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Acta Crystallogr Sect E Struct Rep Online. 2009 July 1; 65(Pt 7): m709–m710.
Published online 2009 June 6. doi:  10.1107/S1600536809019771
PMCID: PMC2969469

catena-Poly[[aqua­(3-methyl­benzoato-κ2 O,O′)lead(II)]-μ-3-methyl­benzoato-κ4 O:O,O′:O′]

Abstract

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 PbII atoms, four MBA ligands and two water mol­ecules. Each PbII 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 [triangle]); Meng et al. (2003 [triangle]); Fan & Zhu (2006 [triangle]); Wang et al. (2006 [triangle]); Masaoka et al. (2001 [triangle]). For related structures, see: Shi et al. (2007 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-0m709-scheme1.jpg

Experimental

Crystal data

  • [Pb(C8H7O2)2(H2O)]
  • M r = 495.48
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m709-efi1.jpg
  • 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 [triangle]) 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[F 2 > 2σ(F 2)] = 0.035
  • wR(F 2) = 0.061
  • S = 1.03
  • 8096 reflections
  • 397 parameters
  • H-atom parameters constrained
  • Δρmax = 0.87 e Å−3
  • Δρmin = −1.00 e Å−3

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

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

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

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

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

Acknowledgments

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

supplementary crystallographic information

Comment

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 PbII 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.

Experimental

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.

Refinement

All H atoms bounded to C atoms were positioned geometrically and allowed to ride on their parent atoms, with C—H distances in the range of 0.93–0.96 Å. The positions of the water H atoms were found from a difference Fourier map and refined with distance restraints O—H = 0.82 Å, Uiso(H) = 1.2Ueq(O).

Figures

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.

Crystal data

[Pb(C8H7O2)2(H2O)]F(000) = 1872
Mr = 495.48Dx = 2.004 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 7418 reflections
a = 7.1745 (3) Åθ = 2.4–25.2°
b = 42.745 (2) ŵ = 10.29 mm1
c = 10.7126 (5) ÅT = 296 K
β = 90.765 (1)°Block, colourless
V = 3285.0 (3) Å30.36 × 0.17 × 0.12 mm
Z = 8

Data collection

Bruker APEXII CCD area-detector diffractometer8096 independent reflections
Radiation source: fine-focus sealed tube6265 reflections with I > 2σ(I)
graphiteRint = 0.056
[var phi] and ω scansθmax = 28.2°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2007)h = −9→9
Tmin = 0.144, Tmax = 0.300k = −56→56
40611 measured reflectionsl = −14→14

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H-atom parameters constrained
wR(F2) = 0.061w = 1/[σ2(Fo2) + (0.0182P)2 + 3.7836P] where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.001
8096 reflectionsΔρmax = 0.87 e Å3
397 parametersΔρmin = −1.00 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.082

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

xyzUiso*/Ueq
Pb10.12243 (2)0.097018 (5)0.352944 (18)0.03251 (6)
Pb20.63079 (2)0.136517 (5)0.498730 (18)0.03285 (6)
O10.0014 (5)0.06035 (8)0.5043 (3)0.0425 (9)
O20.2904 (5)0.04888 (8)0.4562 (3)0.0422 (9)
O3−0.0208 (5)0.12954 (8)0.5322 (3)0.0417 (9)
O40.2740 (4)0.11793 (8)0.5341 (3)0.0382 (8)
O50.4697 (5)0.10648 (9)0.2967 (3)0.0431 (9)
O60.7648 (4)0.11863 (8)0.3157 (3)0.0361 (8)
O70.7820 (5)0.18516 (8)0.4032 (4)0.0456 (9)
O80.4875 (5)0.17631 (9)0.3567 (4)0.0532 (11)
O90.1259 (5)0.15838 (9)0.2844 (4)0.0536 (11)
H9A0.23360.16480.28560.064*
H9B0.04800.16350.33590.064*
O100.6329 (5)0.07555 (8)0.5507 (3)0.0435 (9)
H10B0.55870.06650.50430.052*
H10A0.73510.07040.52430.052*
C10.1464 (7)0.04397 (11)0.5191 (5)0.0350 (12)
C20.1449 (7)0.01859 (11)0.6140 (5)0.0327 (11)
C3−0.0085 (7)0.01413 (12)0.6892 (5)0.0419 (13)
H3A−0.11260.02680.67750.050*
C4−0.0118 (8)−0.00864 (13)0.7814 (5)0.0449 (14)
C50.1437 (9)−0.02741 (13)0.7950 (6)0.0501 (15)
H5A0.1450−0.04280.85630.060*
C60.2948 (8)−0.02395 (13)0.7213 (6)0.0483 (15)
H6A0.3966−0.03720.73190.058*
C70.2988 (8)−0.00088 (12)0.6303 (5)0.0416 (13)
H7A0.40320.00160.58070.050*
C8−0.1813 (10)−0.01275 (18)0.8623 (7)0.080 (2)
H8A−0.1591−0.02940.92100.121*
H8B−0.2874−0.01780.81070.121*
H8C−0.20500.00630.90660.121*
C90.1354 (7)0.13040 (11)0.5855 (4)0.0297 (11)
C100.1578 (7)0.14561 (12)0.7091 (5)0.0367 (12)
C110.0214 (9)0.16600 (13)0.7525 (6)0.0514 (15)
H11A−0.08210.17050.70240.062*
C120.0388 (12)0.17949 (16)0.8690 (7)0.072 (2)
C130.1933 (15)0.1719 (2)0.9412 (7)0.093 (3)
H13A0.20580.18051.02050.111*
C140.3266 (12)0.1524 (2)0.8998 (7)0.081 (2)
H14A0.42970.14810.95050.097*
C150.3122 (9)0.13865 (15)0.7832 (5)0.0563 (17)
H15A0.40400.12510.75510.068*
C16−0.1079 (14)0.2018 (2)0.9145 (9)0.131 (4)
H16A−0.07420.20910.99650.197*
H16B−0.22580.19120.91750.197*
H16C−0.11710.21930.85860.197*
C170.6265 (6)0.10896 (11)0.2509 (5)0.0296 (11)
C180.6596 (7)0.10073 (11)0.1176 (5)0.0308 (11)
C190.5301 (8)0.08355 (12)0.0511 (5)0.0425 (13)
H19A0.42040.07760.08960.051*
C200.5586 (10)0.07500 (14)−0.0711 (6)0.0558 (17)
C210.7238 (11)0.08378 (15)−0.1256 (6)0.0634 (19)
H21A0.74760.0777−0.20720.076*
C220.8544 (10)0.10140 (15)−0.0611 (6)0.0612 (18)
H22A0.96360.1076−0.09990.073*
C230.8229 (8)0.10979 (13)0.0606 (5)0.0420 (13)
H23A0.91100.12150.10450.050*
C240.4110 (11)0.05680 (17)−0.1440 (7)0.090 (3)
H24A0.45430.0528−0.22690.135*
H24B0.29800.0688−0.14830.135*
H24C0.38750.0373−0.10270.135*
C250.6358 (8)0.19171 (13)0.3421 (5)0.0413 (13)
C260.6358 (8)0.21833 (13)0.2526 (5)0.0437 (14)
C270.7935 (9)0.23678 (13)0.2416 (5)0.0500 (15)
H27A0.89800.23240.29080.060*
C280.7986 (11)0.26149 (15)0.1590 (6)0.0643 (19)
C290.6435 (15)0.26682 (19)0.0853 (7)0.091 (3)
H29A0.64460.28320.02830.109*
C300.4891 (14)0.2487 (2)0.0936 (8)0.095 (3)
H30A0.38680.25260.04170.114*
C310.4833 (10)0.22464 (17)0.1785 (7)0.069 (2)
H31A0.37580.21260.18570.083*
C320.9668 (12)0.28192 (18)0.1483 (8)0.107 (3)
H32A0.94380.29780.08650.161*
H32B1.07170.26950.12420.161*
H32C0.99280.29160.22740.161*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Pb10.02451 (10)0.04213 (12)0.03088 (11)−0.00082 (8)0.00003 (7)−0.00184 (9)
Pb20.02385 (9)0.04156 (12)0.03319 (11)0.00000 (8)0.00229 (8)−0.00581 (9)
O10.034 (2)0.042 (2)0.052 (2)0.0036 (17)0.0058 (18)0.0068 (18)
O20.0285 (19)0.049 (2)0.050 (2)−0.0036 (16)0.0087 (17)0.0043 (18)
O30.034 (2)0.053 (2)0.038 (2)0.0047 (17)−0.0067 (17)−0.0090 (18)
O40.0249 (18)0.049 (2)0.041 (2)−0.0005 (16)0.0056 (16)−0.0044 (18)
O50.0280 (19)0.059 (2)0.042 (2)−0.0028 (17)0.0080 (17)−0.0055 (19)
O60.0273 (18)0.050 (2)0.031 (2)−0.0020 (16)−0.0003 (15)−0.0068 (17)
O70.037 (2)0.042 (2)0.058 (3)−0.0016 (17)−0.0059 (19)0.0046 (19)
O80.039 (2)0.052 (2)0.068 (3)−0.0060 (19)−0.012 (2)0.005 (2)
O90.035 (2)0.069 (3)0.057 (3)−0.007 (2)0.0047 (19)0.001 (2)
O100.033 (2)0.053 (2)0.045 (2)0.0014 (17)0.0021 (17)−0.0025 (18)
C10.032 (3)0.034 (3)0.039 (3)−0.005 (2)0.000 (2)−0.004 (2)
C20.036 (3)0.030 (3)0.033 (3)−0.005 (2)−0.001 (2)−0.004 (2)
C30.034 (3)0.041 (3)0.051 (4)−0.003 (2)0.002 (3)−0.006 (3)
C40.047 (3)0.044 (3)0.044 (4)−0.010 (3)0.003 (3)0.001 (3)
C50.069 (4)0.034 (3)0.047 (4)−0.003 (3)−0.007 (3)0.005 (3)
C60.052 (4)0.038 (3)0.055 (4)0.008 (3)−0.002 (3)0.005 (3)
C70.041 (3)0.037 (3)0.047 (4)0.008 (2)0.004 (3)−0.005 (3)
C80.069 (5)0.098 (6)0.074 (5)−0.007 (4)0.018 (4)0.030 (4)
C90.028 (3)0.035 (3)0.026 (3)−0.002 (2)−0.002 (2)0.002 (2)
C100.041 (3)0.039 (3)0.031 (3)−0.007 (2)−0.004 (2)0.004 (2)
C110.064 (4)0.046 (3)0.044 (4)0.005 (3)0.003 (3)−0.008 (3)
C120.111 (6)0.056 (4)0.049 (4)−0.004 (4)0.008 (4)−0.013 (4)
C130.151 (9)0.081 (6)0.045 (5)−0.023 (6)−0.015 (5)−0.022 (4)
C140.105 (7)0.093 (6)0.044 (4)−0.022 (5)−0.029 (4)0.003 (4)
C150.058 (4)0.073 (4)0.038 (4)−0.003 (3)−0.016 (3)0.004 (3)
C160.178 (10)0.098 (7)0.119 (8)0.041 (7)0.035 (7)−0.058 (6)
C170.025 (2)0.034 (3)0.030 (3)0.002 (2)0.002 (2)0.001 (2)
C180.031 (3)0.027 (3)0.034 (3)0.004 (2)0.005 (2)0.002 (2)
C190.056 (4)0.041 (3)0.030 (3)−0.006 (3)−0.001 (3)0.001 (2)
C200.086 (5)0.044 (4)0.037 (4)−0.009 (3)−0.008 (3)−0.008 (3)
C210.106 (6)0.052 (4)0.033 (4)−0.005 (4)0.020 (4)−0.005 (3)
C220.073 (5)0.066 (4)0.046 (4)−0.005 (4)0.026 (3)0.005 (3)
C230.043 (3)0.045 (3)0.038 (3)−0.002 (3)0.003 (3)0.004 (3)
C240.139 (8)0.079 (5)0.052 (5)−0.039 (5)−0.021 (5)−0.021 (4)
C250.039 (3)0.040 (3)0.046 (4)0.000 (3)−0.002 (3)−0.005 (3)
C260.053 (4)0.038 (3)0.040 (3)0.007 (3)−0.004 (3)−0.007 (3)
C270.065 (4)0.043 (3)0.042 (4)0.007 (3)0.005 (3)0.000 (3)
C280.101 (6)0.045 (4)0.047 (4)0.013 (4)0.018 (4)0.002 (3)
C290.148 (9)0.069 (5)0.057 (5)0.025 (6)0.020 (6)0.025 (4)
C300.107 (7)0.104 (7)0.074 (6)0.021 (6)−0.022 (5)0.034 (5)
C310.064 (5)0.077 (5)0.065 (5)0.000 (4)−0.014 (4)0.011 (4)
C320.132 (8)0.070 (5)0.120 (8)−0.018 (5)0.045 (6)0.028 (5)

Geometric parameters (Å, °)

Pb1—O42.386 (3)C10—C151.387 (7)
Pb1—O12.424 (3)C10—C111.395 (7)
Pb1—O32.594 (3)C11—C121.380 (8)
Pb1—O52.603 (3)C11—H11A0.9300
Pb1—O22.622 (4)C12—C131.381 (11)
Pb1—O92.724 (4)C12—C161.505 (10)
Pb1—O6i2.751 (3)C13—C141.348 (11)
Pb2—O62.325 (3)C13—H13A0.9300
Pb2—O82.494 (4)C14—C151.384 (9)
Pb2—O3ii2.538 (3)C14—H14A0.9300
Pb2—O72.565 (4)C15—H15A0.9300
Pb2—O102.665 (3)C16—H16A0.9600
Pb2—O42.712 (3)C16—H16B0.9600
Pb2—O52.757 (4)C16—H16C0.9600
O1—C11.263 (6)C17—C181.493 (7)
O2—C11.258 (6)C18—C191.376 (7)
O3—C91.251 (5)C18—C231.384 (7)
O3—Pb2i2.538 (3)C19—C201.377 (8)
O4—C91.261 (5)C19—H19A0.9300
O5—C171.238 (5)C20—C211.380 (9)
O6—C171.273 (5)C20—C241.521 (8)
O6—Pb1ii2.751 (3)C21—C221.381 (9)
O7—C251.261 (6)C21—H21A0.9300
O8—C251.263 (6)C22—C231.373 (8)
O9—H9A0.8200C22—H22A0.9300
O9—H9B0.8200C23—H23A0.9300
O10—H10B0.8200C24—H24A0.9600
O10—H10A0.8200C24—H24B0.9600
C1—C21.487 (7)C24—H24C0.9600
C2—C31.386 (7)C25—C261.488 (8)
C2—C71.392 (7)C26—C311.370 (8)
C3—C41.387 (7)C26—C271.386 (8)
C3—H3A0.9300C27—C281.378 (8)
C4—C51.380 (8)C27—H27A0.9300
C4—C81.513 (8)C28—C291.375 (11)
C5—C61.358 (8)C28—C321.495 (10)
C5—H5A0.9300C29—C301.355 (11)
C6—C71.388 (7)C29—H29A0.9300
C6—H6A0.9300C30—C311.375 (10)
C7—H7A0.9300C30—H30A0.9300
C8—H8A0.9600C31—H31A0.9300
C8—H8B0.9600C32—H32A0.9600
C8—H8C0.9600C32—H32B0.9600
C9—C101.482 (7)C32—H32C0.9600
O4—Pb1—O182.05 (12)C4—C8—H8B109.5
O4—Pb1—O351.51 (11)H8A—C8—H8B109.5
O1—Pb1—O372.68 (12)C4—C8—H8C109.5
O4—Pb1—O572.72 (11)H8A—C8—H8C109.5
O1—Pb1—O5127.44 (12)H8B—C8—H8C109.5
O3—Pb1—O5118.56 (11)O3—C9—O4119.7 (5)
O4—Pb1—O275.46 (12)O3—C9—C10120.4 (4)
O1—Pb1—O251.48 (11)O4—C9—C10119.9 (4)
O3—Pb1—O2107.02 (11)C15—C10—C11120.2 (5)
O5—Pb1—O277.50 (11)C15—C10—C9119.5 (5)
O4—Pb1—O981.54 (12)C11—C10—C9120.2 (5)
O1—Pb1—O9143.85 (12)C12—C11—C10120.5 (6)
O3—Pb1—O971.86 (12)C12—C11—H11A119.8
O5—Pb1—O977.05 (11)C10—C11—H11A119.8
O2—Pb1—O9149.74 (11)C11—C12—C13118.1 (7)
O4—Pb1—O6i113.97 (10)C11—C12—C16120.2 (8)
O1—Pb1—O6i88.41 (11)C13—C12—C16121.8 (7)
O3—Pb1—O6i63.23 (10)C14—C13—C12121.9 (7)
O5—Pb1—O6i143.91 (11)C14—C13—H13A119.0
O2—Pb1—O6i138.35 (10)C12—C13—H13A119.0
O9—Pb1—O6i69.48 (10)C13—C14—C15121.0 (7)
O6—Pb2—O883.21 (13)C13—C14—H14A119.5
O6—Pb2—O3ii70.29 (11)C15—C14—H14A119.5
O8—Pb2—O3ii124.28 (12)C14—C15—C10118.4 (7)
O6—Pb2—O775.42 (12)C14—C15—H15A120.8
O8—Pb2—O751.46 (12)C10—C15—H15A120.8
O3ii—Pb2—O774.37 (12)C12—C16—H16A109.5
O6—Pb2—O1081.57 (11)C12—C16—H16B109.5
O8—Pb2—O10142.70 (12)H16A—C16—H16B109.5
O3ii—Pb2—O1081.54 (11)C12—C16—H16C109.5
O7—Pb2—O10151.05 (11)H16A—C16—H16C109.5
O6—Pb2—O4115.06 (11)H16B—C16—H16C109.5
O8—Pb2—O484.44 (12)O5—C17—O6121.2 (5)
O3ii—Pb2—O4151.11 (11)O5—C17—C18121.1 (4)
O7—Pb2—O4134.31 (11)O6—C17—C18117.7 (4)
O10—Pb2—O471.75 (10)C19—C18—C23119.4 (5)
O6—Pb2—O550.10 (10)C19—C18—C17120.4 (5)
O8—Pb2—O570.96 (12)C23—C18—C17120.2 (5)
O3ii—Pb2—O5117.25 (10)C18—C19—C20121.8 (6)
O7—Pb2—O5103.86 (11)C18—C19—H19A119.1
O10—Pb2—O573.13 (11)C20—C19—H19A119.1
O4—Pb2—O565.60 (10)C19—C20—C21118.0 (6)
C1—O1—Pb198.1 (3)C19—C20—C24120.8 (6)
C1—O2—Pb188.9 (3)C21—C20—C24121.2 (6)
C9—O3—Pb2i159.3 (3)C20—C21—C22121.2 (6)
C9—O3—Pb189.5 (3)C20—C21—H21A119.4
Pb2i—O3—Pb1110.94 (12)C22—C21—H21A119.4
C9—O4—Pb199.2 (3)C23—C22—C21119.9 (6)
C9—O4—Pb2133.5 (3)C23—C22—H22A120.1
Pb1—O4—Pb2114.63 (13)C21—C22—H22A120.1
C17—O5—Pb1169.4 (3)C22—C23—C18119.8 (6)
C17—O5—Pb284.1 (3)C22—C23—H23A120.1
Pb1—O5—Pb2106.44 (12)C18—C23—H23A120.1
C17—O6—Pb2103.8 (3)C20—C24—H24A109.5
C17—O6—Pb1ii133.6 (3)C20—C24—H24B109.5
Pb2—O6—Pb1ii112.57 (13)H24A—C24—H24B109.5
C25—O7—Pb291.9 (3)C20—C24—H24C109.5
C25—O8—Pb295.2 (3)H24A—C24—H24C109.5
Pb1—O9—H9A109.2H24B—C24—H24C109.5
Pb1—O9—H9B93.9O7—C25—O8121.1 (5)
H9A—O9—H9B123.4O7—C25—C26119.8 (5)
Pb2—O10—H10B109.3O8—C25—C26119.1 (5)
Pb2—O10—H10A101.0C31—C26—C27119.0 (6)
H10B—O10—H10A103.9C31—C26—C25121.1 (6)
O2—C1—O1121.4 (5)C27—C26—C25119.8 (5)
O2—C1—C2120.1 (5)C28—C27—C26121.3 (6)
O1—C1—C2118.5 (5)C28—C27—H27A119.4
C3—C2—C7118.7 (5)C26—C27—H27A119.4
C3—C2—C1120.7 (5)C29—C28—C27117.9 (7)
C7—C2—C1120.6 (5)C29—C28—C32120.4 (7)
C2—C3—C4122.1 (5)C27—C28—C32121.7 (7)
C2—C3—H3A118.9C30—C29—C28121.5 (7)
C4—C3—H3A118.9C30—C29—H29A119.2
C5—C4—C3117.5 (5)C28—C29—H29A119.2
C5—C4—C8121.8 (6)C29—C30—C31120.2 (8)
C3—C4—C8120.7 (5)C29—C30—H30A119.9
C6—C5—C4121.7 (6)C31—C30—H30A119.9
C6—C5—H5A119.1C26—C31—C30120.0 (7)
C4—C5—H5A119.1C26—C31—H31A120.0
C5—C6—C7120.7 (5)C30—C31—H31A120.0
C5—C6—H6A119.6C28—C32—H32A109.5
C7—C6—H6A119.6C28—C32—H32B109.5
C6—C7—C2119.3 (5)H32A—C32—H32B109.5
C6—C7—H7A120.4C28—C32—H32C109.5
C2—C7—H7A120.4H32A—C32—H32C109.5
C4—C8—H8A109.5H32B—C32—H32C109.5

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

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O9—H9A···O80.822.032.805 (5)158
O9—H9B···O7i0.822.253.017 (5)156
O10—H10B···O20.822.122.881 (5)153
O10—H10A···O1ii0.821.972.774 (5)166

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FJ2218).

References

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