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

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ISSN: 2056-9890

(2,2′-Bi­pyridine-κ2N,N′)bis­­(4-hy­droxy­benzoato-κ2O,O′)lead(II) monohydrate

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 27 December 2009; accepted 24 January 2010; online 30 January 2010)

The reaction of lead acetate, 4-hydroxy­benzoic acid and 2,2′-bipyridine in aqueous solution gave the title complex, [Pb(C7H5O3)2(C10H8N2)]·H2O. The asymmetric unit contains one PbII atom, two 4-hydroxy­benzoate ligands, one 2,2′-bipyridine ligand and one uncoordinated water mol­ecule. The PbII atom is hexa­coordinated in a distorted tetra­gonal-bipyramidal geometry and is chelated by four carboxyl­ate O atoms and two N atoms. O—H⋯O hydrogen-bonding inter­actions, involving the uncoordinated water, the carboxyl­ate O atoms and hydr­oxy O atoms, produce a three-dimensional supra­molecular structure.

Related literature

For general background to the potential applications of lead compounds, see: Fan & Zhu (2006[Fan, S. R. & Zhu, L. G. (2006). Inorg. Chem. 45, 7935-7942.]); Hamilton et al. (2004[Hamilton, B. H., Kelley, K. A., Wagler, T. A., Espe, M. P. & Ziegler, C. J. (2004). Inorg. Chem. 43, 50-56.]); 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.]). For the use of aromatic carboxyl­ate ligands in the preparation of metal-organic complexes, see: Wang et al. (2006[Wang, X. L., Qin, C. & Wang, E. B. (2006). Cryst. Growth Des. 6, 439-443.]); Masaoka et al. (2001[Masaoka, S., Furukawa, S., Chang, H. C., Mizutani, T. & Kitagawa, S. (2001). Angew. Chem. Int. Ed. 40, 3817-3819.]). For related lead 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(C7H5O3)2(C10H8N2)]·H2O

  • Mr = 655.61

  • Monoclinic, P 21 /c

  • a = 10.9483 (4) Å

  • b = 17.5194 (6) Å

  • c = 12.0479 (4) Å

  • β = 100.334 (2)°

  • V = 2273.39 (14) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 7.47 mm−1

  • T = 296 K

  • 0.35 × 0.26 × 0.21 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 = 0.180, Tmax = 0.303

  • 18618 measured reflections

  • 4067 independent reflections

  • 3579 reflections with I > σ(I)

  • Rint = 0.037

Refinement
  • R[F2 > 2σ(F2)] = 0.025

  • wR(F2) = 0.072

  • S = 1.01

  • 4067 reflections

  • 315 parameters

  • 3 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 1.05 e Å−3

  • Δρmin = −0.61 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O6—H6A⋯O1i 0.82 1.90 2.671 (4) 157
O3—H3A⋯O1W 0.82 1.89 2.695 (5) 166
O1W—H1A⋯O5ii 0.90 (3) 2.04 (3) 2.849 (4) 148 (5)
O1W—H1B⋯O4iii 0.83 (3) 2.00 (3) 2.789 (4) 158 (5)
Symmetry codes: (i) [-x, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (ii) -x+1, -y+1, -z; (iii) [-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}].

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


Comment top

Recently, lead compounds have been increasingly studied owing to their possible applications in different fields (Fan & Zhu 2006; Hamilton et al. 2004; Shi et al. 2007), such as ion-exchange, non-linear optics and catalysis. Environmental and biological concerns are due to the toxicity of lead and its diverse interactions with biological systems. 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, [Pb(C24H18O6N2)(H2O)], contains a PbII cation, two 4-hydroxybenzonic acid ligands, one 2,2'-bipyridine and one free water molecule, as illustrated in Fig. 1. The PbII atom is hexacoordinate and chelated by four carboxylate O atoms from two 4-hydroxybenzoic acid and two N atoms from one 2,2'-bipyridine. The Pb—O bond lengths are in the range of 2.477 (3) to 2.625 (3) Å. The Pb—N bond lengths are 2.463 (3) to 2.562 (3) Å. The PbII atom has a distorted tetragonal bipyramidal geometry. The free water molecule, carboxylate O atoms and hydroxy O atoms are involved in extensive O—H···O hydrogen-bonding interactions (Table 1).

Related literature top

For general background to the potential applications of lead compounds, see: Fan & Zhu (2006); Hamilton et al. (2004); Shi et al. (2007). For the use of aromatic carboxylate ligands in the preparation of metal-organic complexes, see: Wang et al. (2006); Masaoka et al. (2001). For related lead structures, see: Shi et al. (2007).

Experimental top

A mixture of Pb(CH3COO)2 3H2O (0.199 g, 0.52 mmol), 4-hydroxybenzoic acid (0.116 g, 0.84 mmol), 2,2'-bipyridine (0.033 g, 0.21 mmol) and distilled water (10 ml) was sealed in a 25 ml Teflon-lined stainless autoclave. The mixture was heated at 403 K for 5 days to give colorless crystals suitable for X-ray diffraction analysis.

Refinement top

All H atoms bonded to C atoms and the hydroxy H atoms were placed in calculated positions (C—H = 0.93 Å, O—H = 0.82 Å) and were included in the refinement in the riding model approximation, with Uiso(H) = 1.2Ueq(C) or Uiso(H) = 1.5Ueq(O). The positions of the water H atoms were found in a difference Fourier map and refined with distance restraints O—H = 0.83 Å, Uiso(H) = 1.5Ueq(O).

Structure description top

Recently, lead compounds have been increasingly studied owing to their possible applications in different fields (Fan & Zhu 2006; Hamilton et al. 2004; Shi et al. 2007), such as ion-exchange, non-linear optics and catalysis. Environmental and biological concerns are due to the toxicity of lead and its diverse interactions with biological systems. 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, [Pb(C24H18O6N2)(H2O)], contains a PbII cation, two 4-hydroxybenzonic acid ligands, one 2,2'-bipyridine and one free water molecule, as illustrated in Fig. 1. The PbII atom is hexacoordinate and chelated by four carboxylate O atoms from two 4-hydroxybenzoic acid and two N atoms from one 2,2'-bipyridine. The Pb—O bond lengths are in the range of 2.477 (3) to 2.625 (3) Å. The Pb—N bond lengths are 2.463 (3) to 2.562 (3) Å. The PbII atom has a distorted tetragonal bipyramidal geometry. The free water molecule, carboxylate O atoms and hydroxy O atoms are involved in extensive O—H···O hydrogen-bonding interactions (Table 1).

For general background to the potential applications of lead compounds, see: Fan & Zhu (2006); Hamilton et al. (2004); Shi et al. (2007). For the use of aromatic carboxylate ligands in the preparation of metal-organic complexes, see: Wang et al. (2006); Masaoka et al. (2001). For related lead structures, see: Shi et al. (2007).

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 PbII in the title complex with the atom-labeling scheme. Displacement ellipsoids for non-hydrogen atoms are drawn at the 30% probability level.
(2,2'-Bipyridine-κ2N,N')bis(4-hydroxybenzoato- κ2O,O')lead(II) monohydrate top
Crystal data top
[Pb(C7H5O3)2(C10H8N2)]·H2OF(000) = 1264
Mr = 655.61Dx = 1.915 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9368 reflections
a = 10.9483 (4) Åθ = 2.2–26.9°
b = 17.5194 (6) ŵ = 7.47 mm1
c = 12.0479 (4) ÅT = 296 K
β = 100.334 (2)°Block, colorless
V = 2273.39 (14) Å30.35 × 0.26 × 0.21 mm
Z = 4
Data collection top
Bruker APEXII CCD area-detector
diffractometer
4067 independent reflections
Radiation source: fine-focus sealed tube3579 reflections with I > σ(I)
Graphite monochromatorRint = 0.037
φ and ω scansθmax = 25.1°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Bruker, 2007)
h = 1313
Tmin = 0.180, Tmax = 0.303k = 1920
18618 measured reflectionsl = 1414
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.072H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.0468P)2 + 0.280P]
where P = (Fo2 + 2Fc2)/3
4067 reflections(Δ/σ)max = 0.001
315 parametersΔρmax = 1.05 e Å3
3 restraintsΔρmin = 0.61 e Å3
Crystal data top
[Pb(C7H5O3)2(C10H8N2)]·H2OV = 2273.39 (14) Å3
Mr = 655.61Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.9483 (4) ŵ = 7.47 mm1
b = 17.5194 (6) ÅT = 296 K
c = 12.0479 (4) Å0.35 × 0.26 × 0.21 mm
β = 100.334 (2)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer
4067 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2007)
3579 reflections with I > σ(I)
Tmin = 0.180, Tmax = 0.303Rint = 0.037
18618 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0253 restraints
wR(F2) = 0.072H atoms treated by a mixture of independent and constrained refinement
S = 1.01Δρmax = 1.05 e Å3
4067 reflectionsΔρmin = 0.61 e Å3
315 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.261796 (15)0.580074 (8)0.261115 (12)0.03852 (9)
O50.0806 (3)0.64137 (15)0.1348 (2)0.0475 (7)
C70.4017 (5)0.4162 (2)0.0512 (4)0.0420 (11)
H70.34230.45050.08630.050*
C200.1550 (3)0.4657 (2)0.4545 (3)0.0320 (8)
O20.2797 (3)0.50785 (17)0.0880 (2)0.0483 (7)
N20.2459 (3)0.51668 (19)0.4497 (3)0.0404 (8)
O10.3906 (3)0.45881 (15)0.2420 (2)0.0432 (7)
C190.0708 (4)0.4488 (2)0.3465 (3)0.0315 (8)
C90.0879 (4)0.7114 (2)0.1842 (3)0.0356 (9)
C20.4263 (4)0.4108 (2)0.0654 (4)0.0375 (9)
N10.0957 (3)0.48437 (18)0.2536 (2)0.0380 (8)
O60.3930 (3)0.85265 (16)0.0985 (2)0.0482 (7)
H6A0.40580.87670.15360.072*
C210.1424 (5)0.4314 (2)0.5547 (4)0.0408 (10)
H210.07750.39760.55750.049*
C10.3605 (4)0.4621 (2)0.1352 (3)0.0409 (10)
C130.2517 (4)0.7641 (2)0.0452 (3)0.0419 (10)
H130.29140.76790.02960.050*
C140.1501 (4)0.7182 (2)0.0728 (3)0.0393 (9)
H140.12170.69090.01630.047*
C30.5150 (4)0.3590 (2)0.1156 (3)0.0462 (10)
H30.53180.35430.19370.055*
C100.1360 (4)0.7505 (2)0.2682 (3)0.0420 (10)
H100.09860.74520.34350.050*
C120.2965 (4)0.8055 (2)0.1294 (3)0.0376 (9)
O40.0747 (3)0.65607 (16)0.3160 (2)0.0503 (8)
C180.0272 (4)0.3996 (2)0.3390 (4)0.0424 (10)
H180.04290.37520.40350.051*
C50.5550 (4)0.3211 (2)0.0643 (3)0.0399 (9)
C160.0779 (5)0.4215 (2)0.1430 (4)0.0555 (13)
H160.12750.41320.07290.067*
O30.6169 (3)0.2796 (2)0.1324 (2)0.0587 (8)
H3A0.67780.25940.09400.088*
C170.1021 (4)0.3859 (2)0.2378 (4)0.0504 (11)
H170.16910.35270.23320.061*
C40.5782 (4)0.3146 (2)0.0512 (3)0.0461 (10)
H40.63710.27980.08590.055*
C80.0289 (4)0.6673 (2)0.2142 (3)0.0389 (9)
C150.0219 (5)0.4700 (2)0.1548 (3)0.0521 (12)
H150.03930.49410.09070.063*
C60.4647 (4)0.3710 (2)0.1153 (3)0.0466 (10)
H60.44620.37400.19360.056*
C110.2373 (4)0.7962 (3)0.2403 (3)0.0447 (11)
H110.26770.82190.29710.054*
C240.3265 (4)0.5317 (2)0.5439 (3)0.0517 (11)
H240.39010.56620.54000.062*
C220.2272 (5)0.4478 (2)0.6510 (3)0.0499 (11)
H220.22080.42420.71880.060*
C230.3208 (4)0.4987 (3)0.6463 (3)0.0545 (12)
H230.37860.51070.71040.065*
O1W0.8383 (3)0.23234 (19)0.0179 (3)0.0588 (8)
H1A0.885 (5)0.273 (2)0.030 (4)0.088*
H1B0.867 (5)0.222 (3)0.049 (3)0.088*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.03782 (13)0.03792 (13)0.04067 (12)0.00251 (6)0.00932 (8)0.00471 (6)
O50.0479 (19)0.0526 (17)0.0440 (15)0.0115 (14)0.0139 (14)0.0043 (13)
C70.034 (3)0.048 (3)0.044 (2)0.0059 (18)0.005 (2)0.0071 (17)
C200.025 (2)0.036 (2)0.0352 (19)0.0043 (16)0.0062 (17)0.0005 (15)
O20.0394 (18)0.0588 (18)0.0450 (15)0.0114 (15)0.0032 (14)0.0044 (13)
N20.035 (2)0.0451 (19)0.0393 (17)0.0048 (16)0.0027 (16)0.0004 (14)
O10.0461 (19)0.0453 (17)0.0382 (15)0.0017 (14)0.0077 (13)0.0033 (12)
C190.031 (2)0.0262 (18)0.038 (2)0.0034 (16)0.0068 (17)0.0005 (15)
C90.042 (2)0.031 (2)0.0369 (19)0.0055 (17)0.0141 (19)0.0000 (15)
C20.037 (3)0.037 (2)0.039 (2)0.0053 (17)0.0064 (19)0.0038 (15)
N10.039 (2)0.0410 (19)0.0329 (16)0.0028 (15)0.0029 (15)0.0047 (13)
O60.0435 (19)0.0505 (17)0.0480 (16)0.0107 (14)0.0009 (14)0.0065 (13)
C210.042 (3)0.041 (2)0.039 (2)0.0018 (19)0.007 (2)0.0018 (17)
C10.035 (3)0.043 (2)0.045 (2)0.008 (2)0.008 (2)0.0026 (18)
C130.045 (3)0.044 (2)0.037 (2)0.004 (2)0.0056 (19)0.0038 (17)
C140.045 (3)0.037 (2)0.037 (2)0.0042 (19)0.0129 (19)0.0047 (16)
C30.050 (3)0.047 (2)0.040 (2)0.002 (2)0.006 (2)0.0025 (18)
C100.053 (3)0.045 (2)0.0287 (18)0.006 (2)0.0087 (19)0.0018 (16)
C120.037 (2)0.033 (2)0.043 (2)0.0050 (18)0.0082 (19)0.0024 (16)
O40.059 (2)0.0521 (17)0.0410 (16)0.0137 (15)0.0124 (15)0.0015 (13)
C180.039 (3)0.040 (2)0.047 (2)0.0064 (19)0.006 (2)0.0003 (18)
C50.031 (2)0.051 (2)0.0372 (19)0.0068 (19)0.0069 (18)0.0010 (17)
C160.060 (4)0.056 (3)0.044 (3)0.010 (2)0.008 (2)0.0073 (19)
O30.055 (2)0.076 (2)0.0473 (16)0.0091 (17)0.0158 (16)0.0009 (16)
C170.046 (3)0.047 (3)0.056 (3)0.010 (2)0.001 (2)0.004 (2)
C40.041 (3)0.046 (2)0.050 (2)0.009 (2)0.006 (2)0.0039 (19)
C80.051 (3)0.036 (2)0.0320 (19)0.0002 (19)0.013 (2)0.0014 (15)
C150.065 (3)0.054 (3)0.034 (2)0.014 (2)0.001 (2)0.0032 (18)
C60.042 (3)0.059 (3)0.039 (2)0.006 (2)0.009 (2)0.0073 (19)
C110.049 (3)0.047 (3)0.043 (2)0.006 (2)0.019 (2)0.0029 (17)
C240.041 (3)0.060 (3)0.051 (2)0.010 (2)0.003 (2)0.000 (2)
C220.060 (3)0.055 (3)0.033 (2)0.001 (2)0.003 (2)0.0090 (19)
C230.047 (3)0.068 (3)0.040 (2)0.002 (2)0.013 (2)0.001 (2)
O1W0.060 (2)0.060 (2)0.0592 (19)0.0064 (17)0.0169 (18)0.0124 (16)
Geometric parameters (Å, º) top
Pb1—N12.463 (3)C13—H130.9300
Pb1—O22.477 (3)C14—H140.9300
Pb1—O52.514 (3)C3—C41.370 (6)
Pb1—N22.563 (3)C3—H30.9300
Pb1—O12.583 (3)C10—C111.359 (6)
Pb1—O42.625 (3)C10—H100.9300
O5—C81.279 (4)C12—C111.386 (5)
C7—C61.374 (6)O4—C81.254 (4)
C7—C21.385 (6)C18—C171.363 (6)
C7—H70.9300C18—H180.9300
C20—N21.346 (5)C5—O31.364 (5)
C20—C211.378 (5)C5—C41.374 (5)
C20—C191.484 (5)C5—C61.379 (6)
O2—C11.252 (5)C16—C171.368 (6)
N2—C241.332 (5)C16—C151.371 (6)
O1—C11.271 (5)C16—H160.9300
C19—N11.351 (5)O3—H3A0.8200
C19—C181.366 (6)C17—H170.9300
C9—C141.397 (5)C4—H40.9300
C9—C101.402 (5)C15—H150.9300
C9—C81.482 (6)C6—H60.9300
C2—C31.387 (6)C11—H110.9300
C2—C11.501 (6)C24—C231.374 (6)
N1—C151.337 (5)C24—H240.9300
O6—C121.341 (5)C22—C231.368 (6)
O6—H6A0.8200C22—H220.9300
C21—C221.379 (6)C23—H230.9300
C21—H210.9300O1W—H1A0.90 (3)
C13—C141.364 (6)O1W—H1B0.83 (3)
C13—C121.405 (5)
N1—Pb1—O277.93 (10)C13—C14—H14119.3
N1—Pb1—O576.79 (10)C9—C14—H14119.3
O2—Pb1—O583.20 (9)C4—C3—C2120.7 (4)
N1—Pb1—N264.57 (10)C4—C3—H3119.7
O2—Pb1—N2123.60 (11)C2—C3—H3119.7
O5—Pb1—N2123.38 (10)C11—C10—C9120.3 (4)
N1—Pb1—O181.27 (11)C11—C10—H10119.9
O2—Pb1—O151.53 (9)C9—C10—H10119.9
O5—Pb1—O1132.96 (8)O6—C12—C11123.3 (3)
N2—Pb1—O181.23 (9)O6—C12—C13118.6 (3)
N1—Pb1—O475.54 (10)C11—C12—C13118.2 (4)
O2—Pb1—O4130.87 (9)C8—O4—Pb191.5 (2)
O5—Pb1—O450.89 (8)C17—C18—C19120.6 (4)
N2—Pb1—O479.42 (10)C17—C18—H18119.7
O1—Pb1—O4154.53 (9)C19—C18—H18119.7
C8—O5—Pb196.1 (2)O3—C5—C4122.9 (4)
C6—C7—C2120.3 (4)O3—C5—C6117.6 (3)
C6—C7—H7119.9C4—C5—C6119.5 (4)
C2—C7—H7119.9C17—C16—C15117.7 (4)
N2—C20—C21121.2 (4)C17—C16—H16121.1
N2—C20—C19116.3 (3)C15—C16—H16121.1
C21—C20—C19122.5 (4)C5—O3—H3A109.5
C1—O2—Pb195.8 (2)C18—C17—C16119.4 (4)
C24—N2—C20118.4 (3)C18—C17—H17120.3
C24—N2—Pb1122.0 (3)C16—C17—H17120.3
C20—N2—Pb1119.6 (2)C3—C4—C5120.3 (4)
C1—O1—Pb190.4 (2)C3—C4—H4119.8
N1—C19—C18120.6 (4)C5—C4—H4119.8
N1—C19—C20116.6 (3)O4—C8—O5121.5 (4)
C18—C19—C20122.7 (3)O4—C8—C9119.8 (3)
C14—C9—C10118.1 (4)O5—C8—C9118.7 (3)
C14—C9—C8122.0 (3)N1—C15—C16123.6 (4)
C10—C9—C8119.9 (3)N1—C15—H15118.2
C7—C2—C3118.7 (4)C16—C15—H15118.2
C7—C2—C1120.2 (4)C7—C6—C5120.5 (4)
C3—C2—C1121.1 (4)C7—C6—H6119.8
C15—N1—C19118.1 (3)C5—C6—H6119.8
C15—N1—Pb1119.0 (3)C10—C11—C12121.8 (4)
C19—N1—Pb1122.8 (2)C10—C11—H11119.1
C12—O6—H6A109.5C12—C11—H11119.1
C20—C21—C22119.2 (4)N2—C24—C23123.5 (4)
C20—C21—H21120.4N2—C24—H24118.2
C22—C21—H21120.4C23—C24—H24118.2
O2—C1—O1121.6 (4)C23—C22—C21119.9 (4)
O2—C1—C2119.9 (4)C23—C22—H22120.1
O1—C1—C2118.5 (4)C21—C22—H22120.1
C14—C13—C12120.2 (4)C22—C23—C24117.8 (4)
C14—C13—H13119.9C22—C23—H23121.1
C12—C13—H13119.9C24—C23—H23121.1
C13—C14—C9121.3 (4)H1A—O1W—H1B102 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H6A···O1i0.821.902.671 (4)157
O3—H3A···O1W0.821.892.695 (5)166
O1W—H1A···O5ii0.90 (3)2.04 (3)2.849 (4)148 (5)
O1W—H1B···O4iii0.83 (3)2.00 (3)2.789 (4)158 (5)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x+1, y+1, z; (iii) x+1, y1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Pb(C7H5O3)2(C10H8N2)]·H2O
Mr655.61
Crystal system, space groupMonoclinic, P21/c
Temperature (K)296
a, b, c (Å)10.9483 (4), 17.5194 (6), 12.0479 (4)
β (°) 100.334 (2)
V3)2273.39 (14)
Z4
Radiation typeMo Kα
µ (mm1)7.47
Crystal size (mm)0.35 × 0.26 × 0.21
Data collection
DiffractometerBruker APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Bruker, 2007)
Tmin, Tmax0.180, 0.303
No. of measured, independent and
observed [I > σ(I)] reflections
18618, 4067, 3579
Rint0.037
(sin θ/λ)max1)0.598
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.025, 0.072, 1.01
No. of reflections4067
No. of parameters315
No. of restraints3
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.05, 0.61

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

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H6A···O1i0.821.902.671 (4)156.8
O3—H3A···O1W0.821.892.695 (5)166.4
O1W—H1A···O5ii0.90 (3)2.04 (3)2.849 (4)148 (5)
O1W—H1B···O4iii0.83 (3)2.00 (3)2.789 (4)158 (5)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x+1, y+1, z; (iii) x+1, y1/2, z+1/2.
 

Acknowledgements

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

References

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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

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