Poly[di-μ2-chlorido-tri-μ2-terephthalato-tetra­lead(II)]

Yang, L.; Li, Z.; Li, G.

doi:10.1107/S160053681101779X

metal-organic compounds

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Volume 67| Part 6| June 2011| Page m761

doi:10.1107/S160053681101779X

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Poly[di-μ₂-chlorido-tri-μ₂-terephthalato-tetralead(II)]

Lei Yang,^a ^* Zhongyue Li ^a and Guanghua Li ^b

^aThe Department of Physics–Chemistry, Henan Polytechnic University, Jiao Zuo 454150, People's Republic of China, and ^bState Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, People's Republic of China
^*Correspondence e-mail: xcy78413@tom.com

(Received 14 April 2011; accepted 11 May 2011; online 20 May 2011)

The title compound, [Pb₄(C₈H₄O₄)₃Cl₂]_n, consists of a three-dimensional inorganic–organic hybrid framework. The asymmetric unit contains two Pb²⁺ cations, one Cl⁻ anion and one and a half terephthalate anions, the latter being completed by inversion symmetry. The two Pb²⁺ cations are each surrounded by five O atoms and one Cl atom in the form of irregular polyhedra. The cations are linked by μ₂-O and μ₂-Cl atoms into binuclear units, which are further extended through Pb—O interactions 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_r = 1392.00
Monoclinic, P 2₁ /c
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[F² > 2σ(F²)] = 0.032
wR(F²) = 0.092
S = 1.00
2298 reflections
192 parameters
H-atom parameters constrained
Δρ_max = 2.29 e Å⁻³
Δρ_min = −1.89 e Å⁻³

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) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (ii) x-1, y, z; (iii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

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.

Supporting information

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

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

Supporting information file. DOI: 10.1107/S160053681101779X/wm2483Isup3.cdx

checkCIF report

Comment top

According to the classification scheme of Cheetham et al. (2006), hybrid compounds are divided into two categories: metal-organic coordination polymers and extended inorganic hybrids. In contrast to metal-organic coordination polymers, extended inorganic hybrids which contain extended arrays of inorganic connectivity, M—X—M (M = metal, X = O, Cl, N, and S), have been scarcely investigated. Up to now, only some lead-containing compounds with aromatic carboxylate ligands forming an extended inorganic hybrid network have been reported (Zhang et al., 2009).

The asymmetric unit of the title compound, [Pb₄(C₈H₄O₄)₃Cl₂]_n, consists of two Pb²⁺ cations, one Cl^- anion and one and a half crystallographically independent terephthalate ligands. The C5 containing terephthalate ligand lies in a general position and the other half one is located at a center of inversion. An ORTEP drawing of the coordination environment of the Pb²⁺ cations is shown in Figure 1. The two unique lead atoms are both six-coordinate by five O atoms from tetephtalate anions and one Cl atom in the form of irregular polyhedra. Pb1 is connected to O1 and O2 from a bidentately coordinating anion, to O3, O4 and O6 from three monodentately coordinating anions and to one Cl atom. Pb2 is coordinated by O3, O4, O5, O6 from two bidentatly coordinating anions and by O1 from a monodentately coordinating anion and by one Cl atom. Pb1 and Pb2 atoms are linked by µ₂-O1 and µ₂-Cl1 to form a binuclear unit. These units are further extended into a wave-like 2-D inorganic layer parallel to (001) by sharing additional O atoms (Fig. 2). The Pb—O bond lengths are in the range of 2.4077 (7) to 2.743 (6) Å. The Pb—Cl bond lengths lie in the range of 2.893 (2) to 3.010 (2) Å, values comparable with similar structures (Casas, 2003). The parallel 2-D inorganic layers are connected along [001] by terephthalic groups to form the 3-D framework, as shown in Figure 3.

It is worth noticing that it is rare that in the inorganic layers adjacent Pb atoms are linked by one bridging chloride atom and one bridging oxygen atom other than two Cl or O atoms.

Related literature top

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 top

The title compound was synthesized under hydrothermal conditions. All reagents were of analytical grade. A suspension of Pb(NO₃)₂ (1 mmol) and 4,4'-bipyridine (2 mmol) in water (5 ml) was slowly added into a solution of terephthalic acid (2 mmol) in ethanol (10 ml) and was subsequently stirred. The resulting mixture was further stirred for 4 h at 393 K, and then filtered off. The filtrate pH was adjusted to 3 by hydrochloric acid. The final reaction mixture was heated in a sealed Teflon-lined steel autoclave at 453 K for 7 days. The autoclave was then cooled down to room temperature and colourless block-shaped single crystals were isolated, washed with distilled water and dried in air.

Computing details top

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

Figures top

	Fig. 1. An ORTEP plot of the Pb-environment in the title compound showing 50% probability ellipsoids and the atom labeling scheme.
	Fig. 2. The (001) plane of the title compound, dispaying a wave-like 2-D 12-ring inorganic network with Pb atoms (grey) linked by O (red) and Cl atoms (green).
	Fig. 3. View of the structure along [100], showing the connection of the inorganic layers by terephthalic groups along [001].

Poly[di-µ₂-chlorido-tri-µ₂-terephthalato-tetralead(II)] top

Crystal data top

[Pb₄(C₈H₄O₄)₃Cl₂]	F(000) = 1228
M_r = 1392.00	D_x = 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

Data collection top

Bruker APEXII CCD diffractometer	2298 independent reflections
Radiation source: fine-focus sealed tube	2097 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.044
ω scans	θ_max = 25.0°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −7→7
T_min = 0.000, T_max = 0.004	k = −14→12
9476 measured reflections	l = −21→21

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)] = 0.032	H-atom parameters constrained
wR(F²) = 0.092	w = 1/[σ²(F_o²) + (0.0714P)²] where P = (F_o² + 2F_c²)/3
S = 1.00	(Δ/σ)_max = 0.001
2298 reflections	Δρ_max = 2.29 e Å⁻³
192 parameters	Δρ_min = −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)

Crystal data top

[Pb₄(C₈H₄O₄)₃Cl₂]	V = 1310.98 (4) Å³
M_r = 1392.00	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 5.9900 (1) Å	µ = 25.88 mm⁻¹
b = 11.8529 (2) Å	T = 296 K
c = 18.4737 (3) Å	0.32 × 0.26 × 0.21 mm
β = 91.778 (1)°

Data collection top

Bruker APEXII CCD diffractometer	2298 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2008)	2097 reflections with I > 2σ(I)
T_min = 0.000, T_max = 0.004	R_int = 0.044
9476 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	0 restraints
wR(F²) = 0.092	H-atom parameters constrained
S = 1.00	Δρ_max = 2.29 e Å⁻³
2298 reflections	Δρ_min = −1.89 e Å⁻³
192 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	0.06200 (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)

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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—Pb2^vi	2.408 (6)
Pb2—O1ⁱⁱⁱ	2.712 (6)	O6—C12	1.248 (11)
Pb2—Cl1ⁱⁱⁱ	3.010 (2)	O6—Pb1^vi	2.586 (6)
O3—C5	1.250 (10)	O6—Pb2^vi	2.696 (7)
O1—C1	1.261 (10)	C3—C4^vii	1.381 (13)
O1—Pb2^iv	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—Pb1^v	2.743 (6)	C4—C2	1.393 (12)
C9—C10	1.374 (11)	C4—C3^vii	1.381 (13)
C9—C8	1.412 (12)	C4—H4	0.9300
C9—C12	1.494 (12)	Cl1—Pb2^iv	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—Pb2^vi	99.6 (5)
O5ⁱ—Pb2—O1ⁱⁱⁱ	87.3 (2)	C12—O6—Pb1^vi	151.2 (6)
O4—Pb2—O1ⁱⁱⁱ	149.49 (18)	C12—O6—Pb2^vi	86.1 (5)
O3—Pb2—O1ⁱⁱⁱ	158.89 (17)	Pb1^vi—O6—Pb2^vi	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)	C4^vii—C3—C2	120.7 (8)
O6ⁱ—Pb2—Cl1ⁱⁱⁱ	126.97 (14)	C4^vii—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—C3^vii	119.9 (8)
C1—O1—Pb2^iv	122.4 (5)	C2—C4—H4	120.1
Pb1—O1—Pb2^iv	107.7 (2)	C3^vii—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—Pb1^v	146.6 (5)	C3—C2—C1	120.7 (7)
Pb2—O4—Pb1^v	101.2 (2)	Pb1—Cl1—Pb2^iv	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)	Pb1^v—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)	Pb1^v—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)	Pb1^vi—O6—C12—O5	88.8 (13)
O2—Pb1—O1—C1	−2.0 (5)	Pb2^vi—O6—C12—O5	−13.2 (9)
O6ⁱ—Pb1—O1—C1	173.1 (5)	Pb1^vi—O6—C12—C9	−94.5 (15)
O3—Pb1—O1—C1	92.2 (5)	Pb2^vi—O6—C12—C9	163.4 (7)
O4ⁱⁱ—Pb1—O1—C1	20.9 (6)	Pb2^vi—O5—C12—O6	15.0 (10)
Cl1—Pb1—O1—C1	−92.8 (5)	Pb2^vi—O5—C12—C9	−161.6 (6)
O2—Pb1—O1—Pb2^iv	121.8 (3)	C10—C9—C12—O6	−167.9 (8)
O6ⁱ—Pb1—O1—Pb2^iv	−63.0 (2)	C8—C9—C12—O6	4.6 (13)
O3—Pb1—O1—Pb2^iv	−144.0 (2)	C10—C9—C12—O5	8.9 (13)
O4ⁱⁱ—Pb1—O1—Pb2^iv	144.8 (2)	C8—C9—C12—O5	−178.7 (8)
Cl1—Pb1—O1—Pb2^iv	31.07 (15)	Pb1—O1—C1—O2	3.6 (8)
O1—Pb1—O2—C1	2.0 (4)	Pb2^iv—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)	Pb2^iv—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)	C3^vii—C4—C2—C3	0.8 (14)
O3—Pb2—O4—C5	−5.6 (4)	C3^vii—C4—C2—C1	−179.8 (7)
O6ⁱ—Pb2—O4—C5	−74.9 (5)	C4^vii—C3—C2—C4	−0.8 (14)
O1ⁱⁱⁱ—Pb2—O4—C5	166.5 (4)	C4^vii—C3—C2—C1	179.8 (8)
Cl1ⁱⁱⁱ—Pb2—O4—C5	158.0 (5)	O1—C1—C2—C4	0.5 (12)
O5ⁱ—Pb2—O4—Pb1^v	26.4 (2)	O2—C1—C2—C4	−177.7 (7)
O3—Pb2—O4—Pb1^v	144.8 (3)	O1—C1—C2—C3	179.9 (7)
O6ⁱ—Pb2—O4—Pb1^v	75.6 (2)	O2—C1—C2—C3	1.7 (12)
O1ⁱⁱⁱ—Pb2—O4—Pb1^v	−43.1 (5)	O2—Pb1—Cl1—Pb2^iv	−79.96 (15)
Cl1ⁱⁱⁱ—Pb2—O4—Pb1^v	−51.54 (15)	O1—Pb1—Cl1—Pb2^iv	−26.31 (15)
C10—C9—C8—C7	1.1 (12)	O6ⁱ—Pb1—Cl1—Pb2^iv	50.27 (17)
C12—C9—C8—C7	−171.5 (8)	O3—Pb1—Cl1—Pb2^iv	−17.5 (3)
C9—C8—C7—C6	0.6 (12)	O4ⁱⁱ—Pb1—Cl1—Pb2^iv	−161.53 (15)

Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x−1, y, z; (iii) −x+1, y+1/2, −z+1/2; (iv) −x+1, y−1/2, −z+1/2; (v) x+1, y, z; (vi) x, −y+3/2, z+1/2; (vii) −x+1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	[Pb₄(C₈H₄O₄)₃Cl₂]
M_r	1392.00
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	296
a, b, c (Å)	5.9900 (1), 11.8529 (2), 18.4737 (3)
β (°)	91.778 (1)
V (Å³)	1310.98 (4)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	25.88
Crystal size (mm)	0.32 × 0.26 × 0.21

Data collection
Diffractometer	Bruker APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2008)
T_min, T_max	0.000, 0.004
No. of measured, independent and observed [I > 2σ(I)] reflections	9476, 2298, 2097
R_int	0.044
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.092, 1.00
No. of reflections	2298
No. of parameters	192
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	2.29, −1.89

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXTL (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997).

Selected bond lengths (Å) top

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

Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x−1, y, z; (iii) −x+1, y+1/2, −z+1/2.

Acknowledgements

We would like to thank the National Science Fund for Young Scholars of China (No. 20901028/B0107) and the Open Research Fund of State Key Laboratory of Inorganic Synthesis and Preparative Chemistry (grant No. 2011–26).

References

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