Poly[di-μ(2)-chlorido(μ(2)-1,3-di-4-pyridylpropane-κN:N')lead(II)].

The title Pb(II) coordination polymer, [PbCl(2)(C(13)H(14)N(2))], was prepared by the hydro-thermal reaction of PbCl(2) with 4,4,-trimethyl-enedipyridine in a 1:1 ratio. It exhibits a two-dimensional layered structural motif consisting of PbCl(2) chains and the flexible bridged 4,4'-trimethyl-enedipyridine ligand. The connections result in a cavity of about 4 × 15 Å.

Related literature

For crystal engineering based upon transition metal coordination polymers, see: Abrahams et al. (1999 ▶). For applications of these metal-organic frameworks, see: Moulton & Zaworotko (2001 ▶); Natarajan & Mahata (2009 ▶). For networks with main group metals as connected nodes, see: Shi et al. (2002 ▶). For the related structure, [PbCl2(4,4′-bipy)] (bipy is bipyridine), see: Nordell et al. (2004 ▶).

Experimental

Crystal data

[PbCl2(C13H14N2)]

M = 476.35

Monoclinic,

a = 4.385 (2) Å

b = 15.455 (3) Å

c = 10.935 (2) Å

β = 97.65 (2)°

V = 734.5 (3) Å3

Z = 2

Mo Kα radiation

μ = 11.84 mm−1

T = 298 K

0.19 × 0.15 × 0.11 mm

Data collection

Bruker SMART CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.139, T max = 0.277

2401 measured reflections

1283 independent reflections

1109 reflections with I > 2σ(I)

R int = 0.033

Refinement

R[F 2 > 2σ(F 2)] = 0.033

wR(F 2) = 0.077

S = 1.01

1283 reflections

88 parameters

H-atom parameters constrained

Δρmax = 0.88 e Å−3

Δρmin = −1.16 e Å−3

Data collection: SMART (Bruker, 1996 ▶); cell refinement: SMART and SAINT (Bruker, 1996 ▶); data reduction: SHELXTL (Sheldrick, 2008 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809036150/pb2006sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809036150/pb2006Isup2.hkl

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

[PbCl2(C13H14N2)]	F(000) = 444
Mr = 476.35	Dx = 2.155 Mg m−3
Monoclinic, P21/m	Melting point: 533.15K K
Hall symbol: -P2yb	Mo Kα radiation, λ = 0.71073 Å
a = 4.385 (2) Å	Cell parameters from 1283 reflections
b = 15.455 (3) Å	θ = 2.6–25.0°
c = 10.935 (2) Å	µ = 11.84 mm−1
β = 97.65 (2)°	T = 298 K
V = 734.5 (3) Å3	Block, yellow
Z = 2	0.19 × 0.15 × 0.11 mm

Bruker SMART CCD diffractometer	1283 independent reflections
Radiation source: fine-focus sealed tube	1109 reflections with I > 2σ(I)
graphite	Rint = 0.033
ω scans	θmax = 25.0°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −5→5
Tmin = 0.139, Tmax = 0.277	k = −15→18
2401 measured reflections	l = −7→12

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) = 0.077	H-atom parameters constrained
S = 1.01	w = 1/[σ2(Fo2) + (0.0359P)2] where P = (Fo2 + 2Fc2)/3
1283 reflections	(Δ/σ)max < 0.001
88 parameters	Δρmax = 0.88 e Å−3
0 restraints	Δρmin = −1.16 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
Pb1	0.32077 (9)	0.7500	0.28349 (4)	0.03780 (17)
Cl2	0.7798 (10)	0.7500	0.1052 (3)	0.0748 (10)
Cl1	−0.1094 (10)	0.7500	0.4619 (3)	0.0719 (10)
C5	0.6217 (18)	0.4150 (5)	0.2292 (8)	0.0431 (19)
N1	0.3822 (16)	0.5787 (4)	0.2702 (7)	0.0482 (17)
C2	0.412 (2)	0.4554 (5)	0.1409 (8)	0.049 (2)
H2A	0.3481	0.4278	0.0662	0.059*
C3	0.574 (2)	0.5401 (5)	0.3555 (8)	0.057 (2)
H3A	0.6288	0.5684	0.4303	0.068*
C1	0.297 (2)	0.5358 (5)	0.1631 (8)	0.049 (2)
H1A	0.1573	0.5616	0.1026	0.059*
C6	0.770 (2)	0.3312 (5)	0.2033 (9)	0.055 (2)
H6A	0.9711	0.3283	0.2527	0.066*
H6B	0.8024	0.3302	0.1171	0.066*
C31	0.698 (2)	0.4595 (5)	0.3397 (9)	0.055 (2)
H3B	0.8335	0.4349	0.4030	0.066*
C7	0.584 (2)	0.2500	0.2302 (11)	0.040 (3)
H7A	0.3863	0.2500	0.1783	0.048*
H7C	0.5474	0.2500	0.3159	0.048*

	U11	U22	U33	U12	U13	U23
Pb1	0.0342 (2)	0.0274 (2)	0.0527 (3)	0.000	0.00873 (17)	0.000
Cl2	0.095 (3)	0.082 (2)	0.047 (2)	0.000	0.0061 (17)	0.000
Cl1	0.102 (3)	0.065 (2)	0.048 (2)	0.000	0.0045 (18)	0.000
C5	0.043 (5)	0.026 (4)	0.066 (6)	−0.005 (3)	0.027 (4)	0.002 (4)
N1	0.057 (4)	0.027 (3)	0.062 (5)	0.006 (3)	0.016 (4)	0.006 (3)
C2	0.062 (5)	0.032 (4)	0.052 (5)	−0.003 (4)	0.008 (4)	−0.003 (4)
C3	0.081 (7)	0.032 (4)	0.056 (6)	0.002 (4)	0.003 (5)	−0.001 (4)
C1	0.053 (5)	0.032 (4)	0.059 (6)	−0.002 (4)	−0.002 (4)	0.009 (4)
C6	0.056 (5)	0.032 (4)	0.083 (7)	−0.002 (4)	0.029 (5)	0.004 (4)
C31	0.060 (6)	0.040 (4)	0.066 (6)	−0.007 (4)	0.005 (5)	0.006 (4)
C7	0.035 (6)	0.023 (5)	0.064 (7)	0.000	0.012 (5)	0.000

Pb1—N1i	2.667 (7)	C2—C1	1.374 (10)
Pb1—N1	2.667 (7)	C2—H2A	0.9300
Pb1—Cl2ii	2.862 (6)	C3—C31	1.379 (11)
Pb1—Cl1	2.887 (5)	C3—H3A	0.9300
Pb1—Cl1iii	2.957 (6)	C1—H1A	0.9300
Pb1—Cl2	2.982 (6)	C6—C7	1.548 (10)
Cl2—Pb1iii	2.862 (6)	C6—H6A	0.9700
Cl1—Pb1ii	2.957 (6)	C6—H6B	0.9700
C5—C31	1.392 (12)	C31—H3B	0.9300
C5—C2	1.390 (12)	C7—C6iv	1.548 (10)
C5—C6	1.494 (11)	C7—H7A	0.9700
N1—C3	1.313 (11)	C7—H7C	0.9700
N1—C1	1.354 (11)
N1i—Pb1—N1	166.1 (3)	C1—C2—H2A	119.8
N1i—Pb1—Cl2ii	92.49 (16)	C5—C2—H2A	119.8
N1—Pb1—Cl2ii	92.49 (16)	N1—C3—C31	123.2 (8)
N1i—Pb1—Cl1	96.69 (14)	N1—C3—H3A	118.4
N1—Pb1—Cl1	96.69 (14)	C31—C3—H3A	118.4
Cl2ii—Pb1—Cl1	84.43 (17)	N1—C1—C2	122.1 (7)
N1i—Pb1—Cl1iii	87.32 (16)	N1—C1—H1A	119.0
N1—Pb1—Cl1iii	87.32 (16)	C2—C1—H1A	119.0
Cl2ii—Pb1—Cl1iii	178.36 (9)	C5—C6—C7	114.3 (7)
Cl1—Pb1—Cl1iii	97.21 (17)	C5—C6—H6A	108.7
N1i—Pb1—Cl2	83.26 (14)	C7—C6—H6A	108.7
N1—Pb1—Cl2	83.26 (14)	C5—C6—H6B	108.7
Cl2ii—Pb1—Cl2	97.21 (17)	C7—C6—H6B	108.7
Cl1—Pb1—Cl2	178.36 (11)	H6A—C6—H6B	107.6
Cl1iii—Pb1—Cl2	81.15 (17)	C3—C31—C5	120.1 (8)
Pb1iii—Cl2—Pb1	97.21 (17)	C3—C31—H3B	120.0
Pb1—Cl1—Pb1ii	97.21 (17)	C5—C31—H3B	120.0
C31—C5—C2	116.2 (7)	C6—C7—C6iv	108.3 (9)
C31—C5—C6	122.2 (8)	C6—C7—H7A	110.0
C2—C5—C6	121.5 (8)	C6iv—C7—H7A	110.0
C3—N1—C1	117.9 (7)	C6—C7—H7C	110.0
C3—N1—Pb1	118.2 (6)	C6iv—C7—H7C	110.0
C1—N1—Pb1	121.0 (5)	H7A—C7—H7C	108.4
C1—C2—C5	120.5 (8)