Poly[di-μ(2)-chlorido-tri-μ(2)-terephthalato-tetra-lead(II)].

The title compound, [Pb(4)(C(8)H(4)O(4))(3)Cl(2)](n), consists of a three-dimensional inorganic-organic hybrid framework. The asymmetric unit contains two Pb(2+) cations, one Cl(-) anion and one and a half terephthalate anions, the latter being completed by inversion symmetry. The two Pb(2+) cations are each surrounded by five O atoms and one Cl atom in the form of irregular polyhedra. The cations are linked by μ(2)-O and μ(2)-Cl atoms into binuclear units, which are further extended through Pb-O inter-actions into an undulated inorganic layer parallel to (001). These layers are connected along [001] by the terephthalate groups into a three-dimensional framework.

Related literature

For a description of inorganic–organic hybrid compounds, see: Cheetham et al. (2006 ▶). For Pb—Cl bond lengths, see: Casas (2003 ▶). For a related structure, see: Zhang et al. (2009 ▶).

Experimental

Crystal data

[Pb4(C8H4O4)3Cl2]

M = 1392.00

Monoclinic,

a = 5.9900 (1) Å

b = 11.8529 (2) Å

c = 18.4737 (3) Å

β = 91.778 (1)°

V = 1310.98 (4) Å3

Z = 2

Mo Kα radiation

μ = 25.88 mm−1

T = 296 K

0.32 × 0.26 × 0.21 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T min = 0.000, T max = 0.004

9476 measured reflections

2298 independent reflections

2097 reflections with I > 2σ(I)

R int = 0.044

Refinement

R[F 2 > 2σ(F 2)] = 0.032

wR(F 2) = 0.092

S = 1.00

2298 reflections

192 parameters

H-atom parameters constrained

Δρmax = 2.29 e Å−3

Δρmin = −1.89 e Å−3

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681101779X/wm2483sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053681101779X/wm2483Isup2.hkl

Supplementary material file. DOI: 10.1107/S160053681101779X/wm2483Isup3.cdx

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

[Pb4(C8H4O4)3Cl2]	F(000) = 1228
Mr = 1392.00	Dx = 3.526 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 946 reflections
a = 5.9900 (1) Å	θ = 2.6–25.0°
b = 11.8529 (2) Å	µ = 25.88 mm−1
c = 18.4737 (3) Å	T = 296 K
β = 91.778 (1)°	Block, colourless
V = 1310.98 (4) Å3	0.32 × 0.26 × 0.21 mm
Z = 2

Bruker APEXII CCD diffractometer	2298 independent reflections
Radiation source: fine-focus sealed tube	2097 reflections with I > 2σ(I)
graphite	Rint = 0.044
ω scans	θmax = 25.0°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −7→7
Tmin = 0.000, Tmax = 0.004	k = −14→12
9476 measured reflections	l = −21→21

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)] = 0.032	H-atom parameters constrained
wR(F2) = 0.092	w = 1/[σ2(Fo2) + (0.0714P)2] where P = (Fo2 + 2Fc2)/3
S = 1.00	(Δ/σ)max = 0.001
2298 reflections	Δρmax = 2.29 e Å−3
192 parameters	Δρmin = −1.89 e Å−3
0 restraints	Extinction correction: SHELXTL (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0050 (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	0.06200 (5)	0.80676 (3)	0.303842 (18)	0.01898 (17)
Pb2	0.55452 (5)	1.03175 (2)	0.274731 (18)	0.01933 (17)
O3	0.3541 (9)	0.9266 (5)	0.3789 (3)	0.0218 (13)
O1	0.3892 (9)	0.6746 (5)	0.3379 (4)	0.0225 (13)
O2	0.0928 (10)	0.6826 (5)	0.4068 (4)	0.0294 (15)
O4	0.7213 (10)	0.9102 (5)	0.3742 (3)	0.0267 (14)
C9	0.5436 (13)	0.7355 (7)	0.6138 (5)	0.0172 (17)
C6	0.5453 (14)	0.8489 (6)	0.4809 (5)	0.0187 (18)
C8	0.3524 (13)	0.7937 (6)	0.5872 (5)	0.0185 (18)
H8	0.2240	0.7939	0.6142	0.022*
C7	0.3522 (13)	0.8504 (7)	0.5216 (5)	0.0190 (18)
H7	0.2256	0.8890	0.5049	0.023*
C10	0.7317 (13)	0.7385 (7)	0.5731 (5)	0.0210 (19)
H10	0.8601	0.7021	0.5904	0.025*
C5	0.5390 (13)	0.8979 (6)	0.4063 (4)	0.0163 (17)
C11	0.7360 (13)	0.7938 (7)	0.5077 (5)	0.0185 (18)
H11	0.8660	0.7944	0.4814	0.022*
O5	0.7114 (9)	0.6137 (5)	0.7009 (4)	0.0289 (15)
O6	0.3527 (11)	0.6448 (6)	0.7080 (4)	0.0341 (16)
C12	0.5354 (15)	0.6614 (7)	0.6791 (5)	0.024 (2)
C3	0.2855 (14)	0.5387 (6)	0.5111 (5)	0.0192 (19)
H3	0.1419	0.5653	0.5184	0.023*
C1	0.2880 (13)	0.6461 (6)	0.3939 (5)	0.0175 (18)
C4	0.6133 (14)	0.5318 (6)	0.4382 (5)	0.022 (2)
H4	0.6893	0.5533	0.3973	0.026*
C2	0.3971 (13)	0.5706 (6)	0.4485 (5)	0.0188 (18)
Cl1	−0.0398 (3)	0.5962 (2)	0.23077 (13)	0.0308 (6)

	U11	U22	U33	U12	U13	U23
Pb1	0.0220 (2)	0.0166 (2)	0.0183 (3)	0.00318 (11)	0.00007 (15)	0.00127 (12)
Pb2	0.0310 (2)	0.0113 (2)	0.0157 (3)	0.00216 (11)	0.00038 (15)	0.00016 (12)
O3	0.026 (3)	0.014 (3)	0.026 (4)	0.002 (2)	−0.004 (3)	0.009 (3)
O1	0.026 (3)	0.017 (3)	0.024 (4)	0.003 (2)	0.000 (3)	0.003 (3)
O2	0.031 (3)	0.030 (4)	0.028 (4)	0.008 (3)	0.003 (3)	0.003 (3)
O4	0.033 (3)	0.032 (4)	0.015 (4)	0.003 (3)	0.004 (3)	0.005 (3)
C9	0.026 (4)	0.015 (4)	0.011 (5)	−0.005 (3)	−0.003 (3)	−0.003 (3)
C6	0.033 (4)	0.006 (4)	0.017 (5)	0.005 (3)	0.001 (4)	0.003 (3)
C8	0.022 (4)	0.013 (4)	0.021 (5)	−0.003 (3)	0.001 (4)	0.000 (3)
C7	0.027 (4)	0.011 (4)	0.020 (5)	−0.002 (3)	0.005 (4)	−0.005 (3)
C10	0.020 (4)	0.021 (5)	0.022 (5)	0.001 (3)	0.000 (4)	0.004 (4)
C5	0.029 (4)	0.008 (4)	0.012 (4)	−0.003 (3)	0.000 (3)	−0.002 (3)
C11	0.015 (4)	0.020 (4)	0.020 (5)	0.000 (3)	0.000 (3)	0.000 (4)
O5	0.031 (3)	0.026 (3)	0.029 (4)	0.001 (3)	−0.005 (3)	0.017 (3)
O6	0.038 (3)	0.034 (4)	0.031 (4)	−0.002 (3)	0.011 (3)	0.008 (3)
C12	0.039 (5)	0.009 (4)	0.024 (5)	0.002 (4)	0.008 (4)	−0.003 (4)
C3	0.023 (4)	0.010 (4)	0.025 (5)	0.002 (3)	−0.002 (4)	0.000 (3)
C1	0.029 (4)	0.005 (4)	0.018 (5)	0.000 (3)	−0.003 (4)	−0.004 (3)
C4	0.029 (4)	0.012 (4)	0.025 (5)	−0.006 (3)	0.010 (4)	−0.002 (4)
C2	0.029 (4)	0.006 (4)	0.021 (5)	−0.001 (3)	−0.006 (3)	−0.008 (3)
Cl1	0.0314 (11)	0.0227 (13)	0.0378 (16)	−0.0032 (8)	−0.0046 (10)	−0.0067 (10)

Pb1—O2	2.407 (7)	C6—C7	1.400 (11)
Pb1—O1	2.572 (6)	C6—C5	1.493 (12)
Pb1—O6i	2.586 (6)	C8—C7	1.386 (13)
Pb1—O3	2.618 (6)	C8—H8	0.9300
Pb1—O4ii	2.743 (6)	C7—H7	0.9300
Pb1—Cl1	2.893 (2)	C10—C11	1.376 (13)
Pb2—O5i	2.408 (6)	C10—H10	0.9300
Pb2—O4	2.516 (6)	C11—H11	0.9300
Pb2—O3	2.616 (6)	O5—C12	1.252 (11)
Pb2—O6i	2.696 (7)	O5—Pb2vi	2.408 (6)
Pb2—O1iii	2.712 (6)	O6—C12	1.248 (11)
Pb2—Cl1iii	3.010 (2)	O6—Pb1vi	2.586 (6)
O3—C5	1.250 (10)	O6—Pb2vi	2.696 (7)
O1—C1	1.261 (10)	C3—C4vii	1.381 (13)
O1—Pb2iv	2.712 (6)	C3—C2	1.404 (12)
O2—C1	1.276 (10)	C3—H3	0.9300
O4—C5	1.268 (9)	C1—C2	1.485 (12)
O4—Pb1v	2.743 (6)	C4—C2	1.393 (12)
C9—C10	1.374 (11)	C4—C3vii	1.381 (13)
C9—C8	1.412 (12)	C4—H4	0.9300
C9—C12	1.494 (12)	Cl1—Pb2iv	3.010 (2)
C6—C11	1.394 (12)
O2—Pb1—O1	52.8 (2)	C10—C9—C12	120.3 (8)
O2—Pb1—O6i	129.8 (2)	C8—C9—C12	121.4 (7)
O1—Pb1—O6i	77.2 (2)	C11—C6—C7	119.8 (8)
O2—Pb1—O3	83.1 (2)	C11—C6—C5	120.5 (7)
O1—Pb1—O3	73.08 (18)	C7—C6—C5	119.6 (8)
O6i—Pb1—O3	77.8 (2)	C7—C8—C9	121.3 (8)
O2—Pb1—O4ii	86.51 (19)	C7—C8—H8	119.3
O1—Pb1—O4ii	136.8 (2)	C9—C8—H8	119.3
O6i—Pb1—O4ii	138.75 (19)	C8—C7—C6	119.1 (8)
O3—Pb1—O4ii	90.08 (19)	C8—C7—H7	120.5
O2—Pb1—Cl1	81.44 (17)	C6—C7—H7	120.5
O1—Pb1—Cl1	74.74 (15)	C9—C10—C11	122.1 (8)
O6i—Pb1—Cl1	90.49 (16)	C9—C10—H10	119.0
O3—Pb1—Cl1	147.46 (13)	C11—C10—H10	119.0
O4ii—Pb1—Cl1	117.23 (14)	O3—C5—O4	122.9 (8)
O5i—Pb2—O4	81.4 (2)	O3—C5—C6	118.4 (7)
O5i—Pb2—O3	105.8 (2)	O4—C5—C6	118.7 (7)
O4—Pb2—O3	51.03 (18)	C10—C11—C6	119.9 (8)
O5i—Pb2—O6i	50.39 (19)	C10—C11—H11	120.1
O4—Pb2—O6i	93.0 (2)	C6—C11—H11	120.1
O3—Pb2—O6i	75.9 (2)	C12—O5—Pb2vi	99.6 (5)
O5i—Pb2—O1iii	87.3 (2)	C12—O6—Pb1vi	151.2 (6)
O4—Pb2—O1iii	149.49 (18)	C12—O6—Pb2vi	86.1 (5)
O3—Pb2—O1iii	158.89 (17)	Pb1vi—O6—Pb2vi	99.3 (2)
O6i—Pb2—O1iii	101.5 (2)	O6—C12—O5	122.1 (9)
O5i—Pb2—Cl1iii	76.61 (15)	O6—C12—C9	119.3 (8)
O4—Pb2—Cl1iii	78.94 (14)	O5—C12—C9	118.5 (7)
O3—Pb2—Cl1iii	127.69 (14)	C4vii—C3—C2	120.7 (8)
O6i—Pb2—Cl1iii	126.97 (14)	C4vii—C3—H3	119.7
O1iii—Pb2—Cl1iii	70.88 (13)	C2—C3—H3	119.7
C5—O3—Pb1	129.5 (5)	O1—C1—O2	121.9 (8)
C5—O3—Pb2	90.4 (5)	O1—C1—C2	120.4 (7)
Pb1—O3—Pb2	100.5 (2)	O2—C1—C2	117.6 (8)
C1—O1—Pb1	89.0 (5)	C2—C4—C3vii	119.9 (8)
C1—O1—Pb2iv	122.4 (5)	C2—C4—H4	120.1
Pb1—O1—Pb2iv	107.7 (2)	C3vii—C4—H4	120.1
C1—O2—Pb1	96.2 (5)	C4—C2—C3	119.4 (8)
C5—O4—Pb2	94.6 (5)	C4—C2—C1	119.8 (8)
C5—O4—Pb1v	146.6 (5)	C3—C2—C1	120.7 (7)
Pb2—O4—Pb1v	101.2 (2)	Pb1—Cl1—Pb2iv	92.57 (6)
C10—C9—C8	117.9 (8)
O2—Pb1—O3—C5	53.6 (7)	C11—C6—C7—C8	−2.1 (12)
O1—Pb1—O3—C5	0.4 (6)	C5—C6—C7—C8	172.8 (8)
O6i—Pb1—O3—C5	−79.7 (7)	C8—C9—C10—C11	−1.4 (13)
O4ii—Pb1—O3—C5	140.1 (7)	C12—C9—C10—C11	171.3 (8)
Cl1—Pb1—O3—C5	−8.4 (8)	Pb1—O3—C5—O4	93.5 (9)
O2—Pb1—O3—Pb2	152.9 (2)	Pb2—O3—C5—O4	−10.5 (8)
O1—Pb1—O3—Pb2	99.8 (2)	Pb1—O3—C5—C6	−87.7 (9)
O6i—Pb1—O3—Pb2	19.6 (2)	Pb2—O3—C5—C6	168.3 (6)
O4ii—Pb1—O3—Pb2	−120.60 (19)	Pb2—O4—C5—O3	11.0 (8)
Cl1—Pb1—O3—Pb2	90.9 (3)	Pb1v—O4—C5—O3	−107.5 (10)
O5i—Pb2—O3—C5	70.4 (5)	Pb2—O4—C5—C6	−167.8 (6)
O4—Pb2—O3—C5	5.7 (4)	Pb1v—O4—C5—C6	73.7 (12)
O6i—Pb2—O3—C5	111.4 (5)	C11—C6—C5—O3	166.2 (7)
O1iii—Pb2—O3—C5	−163.2 (5)	C7—C6—C5—O3	−8.6 (11)
Cl1iii—Pb2—O3—C5	−14.7 (5)	C11—C6—C5—O4	−15.0 (12)
O5i—Pb2—O3—Pb1	−60.0 (2)	C7—C6—C5—O4	170.3 (7)
O4—Pb2—O3—Pb1	−124.7 (3)	C9—C10—C11—C6	0.0 (13)
O6i—Pb2—O3—Pb1	−18.97 (19)	C7—C6—C11—C10	1.8 (13)
O1iii—Pb2—O3—Pb1	66.4 (6)	C5—C6—C11—C10	−173.0 (8)
Cl1iii—Pb2—O3—Pb1	−145.12 (11)	Pb1vi—O6—C12—O5	88.8 (13)
O2—Pb1—O1—C1	−2.0 (5)	Pb2vi—O6—C12—O5	−13.2 (9)
O6i—Pb1—O1—C1	173.1 (5)	Pb1vi—O6—C12—C9	−94.5 (15)
O3—Pb1—O1—C1	92.2 (5)	Pb2vi—O6—C12—C9	163.4 (7)
O4ii—Pb1—O1—C1	20.9 (6)	Pb2vi—O5—C12—O6	15.0 (10)
Cl1—Pb1—O1—C1	−92.8 (5)	Pb2vi—O5—C12—C9	−161.6 (6)
O2—Pb1—O1—Pb2iv	121.8 (3)	C10—C9—C12—O6	−167.9 (8)
O6i—Pb1—O1—Pb2iv	−63.0 (2)	C8—C9—C12—O6	4.6 (13)
O3—Pb1—O1—Pb2iv	−144.0 (2)	C10—C9—C12—O5	8.9 (13)
O4ii—Pb1—O1—Pb2iv	144.8 (2)	C8—C9—C12—O5	−178.7 (8)
Cl1—Pb1—O1—Pb2iv	31.07 (15)	Pb1—O1—C1—O2	3.6 (8)
O1—Pb1—O2—C1	2.0 (4)	Pb2iv—O1—C1—O2	−106.9 (8)
O6i—Pb1—O2—C1	−4.1 (6)	Pb1—O1—C1—C2	−174.6 (7)
O3—Pb1—O2—C1	−72.0 (5)	Pb2iv—O1—C1—C2	75.0 (9)
O4ii—Pb1—O2—C1	−162.5 (5)	Pb1—O2—C1—O1	−3.9 (9)
Cl1—Pb1—O2—C1	79.3 (5)	Pb1—O2—C1—C2	174.4 (6)
O5i—Pb2—O4—C5	−124.1 (5)	C3vii—C4—C2—C3	0.8 (14)
O3—Pb2—O4—C5	−5.6 (4)	C3vii—C4—C2—C1	−179.8 (7)
O6i—Pb2—O4—C5	−74.9 (5)	C4vii—C3—C2—C4	−0.8 (14)
O1iii—Pb2—O4—C5	166.5 (4)	C4vii—C3—C2—C1	179.8 (8)
Cl1iii—Pb2—O4—C5	158.0 (5)	O1—C1—C2—C4	0.5 (12)
O5i—Pb2—O4—Pb1v	26.4 (2)	O2—C1—C2—C4	−177.7 (7)
O3—Pb2—O4—Pb1v	144.8 (3)	O1—C1—C2—C3	179.9 (7)
O6i—Pb2—O4—Pb1v	75.6 (2)	O2—C1—C2—C3	1.7 (12)
O1iii—Pb2—O4—Pb1v	−43.1 (5)	O2—Pb1—Cl1—Pb2iv	−79.96 (15)
Cl1iii—Pb2—O4—Pb1v	−51.54 (15)	O1—Pb1—Cl1—Pb2iv	−26.31 (15)
C10—C9—C8—C7	1.1 (12)	O6i—Pb1—Cl1—Pb2iv	50.27 (17)
C12—C9—C8—C7	−171.5 (8)	O3—Pb1—Cl1—Pb2iv	−17.5 (3)
C9—C8—C7—C6	0.6 (12)	O4ii—Pb1—Cl1—Pb2iv	−161.53 (15)

Table 1

Selected bond lengths (Å)

Pb1—O2	2.407 (7)
Pb1—O1	2.572 (6)
Pb1—O6i	2.586 (6)
Pb1—O3	2.618 (6)
Pb1—O4ii	2.743 (6)
Pb1—Cl1	2.893 (2)
Pb2—O5i	2.408 (6)
Pb2—O4	2.516 (6)
Pb2—O3	2.616 (6)
Pb2—O6i	2.696 (7)
Pb2—O1iii	2.712 (6)
Pb2—Cl1iii	3.010 (2)

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