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Acta Crystallogr Sect E Struct Rep Online. 2009 August 1; 65(Pt 8): m989.
Published online 2009 July 25. doi:  10.1107/S1600536809028542
PMCID: PMC2977498

Poly[μ-aqua-di-μ-benzoato-lead(II)]

Abstract

The reaction of lead(II) nitrate and benzoic acid in aqueous solution yields the title polymer, [Pb(C7H5O2)2(H2O)]n. The asymmetric unit contains one PbII ion, two benzoate ligands and one water mol­ecule. The Pb—O bond distances are in the range 2.494 (4)–2.735 (4) Å. The Pb(...)Pb distance is 4.0683 (4) Å, indicating an insignificant metal–metal inter­action. The PbII atom has a distorted penta­gonal-bipyramidal geometry chelated by two carboxyl­ate O atoms. The Pb atoms are bridged through a coordinating water mol­ecule and two carboxyl­ate O atoms from another two benzoate ligands, giving an infinite three-dimensional supra­molecular structure. O—H(...)O hydrogen-bonding inter­actions involved the coordinating water and carboxyl­ate O atoms enhance the stability of the supra­molecular arrangement.

Related literature

For general background to lead(II) compounds, see: Shi et al. (2007 [triangle]); Fan & Zhu (2006 [triangle]); Wang et al. (2006 [triangle]); Kim 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-65-0m989-scheme1.jpg

Experimental

Crystal data

  • [Pb(C7H5O2)2(H2O)]
  • M r = 467.43
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m989-efi1.jpg
  • a = 15.4118 (12) Å
  • b = 7.5122 (6) Å
  • c = 11.4856 (9) Å
  • β = 91.2930 (10)°
  • V = 1329.42 (18) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 12.71 mm−1
  • T = 295 K
  • 0.40 × 0.10 × 0.08 mm

Data collection

  • Bruker APEXII CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2007 [triangle]) T min = 0.1, T max = 0.247 (expected range = 0.146–0.362)
  • 13406 measured reflections
  • 2664 independent reflections
  • 2315 reflections with I > 2σ(I)
  • R int = 0.057

Refinement

  • R[F 2 > 2σ(F 2)] = 0.034
  • wR(F 2) = 0.087
  • S = 1.09
  • 2664 reflections
  • 181 parameters
  • H-atom parameters constrained
  • Δρmax = 3.35 e Å−3
  • Δρmin = −1.31 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/S1600536809028542/fj2238sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809028542/fj2238Isup2.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

Lead(II) compounds have been increasingly studied (Shi et al. 2007; Fan et al. 2006) 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; Kim et al. 2001). Herein, we report the structure of the title complex.

The asymmetric unit of the title complex, [Pb(C7H5O2)2(H2O)]n, contains a PbII cation, two BA ligands and one water molecule, as illustrated in Fig. 1. The PbII atom is heptacoordinated and chelated by two carboxylate O atoms. The Pb atoms are bridged through a coordinating water and two carboxylate O atoms from another two BA ligands. The Pb—O bond lengths are in the range of 2.494 (4) to 2.735 (4) Å. The inter-distance of Pb···Pb is 4.0683 (4) Å, indicating the weak metal-metal interaction. The PbII atom has a distorted pentagonal bipyramidal geometry and the complexes extend infinitely to three-dimensional supramolecular structure. The coordinating water molecule and carboxylate O atoms are involved in extensive O—H···O hydrogen-bonding interactions (Table 2).

Experimental

A mixture of Pb(NO3)2 3H2O (0.172 g, 0.52 mmol), BA (0.102 g, 0.84 mmol), melamine (0.026 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 403 K for 6 days to give the colorless stick 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 of 0.93 Å. The positions of the water H atoms were found from a difference Fourier map and refined with distance restraints O—H = 0.85 Å, Uiso(H) = 1.5Ueq(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 three-dimensional structure of the title compound.

Crystal data

[Pb(C7H5O2)2(H2O)]F(000) = 872
Mr = 467.43Dx = 2.335 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4827 reflections
a = 15.4118 (12) Åθ = 2.6–28.5°
b = 7.5122 (6) ŵ = 12.71 mm1
c = 11.4856 (9) ÅT = 295 K
β = 91.293 (1)°Block, colorless
V = 1329.42 (18) Å30.4 × 0.1 × 0.08 mm
Z = 4

Data collection

Bruker APEXII CCD area-detector diffractometer2664 independent reflections
Radiation source: fine-focus sealed tube2315 reflections with I > 2σ(I)
graphiteRint = 0.057
[var phi] and ω scansθmax = 26.2°, θmin = 3.2°
Absorption correction: multi-scan (SADABS; Bruker, 2007)h = −19→18
Tmin = 0.1, Tmax = 0.247k = −9→9
13406 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)] = 0.034H-atom parameters constrained
wR(F2) = 0.087w = 1/[σ2(Fo2) + (0.047P)2] where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max < 0.001
2664 reflectionsΔρmax = 3.35 e Å3
181 parametersΔρmin = −1.31 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008)
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.082

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

xyzUiso*/Ueq
Pb10.478855 (16)0.52214 (3)0.311202 (19)0.02834 (12)
O10.6082 (3)0.3213 (6)0.3120 (4)0.0390 (11)
O20.5947 (4)0.4879 (5)0.4674 (4)0.0401 (12)
O30.5875 (3)0.6929 (5)0.1986 (4)0.0372 (11)
O40.6356 (4)0.5476 (7)0.0428 (4)0.0453 (13)
O50.4960 (3)0.3455 (6)0.1048 (3)0.0349 (10)
H5A0.45620.36480.05390.052*
H5B0.53740.38650.06510.052*
C10.6397 (4)0.3861 (8)0.4045 (5)0.0310 (14)
C20.7318 (4)0.3531 (8)0.4365 (5)0.0286 (13)
C30.7840 (5)0.2548 (9)0.3639 (5)0.0370 (15)
H3A0.75960.19940.29860.044*
C40.8716 (5)0.2383 (10)0.3876 (6)0.0469 (18)
H4A0.90620.17320.33780.056*
C50.9082 (5)0.3177 (10)0.4847 (6)0.0495 (19)
H5C0.96750.30820.49960.059*
C60.8567 (5)0.4114 (10)0.5599 (6)0.0470 (18)
H6A0.88100.46240.62680.056*
C70.7695 (5)0.4291 (9)0.5356 (6)0.0405 (16)
H7A0.73510.49300.58630.049*
C80.6480 (4)0.6270 (8)0.1387 (5)0.0309 (14)
C90.7395 (4)0.6483 (7)0.1816 (5)0.0270 (13)
C100.8062 (4)0.5691 (9)0.1224 (5)0.0346 (14)
H10A0.79380.50330.05540.042*
C110.8914 (5)0.5869 (11)0.1619 (6)0.0462 (17)
H11A0.93610.53590.12030.055*
C120.9098 (5)0.6794 (11)0.2623 (6)0.0503 (19)
H12A0.96680.68960.28980.060*
C130.8433 (5)0.7573 (10)0.3222 (6)0.050 (2)
H13A0.85600.82090.38990.060*
C140.7587 (5)0.7427 (9)0.2838 (6)0.0408 (17)
H14A0.71440.79520.32540.049*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Pb10.02962 (19)0.02363 (16)0.03171 (17)0.00173 (9)−0.00073 (11)0.00129 (8)
O10.030 (3)0.042 (3)0.044 (3)0.001 (2)−0.010 (2)−0.004 (2)
O20.039 (3)0.041 (3)0.041 (3)0.015 (2)0.005 (2)0.0009 (19)
O30.036 (3)0.027 (2)0.049 (3)0.0032 (19)0.011 (2)0.0011 (19)
O40.037 (3)0.056 (3)0.043 (3)−0.001 (2)−0.004 (2)−0.006 (2)
O50.043 (3)0.033 (2)0.028 (2)−0.005 (2)−0.0034 (19)0.0054 (17)
C10.035 (4)0.030 (3)0.028 (3)−0.003 (3)−0.001 (3)0.009 (2)
C20.027 (4)0.026 (3)0.032 (3)0.004 (2)−0.002 (3)0.003 (2)
C30.039 (4)0.041 (4)0.031 (3)0.001 (3)−0.005 (3)−0.003 (3)
C40.037 (5)0.053 (5)0.051 (4)0.005 (3)0.008 (3)0.003 (3)
C50.034 (4)0.057 (5)0.057 (5)−0.003 (4)−0.006 (4)0.012 (4)
C60.052 (5)0.045 (4)0.044 (4)−0.006 (4)−0.011 (4)−0.002 (3)
C70.048 (5)0.038 (4)0.035 (4)0.005 (3)−0.010 (3)−0.008 (3)
C80.037 (4)0.021 (3)0.035 (3)0.002 (3)0.001 (3)0.006 (2)
C90.031 (4)0.022 (3)0.028 (3)−0.006 (2)0.000 (2)0.006 (2)
C100.029 (4)0.041 (4)0.034 (3)−0.003 (3)0.002 (3)−0.003 (3)
C110.033 (4)0.055 (5)0.051 (4)0.003 (4)0.006 (3)−0.004 (4)
C120.039 (5)0.060 (5)0.052 (4)−0.004 (4)−0.012 (4)0.002 (4)
C130.057 (6)0.053 (5)0.039 (4)−0.008 (4)−0.012 (4)−0.007 (3)
C140.048 (5)0.033 (4)0.041 (4)−0.004 (3)0.008 (3)−0.005 (3)

Geometric parameters (Å, °)

Pb1—O32.494 (4)C4—C51.374 (10)
Pb1—O12.499 (4)C4—H4A0.9300
Pb1—O22.515 (5)C5—C61.379 (10)
Pb1—O5i2.639 (4)C5—H5C0.9300
Pb1—O3ii2.677 (4)C6—C71.374 (10)
Pb1—O52.735 (4)C6—H6A0.9300
Pb1—C12.867 (6)C7—H7A0.9300
O1—C11.256 (7)C8—C91.493 (8)
O2—C11.269 (8)C9—C101.379 (9)
O3—C81.271 (7)C9—C141.397 (8)
O3—Pb1i2.677 (4)C10—C111.386 (10)
O4—C81.264 (7)C10—H10A0.9300
O5—Pb1ii2.639 (4)C11—C121.370 (10)
O5—H5A0.8500C11—H11A0.9300
O5—H5B0.8500C12—C131.378 (10)
C1—C21.479 (8)C12—H12A0.9300
C2—C31.385 (8)C13—C141.371 (10)
C2—C71.389 (8)C13—H13A0.9300
C3—C41.377 (10)C14—H14A0.9300
C3—H3A0.9300
O3—Pb1—O176.58 (15)C3—C2—C1120.5 (5)
O3—Pb1—O287.06 (16)C7—C2—C1121.1 (6)
O1—Pb1—O251.87 (14)C4—C3—C2120.6 (6)
O3—Pb1—O5i67.76 (13)C4—C3—H3A119.7
O1—Pb1—O5i116.34 (14)C2—C3—H3A119.7
O2—Pb1—O5i74.78 (13)C5—C4—C3120.2 (7)
O3—Pb1—O3ii135.53 (10)C5—C4—H4A119.9
O1—Pb1—O3ii75.30 (14)C3—C4—H4A119.9
O2—Pb1—O3ii101.51 (14)C4—C5—C6119.9 (7)
O5i—Pb1—O3ii156.67 (12)C4—C5—H5C120.0
O3—Pb1—O573.78 (13)C6—C5—H5C120.0
O1—Pb1—O567.52 (13)C7—C6—C5119.7 (7)
O2—Pb1—O5119.18 (14)C7—C6—H6A120.1
O5i—Pb1—O5138.36 (11)C5—C6—H6A120.1
O3ii—Pb1—O563.89 (12)C6—C7—C2121.1 (7)
O3—Pb1—C178.02 (15)C6—C7—H7A119.5
O1—Pb1—C125.93 (15)C2—C7—H7A119.5
O2—Pb1—C126.25 (15)O4—C8—O3123.8 (6)
O5i—Pb1—C194.18 (15)O4—C8—C9117.5 (6)
O3ii—Pb1—C190.71 (16)O3—C8—C9118.7 (5)
O5—Pb1—C192.94 (15)C10—C9—C14119.2 (6)
C1—O1—Pb193.6 (4)C10—C9—C8120.0 (5)
C1—O2—Pb192.5 (4)C14—C9—C8120.8 (6)
C8—O3—Pb1126.1 (4)C9—C10—C11120.5 (6)
C8—O3—Pb1i128.4 (4)C9—C10—H10A119.8
Pb1—O3—Pb1i103.70 (15)C11—C10—H10A119.8
Pb1ii—O5—Pb198.38 (12)C12—C11—C10120.1 (7)
Pb1ii—O5—H5A120.4C12—C11—H11A119.9
Pb1—O5—H5A115.5C10—C11—H11A119.9
Pb1ii—O5—H5B115.0C11—C12—C13119.5 (7)
Pb1—O5—H5B112.2C11—C12—H12A120.3
H5A—O5—H5B96.3C13—C12—H12A120.3
O1—C1—O2120.6 (6)C14—C13—C12121.2 (7)
O1—C1—C2119.7 (6)C14—C13—H13A119.4
O2—C1—C2119.5 (6)C12—C13—H13A119.4
O1—C1—Pb160.5 (3)C13—C14—C9119.5 (7)
O2—C1—Pb161.2 (4)C13—C14—H14A120.3
C2—C1—Pb1165.8 (4)C9—C14—H14A120.3
C3—C2—C7118.3 (6)

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

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O5—H5A···O4iii0.851.902.734 (7)168
O5—H5B···O40.851.962.740 (7)152

Symmetry codes: (iii) −x+1, −y+1, −z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FJ2238).

References

  • Bruker (2007). APEX2, SAINT and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Fan, S. R. & Zhu, L. G. (2006). Inorg. Chem.45, 7935–7942. [PubMed]
  • Kim, J., Chen, B., Reneke, T. M., Li, H., Eddaoudi, M., Moler, D. B., O’Keeffe, M. & Yaghi, O. M. (2001). J. Am. Chem. Soc.123, 8239–8247. [PubMed]
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • 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.
  • Wang, X. L., Qin, C. & Wang, E. B. (2006). Cryst. Growth. Des.6, 439–443.

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