00182 (12)	0.00032 (10)

C1—N1	1.507 (9)	C4—H4B	0.9900
C1—C2	1.530 (10)	N1—H1C	0.9100
C1—H1A	0.9900	N1—H1D	0.9100
C1—H1B	0.9900	N1—H1E	0.9100
C2—C4	1.536 (10)	I1—Pb1	3.2243 (6)
C2—C3	1.554 (9)	I2—Pb1	3.1824 (5)
C2—H2	1.0000	I2—Pb1ii	3.1875 (5)
C3—C4i	1.510 (10)	Pb1—I2iii	3.1824 (5)
C3—H3A	0.9900	Pb1—I2iv	3.1875 (5)
C3—H3B	0.9900	Pb1—I2v	3.1875 (5)
C4—C3i	1.510 (10)	Pb1—I1iii	3.2243 (6)
C4—H4A	0.9900
N1—C1—C2	110.5 (6)	H4A—C4—H4B	108.1
N1—C1—H1A	109.5	C1—N1—H1C	109.5
C2—C1—H1A	109.5	C1—N1—H1D	109.5
N1—C1—H1B	109.5	H1C—N1—H1D	109.5
C2—C1—H1B	109.5	C1—N1—H1E	109.5
H1A—C1—H1B	108.1	H1C—N1—H1E	109.5
C4—C2—C1	113.3 (6)	H1D—N1—H1E	109.5
C4—C2—C3	109.8 (6)	Pb1—I2—Pb1ii	153.144 (15)
C1—C2—C3	109.0 (6)	I2—Pb1—I2iii	180.00 (2)
C4—C2—H2	108.2	I2—Pb1—I2iv	90.294 (11)
C1—C2—H2	108.2	I2iii—Pb1—I2iv	89.706 (11)
C3—C2—H2	108.2	I2—Pb1—I2v	89.706 (11)
C4i—C3—C2	111.1 (6)	I2iii—Pb1—I2v	90.294 (11)
C4i—C3—H3A	109.4	I2iv—Pb1—I2v	180.0
C2—C3—H3A	109.4	I2—Pb1—I1iii	89.999 (12)
C4i—C3—H3B	109.4	I2iii—Pb1—I1iii	90.001 (12)
C2—C3—H3B	109.4	I2iv—Pb1—I1iii	94.518 (12)
H3A—C3—H3B	108.0	I2v—Pb1—I1iii	85.482 (12)
C3i—C4—C2	110.6 (6)	I2—Pb1—I1	90.001 (12)
C3i—C4—H4A	109.5	I2iii—Pb1—I1	89.999 (12)
C2—C4—H4A	109.5	I2iv—Pb1—I1	85.482 (12)
C3i—C4—H4B	109.5	I2v—Pb1—I1	94.518 (12)
C2—C4—H4B	109.5	I1iii—Pb1—I1	180.0
N1—C1—C2—C4	−55.7 (8)	C3—C2—C4—C3i	−57.0 (9)
N1—C1—C2—C3	−178.2 (6)	Pb1ii—I2—Pb1—I2iv	−0.35 (4)
C4—C2—C3—C4i	57.3 (8)	Pb1ii—I2—Pb1—I2v	179.65 (4)
C1—C2—C3—C4i	−178.1 (6)	Pb1ii—I2—Pb1—I1iii	−94.87 (4)
C1—C2—C4—C3i	−179.1 (6)	Pb1ii—I2—Pb1—I1	85.13 (4)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1D···I1iii	0.91	2.88	3.598 (5)	137
N1—H1E···I1v	0.91	2.84	3.619 (6)	144
N1—H1E···I2vi	0.91	3.12	3.672 (6)	121
N1—H1C···I2	0.91	2.78	3.611 (6)	152

Table 1

Selected bond lengths (Å)

Pb1—I2i	3.1824 (5)
Pb1—I2ii	3.1875 (5)
Pb1—I1i	3.2243 (6)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1D⋯I1i	0.91	2.88	3.598 (5)	137
N1—H1E⋯I1iii	0.91	2.84	3.619 (6)	144
N1—H1E⋯I2iv	0.91	3.12	3.672 (6)	121
N1—H1C⋯I2	0.91	2.78	3.611 (6)	152

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