catena-Poly[[aqua­(3-methyl­benzoato-κ2O,O′)lead(II)]-μ-3-methyl­benzoato-κ4O:O,O′:O′]

Dai, J.; Yang, J.; An, X.

doi:10.1107/S1600536809019771

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 65| Part 7| July 2009| Pages m709-m710

doi:10.1107/S1600536809019771

Open

access

catena-Poly[[aqua(3-methylbenzoato-κ²O,O′)lead(II)]-μ-3-methylbenzoato-κ⁴O:O,O′:O′]

Jun Dai,^a Juan Yang ^b ^* and Xiaobing An ^b

^aInstitute of Safety Science and Engineering, Henan Polytechnic University, Jiaozuo 454003, People's Republic of China, and ^bDepartment of Physical Chemistry, Henan Polytechnic University, Jiaozuo 454003, People's Republic of China
^*Correspondence e-mail: yangjuan0302@yahoo.cn

(Received 10 May 2009; accepted 25 May 2009; online 6 June 2009)

The reaction of lead(II) acetate and 3-methylbenzoic acid (MBA) in aqueous solution yielded the title polymer, [Pb(C₈H₇O₂)₂(H₂O)]_n. The asymmetric unit contains two Pb^II atoms, four MBA ligands and two water molecules. Each Pb^II cation is heptacoordinated and chelated by four carboxylate O atoms from two MBA ligands. The Pb atoms are bridged through the carboxylate O atoms from another two MBA ligands, leading to a central Pb₂O₂ core. The Pb—O bond lengths are in the range 2.325 (3)–2.757 (4) Å. The intra- and interdimer Pb⋯Pb distances are 4.2942 (3) and 4.2283 (3) Å, respectively, indicating little direct metal–metal interaction. The coordinating water molecules and carboxylate O atoms are involved in extensive O—H⋯O hydrogen-bonding interactions. The complex has an extended ladder-like chain structure and the chains are assembled by hydrogen bonds and π–π interactions [centroid–centroid distance = 3.6246 (3) Å] into a three-dimensional supramolecular structure.

Related literature

For general background to metal-organic frameworks and their applications, see: Hamilton et al. (2004 ); Meng et al. (2003 ); Fan & Zhu (2006 ); Wang et al. (2006 ); Masaoka et al. (2001 ). For related structures, see: Shi et al. (2007 ).

Experimental

Crystal data

[Pb(C₈H₇O₂)₂(H₂O)]
M_r = 495.48
Monoclinic, P 2₁ /n
a = 7.1745 (3) Å
b = 42.745 (2) Å
c = 10.7126 (5) Å
β = 90.765 (1)°
V = 3285.0 (3) Å³
Z = 8
Mo Kα radiation
μ = 10.29 mm⁻¹
T = 296 K
0.36 × 0.17 × 0.12 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2007 ) T_min = 0.144, T_max = 0.300
40611 measured reflections
8096 independent reflections
6265 reflections with I > 2σ(I)
R_int = 0.056

Refinement

R[F² > 2σ(F²)] = 0.035
wR(F²) = 0.061
S = 1.03
8096 reflections
397 parameters
H-atom parameters constrained
Δρ_max = 0.87 e Å⁻³
Δρ_min = −1.00 e Å⁻³

Table 1
Selected bond lengths (Å)

Pb1—O4	2.386 (3)
Pb1—O1	2.424 (3)
Pb1—O3	2.594 (3)
Pb1—O5	2.603 (3)
Pb1—O2	2.622 (4)
Pb1—O9	2.724 (4)
Pb1—O6ⁱ	2.751 (3)
Pb2—O6	2.325 (3)
Pb2—O8	2.494 (4)
Pb2—O3ⁱⁱ	2.538 (3)
Pb2—O7	2.565 (4)
Pb2—O10	2.665 (3)
Pb2—O4	2.712 (3)
Pb2—O5	2.757 (4)
Symmetry codes: (i) x-1, y, z; (ii) x+1, y, z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O9—H9A⋯O8	0.82	2.03	2.805 (5)	158
O9—H9B⋯O7ⁱ	0.82	2.25	3.017 (5)	156
O10—H10B⋯O2	0.82	2.12	2.881 (5)	153
O10—H10A⋯O1ⁱⁱ	0.82	1.97	2.774 (5)	166
Symmetry codes: (i) x-1, y, z; (ii) x+1, y, z.

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809019771/fj2218sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809019771/fj2218Isup2.hkl

checkCIF report

Comment top

Interest in porous metal-organic frameworks (MOFs) has been driven by the prospect of generating a wide range of materials with useful properties for applications such as ion-exchange, nonlinear optics and catalysis (Hamilton et al., 2004; Meng et al., 2003; Fan et al. 2006). On the other hand, lead(II) compounds have been increasingly studied (Shi et al. 2007) owing to their possible applications in different fields, especially in environmental protection due to the toxicity of lead and in biological systems for its diverse interactions with biological molecules. As an important family of multidentate O-donor ligands, aromatic carboxylate ligands have been extensively employed in the preparation of metal-organic complexes because of their potential properties and intriguing structural topologies (Wang et al., 2006; Masaoka et al. 2001). Herein, we report the structure of the title complex.

The asymmetric unit of the title complex, [Pb₂(C₈H₇O₂)₄(H₂O)₂]_n, contains two Pb^II cation, four MBA ligands and two coordinating water molecule, as illustrated in Fig. 1. The two Pb atoms are connected via two bridging O atoms belonging to two MBA ligands, resulting the central Pb₂O₂ core tetratomic ring. The Pb—O bond lengths are in the range of 2.325 (3) to 2.757 (4) Å (Table 1). The average distance of two Pb atoms is 4.2942 Å, which leads to the weak metal-metal interactions. This coordination polymer structure presents extended ladder-like chain along the a axis direction. The coordinating water molecules and carboxylate O atoms are involved in extensive O—H···O hydrogen-bonding interactions (Table 2). These chains are assembled by H-bonds and π-π interactions to three-dimensional supramolecular structure.

Related literature top

For general background to metal-organic frameworks and their applications, see: Hamilton et al. (2004); Meng et al. (2003); Fan et al. (2006); Wang et al. (2006); Masaoka et al. (2001). For related structures, see: Shi et al. (2007).

Experimental top

A mixture of Pb(CH₃COO)₂ 3H2O (0.1992 g, 0.52 mmol), MBA (0.1139 g, 0.84 mmol), melamine (0.0255 g, 0.20 mmol) and distilled water (10 ml) was sealed in a 25 ml Teflon-lined stainless autoclave (Shi et al. 2007). The mixture was heated at 373 K for 5 days to give colorless crystals suitable for X-ray diffraction analysis.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The coordination environment around Pb(II) in the title complex with the atom-labeling scheme. Displacement ellipsoids for non-hydrogen atoms are drawn at the 30% probability level.
	Fig. 2. The extended ladder-like chain structure of the title compound.
	Fig. 3. The two-dimensional layer structure of the title compound.
	Fig. 4. The three-dimensional structure of the title compound.

catena-Poly[[aqua(3-methylbenzoato-κ²O,O')lead(II)]- µ-3-methylbenzoato-κ⁴O:O,O':O'] top

Crystal data top

[Pb(C₈H₇O₂)₂(H₂O)]	F(000) = 1872
M_r = 495.48	D_x = 2.004 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 7418 reflections
a = 7.1745 (3) Å	θ = 2.4–25.2°
b = 42.745 (2) Å	µ = 10.29 mm⁻¹
c = 10.7126 (5) Å	T = 296 K
β = 90.765 (1)°	Block, colourless
V = 3285.0 (3) Å³	0.36 × 0.17 × 0.12 mm
Z = 8

Data collection top

Bruker APEXII CCD area-detector diffractometer	8096 independent reflections
Radiation source: fine-focus sealed tube	6265 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.056
ϕ and ω scans	θ_max = 28.2°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −9→9
T_min = 0.144, T_max = 0.300	k = −56→56
40611 measured reflections	l = −14→14

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)] = 0.035	H-atom parameters constrained
wR(F²) = 0.061	w = 1/[σ²(F_o²) + (0.0182P)² + 3.7836P] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max = 0.001
8096 reflections	Δρ_max = 0.87 e Å⁻³
397 parameters	Δρ_min = −1.00 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.082

Crystal data top

[Pb(C₈H₇O₂)₂(H₂O)]	V = 3285.0 (3) Å³
M_r = 495.48	Z = 8
Monoclinic, P2₁/n	Mo Kα radiation
a = 7.1745 (3) Å	µ = 10.29 mm⁻¹
b = 42.745 (2) Å	T = 296 K
c = 10.7126 (5) Å	0.36 × 0.17 × 0.12 mm
β = 90.765 (1)°

Data collection top

Bruker APEXII CCD area-detector diffractometer	8096 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2007)	6265 reflections with I > 2σ(I)
T_min = 0.144, T_max = 0.300	R_int = 0.056
40611 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.035	0 restraints
wR(F²) = 0.061	H-atom parameters constrained
S = 1.03	Δρ_max = 0.87 e Å⁻³
8096 reflections	Δρ_min = −1.00 e Å⁻³
397 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Pb1	0.12243 (2)	0.097018 (5)	0.352944 (18)	0.03251 (6)
Pb2	0.63079 (2)	0.136517 (5)	0.498730 (18)	0.03285 (6)
O1	0.0014 (5)	0.06035 (8)	0.5043 (3)	0.0425 (9)
O2	0.2904 (5)	0.04888 (8)	0.4562 (3)	0.0422 (9)
O3	−0.0208 (5)	0.12954 (8)	0.5322 (3)	0.0417 (9)
O4	0.2740 (4)	0.11793 (8)	0.5341 (3)	0.0382 (8)
O5	0.4697 (5)	0.10648 (9)	0.2967 (3)	0.0431 (9)
O6	0.7648 (4)	0.11863 (8)	0.3157 (3)	0.0361 (8)
O7	0.7820 (5)	0.18516 (8)	0.4032 (4)	0.0456 (9)
O8	0.4875 (5)	0.17631 (9)	0.3567 (4)	0.0532 (11)
O9	0.1259 (5)	0.15838 (9)	0.2844 (4)	0.0536 (11)
H9A	0.2336	0.1648	0.2856	0.064*
H9B	0.0480	0.1635	0.3359	0.064*
O10	0.6329 (5)	0.07555 (8)	0.5507 (3)	0.0435 (9)
H10B	0.5587	0.0665	0.5043	0.052*
H10A	0.7351	0.0704	0.5243	0.052*
C1	0.1464 (7)	0.04397 (11)	0.5191 (5)	0.0350 (12)
C2	0.1449 (7)	0.01859 (11)	0.6140 (5)	0.0327 (11)
C3	−0.0085 (7)	0.01413 (12)	0.6892 (5)	0.0419 (13)
H3A	−0.1126	0.0268	0.6775	0.050*
C4	−0.0118 (8)	−0.00864 (13)	0.7814 (5)	0.0449 (14)
C5	0.1437 (9)	−0.02741 (13)	0.7950 (6)	0.0501 (15)
H5A	0.1450	−0.0428	0.8563	0.060*
C6	0.2948 (8)	−0.02395 (13)	0.7213 (6)	0.0483 (15)
H6A	0.3966	−0.0372	0.7319	0.058*
C7	0.2988 (8)	−0.00088 (12)	0.6303 (5)	0.0416 (13)
H7A	0.4032	0.0016	0.5807	0.050*
C8	−0.1813 (10)	−0.01275 (18)	0.8623 (7)	0.080 (2)
H8A	−0.1591	−0.0294	0.9210	0.121*
H8B	−0.2874	−0.0178	0.8107	0.121*
H8C	−0.2050	0.0063	0.9066	0.121*
C9	0.1354 (7)	0.13040 (11)	0.5855 (4)	0.0297 (11)
C10	0.1578 (7)	0.14561 (12)	0.7091 (5)	0.0367 (12)
C11	0.0214 (9)	0.16600 (13)	0.7525 (6)	0.0514 (15)
H11A	−0.0821	0.1705	0.7024	0.062*
C12	0.0388 (12)	0.17949 (16)	0.8690 (7)	0.072 (2)
C13	0.1933 (15)	0.1719 (2)	0.9412 (7)	0.093 (3)
H13A	0.2058	0.1805	1.0205	0.111*
C14	0.3266 (12)	0.1524 (2)	0.8998 (7)	0.081 (2)
H14A	0.4297	0.1481	0.9505	0.097*
C15	0.3122 (9)	0.13865 (15)	0.7832 (5)	0.0563 (17)
H15A	0.4040	0.1251	0.7551	0.068*
C16	−0.1079 (14)	0.2018 (2)	0.9145 (9)	0.131 (4)
H16A	−0.0742	0.2091	0.9965	0.197*
H16B	−0.2258	0.1912	0.9175	0.197*
H16C	−0.1171	0.2193	0.8586	0.197*
C17	0.6265 (6)	0.10896 (11)	0.2509 (5)	0.0296 (11)
C18	0.6596 (7)	0.10073 (11)	0.1176 (5)	0.0308 (11)
C19	0.5301 (8)	0.08355 (12)	0.0511 (5)	0.0425 (13)
H19A	0.4204	0.0776	0.0896	0.051*
C20	0.5586 (10)	0.07500 (14)	−0.0711 (6)	0.0558 (17)
C21	0.7238 (11)	0.08378 (15)	−0.1256 (6)	0.0634 (19)
H21A	0.7476	0.0777	−0.2072	0.076*
C22	0.8544 (10)	0.10140 (15)	−0.0611 (6)	0.0612 (18)
H22A	0.9636	0.1076	−0.0999	0.073*
C23	0.8229 (8)	0.10979 (13)	0.0606 (5)	0.0420 (13)
H23A	0.9110	0.1215	0.1045	0.050*
C24	0.4110 (11)	0.05680 (17)	−0.1440 (7)	0.090 (3)
H24A	0.4543	0.0528	−0.2269	0.135*
H24B	0.2980	0.0688	−0.1483	0.135*
H24C	0.3875	0.0373	−0.1027	0.135*
C25	0.6358 (8)	0.19171 (13)	0.3421 (5)	0.0413 (13)
C26	0.6358 (8)	0.21833 (13)	0.2526 (5)	0.0437 (14)
C27	0.7935 (9)	0.23678 (13)	0.2416 (5)	0.0500 (15)
H27A	0.8980	0.2324	0.2908	0.060*
C28	0.7986 (11)	0.26149 (15)	0.1590 (6)	0.0643 (19)
C29	0.6435 (15)	0.26682 (19)	0.0853 (7)	0.091 (3)
H29A	0.6446	0.2832	0.0283	0.109*
C30	0.4891 (14)	0.2487 (2)	0.0936 (8)	0.095 (3)
H30A	0.3868	0.2526	0.0417	0.114*
C31	0.4833 (10)	0.22464 (17)	0.1785 (7)	0.069 (2)
H31A	0.3758	0.2126	0.1857	0.083*
C32	0.9668 (12)	0.28192 (18)	0.1483 (8)	0.107 (3)
H32A	0.9438	0.2978	0.0865	0.161*
H32B	1.0717	0.2695	0.1242	0.161*
H32C	0.9928	0.2916	0.2274	0.161*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.02451 (10)	0.04213 (12)	0.03088 (11)	−0.00082 (8)	0.00003 (7)	−0.00184 (9)
Pb2	0.02385 (9)	0.04156 (12)	0.03319 (11)	0.00000 (8)	0.00229 (8)	−0.00581 (9)
O1	0.034 (2)	0.042 (2)	0.052 (2)	0.0036 (17)	0.0058 (18)	0.0068 (18)
O2	0.0285 (19)	0.049 (2)	0.050 (2)	−0.0036 (16)	0.0087 (17)	0.0043 (18)
O3	0.034 (2)	0.053 (2)	0.038 (2)	0.0047 (17)	−0.0067 (17)	−0.0090 (18)
O4	0.0249 (18)	0.049 (2)	0.041 (2)	−0.0005 (16)	0.0056 (16)	−0.0044 (18)
O5	0.0280 (19)	0.059 (2)	0.042 (2)	−0.0028 (17)	0.0080 (17)	−0.0055 (19)
O6	0.0273 (18)	0.050 (2)	0.031 (2)	−0.0020 (16)	−0.0003 (15)	−0.0068 (17)
O7	0.037 (2)	0.042 (2)	0.058 (3)	−0.0016 (17)	−0.0059 (19)	0.0046 (19)
O8	0.039 (2)	0.052 (2)	0.068 (3)	−0.0060 (19)	−0.012 (2)	0.005 (2)
O9	0.035 (2)	0.069 (3)	0.057 (3)	−0.007 (2)	0.0047 (19)	0.001 (2)
O10	0.033 (2)	0.053 (2)	0.045 (2)	0.0014 (17)	0.0021 (17)	−0.0025 (18)
C1	0.032 (3)	0.034 (3)	0.039 (3)	−0.005 (2)	0.000 (2)	−0.004 (2)
C2	0.036 (3)	0.030 (3)	0.033 (3)	−0.005 (2)	−0.001 (2)	−0.004 (2)
C3	0.034 (3)	0.041 (3)	0.051 (4)	−0.003 (2)	0.002 (3)	−0.006 (3)
C4	0.047 (3)	0.044 (3)	0.044 (4)	−0.010 (3)	0.003 (3)	0.001 (3)
C5	0.069 (4)	0.034 (3)	0.047 (4)	−0.003 (3)	−0.007 (3)	0.005 (3)
C6	0.052 (4)	0.038 (3)	0.055 (4)	0.008 (3)	−0.002 (3)	0.005 (3)
C7	0.041 (3)	0.037 (3)	0.047 (4)	0.008 (2)	0.004 (3)	−0.005 (3)
C8	0.069 (5)	0.098 (6)	0.074 (5)	−0.007 (4)	0.018 (4)	0.030 (4)
C9	0.028 (3)	0.035 (3)	0.026 (3)	−0.002 (2)	−0.002 (2)	0.002 (2)
C10	0.041 (3)	0.039 (3)	0.031 (3)	−0.007 (2)	−0.004 (2)	0.004 (2)
C11	0.064 (4)	0.046 (3)	0.044 (4)	0.005 (3)	0.003 (3)	−0.008 (3)
C12	0.111 (6)	0.056 (4)	0.049 (4)	−0.004 (4)	0.008 (4)	−0.013 (4)
C13	0.151 (9)	0.081 (6)	0.045 (5)	−0.023 (6)	−0.015 (5)	−0.022 (4)
C14	0.105 (7)	0.093 (6)	0.044 (4)	−0.022 (5)	−0.029 (4)	0.003 (4)
C15	0.058 (4)	0.073 (4)	0.038 (4)	−0.003 (3)	−0.016 (3)	0.004 (3)
C16	0.178 (10)	0.098 (7)	0.119 (8)	0.041 (7)	0.035 (7)	−0.058 (6)
C17	0.025 (2)	0.034 (3)	0.030 (3)	0.002 (2)	0.002 (2)	0.001 (2)
C18	0.031 (3)	0.027 (3)	0.034 (3)	0.004 (2)	0.005 (2)	0.002 (2)
C19	0.056 (4)	0.041 (3)	0.030 (3)	−0.006 (3)	−0.001 (3)	0.001 (2)
C20	0.086 (5)	0.044 (4)	0.037 (4)	−0.009 (3)	−0.008 (3)	−0.008 (3)
C21	0.106 (6)	0.052 (4)	0.033 (4)	−0.005 (4)	0.020 (4)	−0.005 (3)
C22	0.073 (5)	0.066 (4)	0.046 (4)	−0.005 (4)	0.026 (3)	0.005 (3)
C23	0.043 (3)	0.045 (3)	0.038 (3)	−0.002 (3)	0.003 (3)	0.004 (3)
C24	0.139 (8)	0.079 (5)	0.052 (5)	−0.039 (5)	−0.021 (5)	−0.021 (4)
C25	0.039 (3)	0.040 (3)	0.046 (4)	0.000 (3)	−0.002 (3)	−0.005 (3)
C26	0.053 (4)	0.038 (3)	0.040 (3)	0.007 (3)	−0.004 (3)	−0.007 (3)
C27	0.065 (4)	0.043 (3)	0.042 (4)	0.007 (3)	0.005 (3)	0.000 (3)
C28	0.101 (6)	0.045 (4)	0.047 (4)	0.013 (4)	0.018 (4)	0.002 (3)
C29	0.148 (9)	0.069 (5)	0.057 (5)	0.025 (6)	0.020 (6)	0.025 (4)
C30	0.107 (7)	0.104 (7)	0.074 (6)	0.021 (6)	−0.022 (5)	0.034 (5)
C31	0.064 (5)	0.077 (5)	0.065 (5)	0.000 (4)	−0.014 (4)	0.011 (4)
C32	0.132 (8)	0.070 (5)	0.120 (8)	−0.018 (5)	0.045 (6)	0.028 (5)

Geometric parameters (Å, º) top

Pb1—O4	2.386 (3)	C10—C15	1.387 (7)
Pb1—O1	2.424 (3)	C10—C11	1.395 (7)
Pb1—O3	2.594 (3)	C11—C12	1.380 (8)
Pb1—O5	2.603 (3)	C11—H11A	0.9300
Pb1—O2	2.622 (4)	C12—C13	1.381 (11)
Pb1—O9	2.724 (4)	C12—C16	1.505 (10)
Pb1—O6ⁱ	2.751 (3)	C13—C14	1.348 (11)
Pb2—O6	2.325 (3)	C13—H13A	0.9300
Pb2—O8	2.494 (4)	C14—C15	1.384 (9)
Pb2—O3ⁱⁱ	2.538 (3)	C14—H14A	0.9300
Pb2—O7	2.565 (4)	C15—H15A	0.9300
Pb2—O10	2.665 (3)	C16—H16A	0.9600
Pb2—O4	2.712 (3)	C16—H16B	0.9600
Pb2—O5	2.757 (4)	C16—H16C	0.9600
O1—C1	1.263 (6)	C17—C18	1.493 (7)
O2—C1	1.258 (6)	C18—C19	1.376 (7)
O3—C9	1.251 (5)	C18—C23	1.384 (7)
O3—Pb2ⁱ	2.538 (3)	C19—C20	1.377 (8)
O4—C9	1.261 (5)	C19—H19A	0.9300
O5—C17	1.238 (5)	C20—C21	1.380 (9)
O6—C17	1.273 (5)	C20—C24	1.521 (8)
O6—Pb1ⁱⁱ	2.751 (3)	C21—C22	1.381 (9)
O7—C25	1.261 (6)	C21—H21A	0.9300
O8—C25	1.263 (6)	C22—C23	1.373 (8)
O9—H9A	0.8200	C22—H22A	0.9300
O9—H9B	0.8200	C23—H23A	0.9300
O10—H10B	0.8200	C24—H24A	0.9600
O10—H10A	0.8200	C24—H24B	0.9600
C1—C2	1.487 (7)	C24—H24C	0.9600
C2—C3	1.386 (7)	C25—C26	1.488 (8)
C2—C7	1.392 (7)	C26—C31	1.370 (8)
C3—C4	1.387 (7)	C26—C27	1.386 (8)
C3—H3A	0.9300	C27—C28	1.378 (8)
C4—C5	1.380 (8)	C27—H27A	0.9300
C4—C8	1.513 (8)	C28—C29	1.375 (11)
C5—C6	1.358 (8)	C28—C32	1.495 (10)
C5—H5A	0.9300	C29—C30	1.355 (11)
C6—C7	1.388 (7)	C29—H29A	0.9300
C6—H6A	0.9300	C30—C31	1.375 (10)
C7—H7A	0.9300	C30—H30A	0.9300
C8—H8A	0.9600	C31—H31A	0.9300
C8—H8B	0.9600	C32—H32A	0.9600
C8—H8C	0.9600	C32—H32B	0.9600
C9—C10	1.482 (7)	C32—H32C	0.9600

O4—Pb1—O1	82.05 (12)	C4—C8—H8B	109.5
O4—Pb1—O3	51.51 (11)	H8A—C8—H8B	109.5
O1—Pb1—O3	72.68 (12)	C4—C8—H8C	109.5
O4—Pb1—O5	72.72 (11)	H8A—C8—H8C	109.5
O1—Pb1—O5	127.44 (12)	H8B—C8—H8C	109.5
O3—Pb1—O5	118.56 (11)	O3—C9—O4	119.7 (5)
O4—Pb1—O2	75.46 (12)	O3—C9—C10	120.4 (4)
O1—Pb1—O2	51.48 (11)	O4—C9—C10	119.9 (4)
O3—Pb1—O2	107.02 (11)	C15—C10—C11	120.2 (5)
O5—Pb1—O2	77.50 (11)	C15—C10—C9	119.5 (5)
O4—Pb1—O9	81.54 (12)	C11—C10—C9	120.2 (5)
O1—Pb1—O9	143.85 (12)	C12—C11—C10	120.5 (6)
O3—Pb1—O9	71.86 (12)	C12—C11—H11A	119.8
O5—Pb1—O9	77.05 (11)	C10—C11—H11A	119.8
O2—Pb1—O9	149.74 (11)	C11—C12—C13	118.1 (7)
O4—Pb1—O6ⁱ	113.97 (10)	C11—C12—C16	120.2 (8)
O1—Pb1—O6ⁱ	88.41 (11)	C13—C12—C16	121.8 (7)
O3—Pb1—O6ⁱ	63.23 (10)	C14—C13—C12	121.9 (7)
O5—Pb1—O6ⁱ	143.91 (11)	C14—C13—H13A	119.0
O2—Pb1—O6ⁱ	138.35 (10)	C12—C13—H13A	119.0
O9—Pb1—O6ⁱ	69.48 (10)	C13—C14—C15	121.0 (7)
O6—Pb2—O8	83.21 (13)	C13—C14—H14A	119.5
O6—Pb2—O3ⁱⁱ	70.29 (11)	C15—C14—H14A	119.5
O8—Pb2—O3ⁱⁱ	124.28 (12)	C14—C15—C10	118.4 (7)
O6—Pb2—O7	75.42 (12)	C14—C15—H15A	120.8
O8—Pb2—O7	51.46 (12)	C10—C15—H15A	120.8
O3ⁱⁱ—Pb2—O7	74.37 (12)	C12—C16—H16A	109.5
O6—Pb2—O10	81.57 (11)	C12—C16—H16B	109.5
O8—Pb2—O10	142.70 (12)	H16A—C16—H16B	109.5
O3ⁱⁱ—Pb2—O10	81.54 (11)	C12—C16—H16C	109.5
O7—Pb2—O10	151.05 (11)	H16A—C16—H16C	109.5
O6—Pb2—O4	115.06 (11)	H16B—C16—H16C	109.5
O8—Pb2—O4	84.44 (12)	O5—C17—O6	121.2 (5)
O3ⁱⁱ—Pb2—O4	151.11 (11)	O5—C17—C18	121.1 (4)
O7—Pb2—O4	134.31 (11)	O6—C17—C18	117.7 (4)
O10—Pb2—O4	71.75 (10)	C19—C18—C23	119.4 (5)
O6—Pb2—O5	50.10 (10)	C19—C18—C17	120.4 (5)
O8—Pb2—O5	70.96 (12)	C23—C18—C17	120.2 (5)
O3ⁱⁱ—Pb2—O5	117.25 (10)	C18—C19—C20	121.8 (6)
O7—Pb2—O5	103.86 (11)	C18—C19—H19A	119.1
O10—Pb2—O5	73.13 (11)	C20—C19—H19A	119.1
O4—Pb2—O5	65.60 (10)	C19—C20—C21	118.0 (6)
C1—O1—Pb1	98.1 (3)	C19—C20—C24	120.8 (6)
C1—O2—Pb1	88.9 (3)	C21—C20—C24	121.2 (6)
C9—O3—Pb2ⁱ	159.3 (3)	C20—C21—C22	121.2 (6)
C9—O3—Pb1	89.5 (3)	C20—C21—H21A	119.4
Pb2ⁱ—O3—Pb1	110.94 (12)	C22—C21—H21A	119.4
C9—O4—Pb1	99.2 (3)	C23—C22—C21	119.9 (6)
C9—O4—Pb2	133.5 (3)	C23—C22—H22A	120.1
Pb1—O4—Pb2	114.63 (13)	C21—C22—H22A	120.1
C17—O5—Pb1	169.4 (3)	C22—C23—C18	119.8 (6)
C17—O5—Pb2	84.1 (3)	C22—C23—H23A	120.1
Pb1—O5—Pb2	106.44 (12)	C18—C23—H23A	120.1
C17—O6—Pb2	103.8 (3)	C20—C24—H24A	109.5
C17—O6—Pb1ⁱⁱ	133.6 (3)	C20—C24—H24B	109.5
Pb2—O6—Pb1ⁱⁱ	112.57 (13)	H24A—C24—H24B	109.5
C25—O7—Pb2	91.9 (3)	C20—C24—H24C	109.5
C25—O8—Pb2	95.2 (3)	H24A—C24—H24C	109.5
Pb1—O9—H9A	109.2	H24B—C24—H24C	109.5
Pb1—O9—H9B	93.9	O7—C25—O8	121.1 (5)
H9A—O9—H9B	123.4	O7—C25—C26	119.8 (5)
Pb2—O10—H10B	109.3	O8—C25—C26	119.1 (5)
Pb2—O10—H10A	101.0	C31—C26—C27	119.0 (6)
H10B—O10—H10A	103.9	C31—C26—C25	121.1 (6)
O2—C1—O1	121.4 (5)	C27—C26—C25	119.8 (5)
O2—C1—C2	120.1 (5)	C28—C27—C26	121.3 (6)
O1—C1—C2	118.5 (5)	C28—C27—H27A	119.4
C3—C2—C7	118.7 (5)	C26—C27—H27A	119.4
C3—C2—C1	120.7 (5)	C29—C28—C27	117.9 (7)
C7—C2—C1	120.6 (5)	C29—C28—C32	120.4 (7)
C2—C3—C4	122.1 (5)	C27—C28—C32	121.7 (7)
C2—C3—H3A	118.9	C30—C29—C28	121.5 (7)
C4—C3—H3A	118.9	C30—C29—H29A	119.2
C5—C4—C3	117.5 (5)	C28—C29—H29A	119.2
C5—C4—C8	121.8 (6)	C29—C30—C31	120.2 (8)
C3—C4—C8	120.7 (5)	C29—C30—H30A	119.9
C6—C5—C4	121.7 (6)	C31—C30—H30A	119.9
C6—C5—H5A	119.1	C26—C31—C30	120.0 (7)
C4—C5—H5A	119.1	C26—C31—H31A	120.0
C5—C6—C7	120.7 (5)	C30—C31—H31A	120.0
C5—C6—H6A	119.6	C28—C32—H32A	109.5
C7—C6—H6A	119.6	C28—C32—H32B	109.5
C6—C7—C2	119.3 (5)	H32A—C32—H32B	109.5
C6—C7—H7A	120.4	C28—C32—H32C	109.5
C2—C7—H7A	120.4	H32A—C32—H32C	109.5
C4—C8—H8A	109.5	H32B—C32—H32C	109.5

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9A···O8	0.82	2.03	2.805 (5)	158
O9—H9B···O7ⁱ	0.82	2.25	3.017 (5)	156
O10—H10B···O2	0.82	2.12	2.881 (5)	153
O10—H10A···O1ⁱⁱ	0.82	1.97	2.774 (5)	166

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

Experimental details

Crystal data
Chemical formula	[Pb(C₈H₇O₂)₂(H₂O)]
M_r	495.48
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	296
a, b, c (Å)	7.1745 (3), 42.745 (2), 10.7126 (5)
β (°)	90.765 (1)
V (Å³)	3285.0 (3)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	10.29
Crystal size (mm)	0.36 × 0.17 × 0.12

Data collection
Diffractometer	Bruker APEXII CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2007)
T_min, T_max	0.144, 0.300
No. of measured, independent and observed [I > 2σ(I)] reflections	40611, 8096, 6265
R_int	0.056
(sin θ/λ)_max (Å⁻¹)	0.665

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.035, 0.061, 1.03
No. of reflections	8096
No. of parameters	397
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.87, −1.00

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Pb1—O4	2.386 (3)	Pb2—O6	2.325 (3)
Pb1—O1	2.424 (3)	Pb2—O8	2.494 (4)
Pb1—O3	2.594 (3)	Pb2—O3ⁱⁱ	2.538 (3)
Pb1—O5	2.603 (3)	Pb2—O7	2.565 (4)
Pb1—O2	2.622 (4)	Pb2—O10	2.665 (3)
Pb1—O9	2.724 (4)	Pb2—O4	2.712 (3)
Pb1—O6ⁱ	2.751 (3)	Pb2—O5	2.757 (4)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9A···O8	0.82	2.03	2.805 (5)	158
O9—H9B···O7ⁱ	0.82	2.25	3.017 (5)	156
O10—H10B···O2	0.82	2.12	2.881 (5)	153
O10—H10A···O1ⁱⁱ	0.82	1.97	2.774 (5)	166

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

Acknowledgements

The authors acknowledge the Doctoral Foundation of Henan Polytechnic University (B2008–58 648265).

References

Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Fan, S. R. & Zhu, L. G. (2006). Inorg. Chem. 45, 7935–7942. Web of Science CSD CrossRef PubMed CAS Google Scholar
Hamilton, B. H., Kelly, K. A., Wagler, T. A., Espe, M. P. & Ziegler, C. J. (2004). Inorg. Chem. 43, 50–56. Web of Science CSD CrossRef PubMed CAS Google Scholar
Masaoka, S., Furukawa, S., Chang, H. C., Mizutani, T. & Kitagawa, S. (2001). Angew. Chem. Int. Ed. 40, 3817–3819. CrossRef CAS Google Scholar
Meng, X. R., Song, Y. L., Hou, H. W., Fan, Y. T., Li, G. & Zhu, Y. (2003). Inorg. Chem. 42, 1306–1315. Web of Science CSD CrossRef PubMed CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Shi, J., Xu, J.-N., Zhang, P., Fan, Y., Wang, L., Bi, M.-H., Ma, K.-R. & Song, T.-Y. (2007). Chem. J. Chin. Univ. 28, 1617–1621. CAS Google Scholar
Wang, X. L., Qin, C. & Wang, E. B. (2006). Cryst. Growth. Des. 6, 439-443. Web of Science CSD CrossRef CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 65| Part 7| July 2009| Pages m709-m710

doi:10.1107/S1600536809019771

Open

access

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)