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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 65| Part 8| August 2009| Page m989
doi:10.1107/S1600536809028542

Poly[μ-aqua-di-μ-benzoato-lead(II)]

Jiantong Lia and Juan Yanga*

aDepartment of Physical Chemistry, Henan Polytechnic University, Jiaozuo 454003, People's Republic of China
*Correspondence e-mail: yangjuan0302@yahoo.cn

(Received 11 July 2009; accepted 20 July 2009; online 25 July 2009)

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[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.]); Fan & Zhu (2006[Fan, S. R. & Zhu, L. G. (2006). Inorg. Chem. 45, 7935-7942.]); Wang et al. (2006[Wang, X. L., Qin, C. & Wang, E. B. (2006). Cryst. Growth. Des. 6, 439-443.]); Kim et al. (2001[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.]). For related structures, see: Shi et al. (2007[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.]).

[Scheme 1]

Experimental

Crystal data

  • [Pb(C7H5O2)2(H2O)]

  • Mr = 467.43

  • Monoclinic, P 21 /c

  • 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[Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.1, Tmax = 0.247 (expected range = 0.146–0.362)

  • 13406 measured reflections

  • 2664 independent reflections

  • 2315 reflections with I > 2σ(I)

  • Rint = 0.057
Refinement

  • R[F2 > 2σ(F2)] = 0.034

  • wR(F2) = 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

Table 1
Selected bond lengths (Å)

Pb1—O3 2.494 (4)
Pb1—O1 2.499 (4)
Pb1—O2 2.515 (5)
Pb1—O5i 2.639 (4)
Pb1—O3ii 2.677 (4)
Pb1—O5 2.735 (4)
Pb1—C1ii 2.867 (6)
Symmetry codes: (i) [-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (ii) [-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}].

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O5—H5A⋯O4iii 0.85 1.90 2.734 (7) 168
O5—H5B⋯O4 0.85 1.96 2.740 (7) 152
Symmetry code: (iii) -x+1, -y+1, -z.

Data collection: APEX2 (Bruker, 2007[Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2007[Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809028542/fj2238sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809028542/fj2238Isup2.hkl

checkCIF report


Comment top

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).

Related literature top

For general background to lead(II) compounds, see: Shi et al. (2007); Fan et al. (2006); Wang et al. (2006); Kim et al. (2001). For related structures, see: Shi et al. (2007).

Experimental top

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 top

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).

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
[Figure 1] 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.
[Figure 2] Fig. 2. The three-dimensional structure of the title compound.
Poly[µ-aqua-di-µ-benzoato-lead(II)] top
Crystal data top
[Pb(C7H5O2)2(H2O)]F(000) = 872
Mr = 467.43Dx = 2.335 Mg m−3
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 mm−1
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 top
Bruker APEXII CCD area-detector
diffractometer		2664 independent reflections
Radiation source: fine-focus sealed tube2315 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.057
ϕ 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 top
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) = 0.087 w = 1/[σ2(Fo2) + (0.047P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max < 0.001
2664 reflectionsΔρmax = 3.35 e Å−3
181 parametersΔρmin = −1.31 e Å−3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008)
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.082
Crystal data top
[Pb(C7H5O2)2(H2O)]V = 1329.42 (18) Å3
Mr = 467.43Z = 4
Monoclinic, P21/cMo Kα radiation
a = 15.4118 (12) ŵ = 12.71 mm−1
b = 7.5122 (6) ÅT = 295 K
c = 11.4856 (9) Å0.4 × 0.1 × 0.08 mm
β = 91.293 (1)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer		2664 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2007)		2315 reflections with I > 2σ(I)
Tmin = 0.1, Tmax = 0.247Rint = 0.057
13406 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.087H-atom parameters constrained
S = 1.09Δρmax = 3.35 e Å−3
2664 reflectionsΔρmin = −1.31 e Å−3
181 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
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) top
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, º) top
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, º) top
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 code: (iii) −x+1, −y+1, −z.

Experimental details

Crystal data
Chemical formula[Pb(C7H5O2)2(H2O)]
Mr467.43
Crystal system, space groupMonoclinic, P21/c
Temperature (K)295
a, b, c (Å)15.4118 (12), 7.5122 (6), 11.4856 (9)
β (°) 91.293 (1)
V (Å3)1329.42 (18)
Z4
Radiation typeMo Kα
µ (mm−1)12.71
Crystal size (mm)0.4 × 0.1 × 0.08
Data collection
DiffractometerBruker APEXII CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2007)
Tmin, Tmax0.1, 0.247
No. of measured, independent and
observed [I > 2σ(I)] reflections		13406, 2664, 2315
Rint0.057
(sin θ/λ)max (Å−1)0.621
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.087, 1.09
No. of reflections2664
No. of parameters181
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)3.35, −1.31

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

Selected bond lengths (Å) top
Pb1—O32.494 (4)Pb1—O3ii2.677 (4)
Pb1—O12.499 (4)Pb1—O52.735 (4)
Pb1—O22.515 (5)O3—Pb1i2.677 (4)
Pb1—O5i2.639 (4)O5—Pb1ii2.639 (4)
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x+1, y−1/2, −z+1/2.
Hydrogen-bond geometry (Å, º) top
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 code: (iii) −x+1, −y+1, −z.
 

Acknowledgements

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

References

First citationBruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationFan, S. R. & Zhu, L. G. (2006). Inorg. Chem. 45, 7935–7942.  Web of Science CSD CrossRef PubMed CAS Google Scholar
 First citationKim, 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.  Web of Science CSD CrossRef PubMed CAS Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationShi, 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
 First citationWang, 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.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 65| Part 8| August 2009| Page m989
doi:10.1107/S1600536809028542
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