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 3| March 2009| Pages m275-m276

Penta­aqua­bis­[4-(2-hy­droxy­benzyl­­idene­amino)benzene­sulfonato]lead(II)

aDepartment of Chemistry and Chemical Engineering, Weifang University, Weifang 261061, People's Republic of China
*Correspondence e-mail: taixishi@lzu.edu.cn

(Received 4 February 2009; accepted 8 February 2009; online 13 February 2009)

In the structure of the title compound, [Pb(C13H10NO4S)2(H2O)5], two S—O bonds and one C—N bond have lengths of 1.421 (9), 1.425 (8) and 1.268 (11) Å, respectively, which suggests they are double bonds. Mol­ecules form a two-dimensional layered structure via O—H⋯O and O—H⋯N inter­actions. The Pb atom adopts distorted cubo-octahedral coordination.

Related literature

For our previous work on the coordination chemistry of aroylhydrazones, see: Tai et al. (2003[Tai, X.-S., Yin, X.-H., Tan, M.-Y. & Li, Y.-Z. (2003). Acta Cryst. E59, o681-o682.], 2008[Tai, X.-S., Feng, Y.-M. & Kong, F.-Y. (2008). Acta Cryst. E64, o750.]); Tai, Yin & Feng (2007[Tai, X. S., Yin, J. & Feng, Y. M. (2007). Z. Kristallogr. New Cryst. Struct. 222, 343-344.]); Tai, Yin & Kong (2007[Tai, X. S., Yin, J. & Kong, F. Y. (2007). Z. Kristallogr. New Cryst. Struct. 222, 401-402.]); Xi-Shi & Yi-Min (2008[Xi-Shi, T. & Yi-Min, F. (2008). Acta Cryst. E64, o707.]).

[Scheme 1]

Experimental

Crystal data
  • [Pb(C13H10NO4S)2(H2O)5]

  • Mr = 849.83

  • Monoclinic, P 21 /c

  • a = 35.618 (4) Å

  • b = 7.3407 (10) Å

  • c = 11.6218 (18) Å

  • β = 99.146 (2)°

  • V = 3000.0 (7) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 5.83 mm−1

  • T = 298 K

  • 0.50 × 0.40 × 0.38 mm

Data collection
  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.159, Tmax = 0.215 (expected range = 0.080–0.109)

  • 14411 measured reflections

  • 5264 independent reflections

  • 4635 reflections with I > 2σ(I)

  • Rint = 0.045

Refinement
  • R[F2 > 2σ(F2)] = 0.051

  • wR(F2) = 0.129

  • S = 1.09

  • 5264 reflections

  • 397 parameters

  • H-atom parameters constrained

  • Δρmax = 1.95 e Å−3

  • Δρmin = −4.10 e Å−3

Table 1
Selected geometric parameters (Å, °)

Pb1—O9 2.523 (7)
Pb1—O5 2.531 (6)
Pb1—O10 2.534 (7)
Pb1—O11 2.576 (7)
Pb1—O12 2.702 (7)
Pb1—O13 2.713 (8)
Pb1—O1 2.761 (8)
Pb1—O2 2.882 (8)
S1—O1—Pb1 102.3 (4)
S1—O2—Pb1 97.8 (4)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O4—H4⋯N1 0.82 1.90 2.626 (9) 147
O4—H4⋯O4i 0.82 2.59 2.897 (9) 104
O8—H8⋯N2 0.82 1.88 2.611 (10) 147
O8—H8⋯O8ii 0.82 2.60 2.933 (9) 106
O9—H9A⋯O6 0.85 2.04 2.781 (11) 146
O9—H9B⋯O5iii 0.85 2.17 2.911 (9) 146
O10—H10A⋯O6iv 0.85 2.12 2.914 (9) 156
O10—H10B⋯O7iii 0.85 1.94 2.771 (9) 167
O11—H11A⋯O3v 0.85 2.07 2.883 (11) 162
O11—H11B⋯O7iv 0.85 2.06 2.772 (9) 141
O12—H12A⋯O3v 0.85 2.03 2.841 (13) 159
O12—H12B⋯O2vi 0.85 2.08 2.922 (11) 170
O13—H13A⋯O2vi 0.85 2.54 3.287 (13) 148
O13—H13B⋯O1vii 0.85 2.23 2.867 (11) 132
C6—H6⋯O1 0.93 2.52 2.898 (10) 104
C15—H15⋯O6 0.93 2.52 2.907 (10) 105
Symmetry codes: (i) -x+1, -y+1, -z+2; (ii) -x, -y+2, -z+2; (iii) [x, -y+{\script{1\over 2}}, z-{\script{3\over 2}}]; (iv) x, y-1, z; (v) [x, -y-{\script{1\over 2}}, z-{\script{1\over 2}}]; (vi) [x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]; (vii) x, y+1, z.

Data collection: SMART (Bruker, 2000[Bruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2000[Bruker (2000). SMART, 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

As part of our ongoing studies of the coordination chemistry of aroylhydrazones ligands (Tai et al., 2003, 2008; Xi-Shi & Yi-Min, 2008; Tai, Yin & Feng, 2007; Tai, Yin & Kong, 2007), we now report the synthesis and structure of the title compound, (I), (Fig. 1).

In the molecule of (I), both C7—N1 [1.268 (11) Å], S1—O2 [1.421 (9) Å] and S1—O3 [1.425 (8) Å] are close to double-bond separations, indicating that the Lewis structure shown in the scheme is only an approximation to the electron distribution in the molecule. Otherwise, the geometrical parameters for (I) are normal (Table 1). The molecules form a two-dimensional layered structure by the O—H···O and O—H···N interactions (Table 2).

Related literature top

For our previous work on the coordination chemistry of aroylhydrazones, see: Tai et al. (2003, 2008); Tai, Yin & Feng (2007); Tai, Yin & Kong (2007); Xi-Shi & Yi-Min (2008).

Experimental top

The solution of 1.0 mmol 4-(2-hydroxybenzylideneamino)benzene sulfonic acid and 1.0 mmol NaOH in 5 ml 95% ethanol was added to a solution of 0.5 mmol Pb(CH3COO)2.4H2O in 5 ml ethanol at room temperature. The mixture was refluxed for 4 h with stirring, then the resulting precipitate was filtered, washed, and dried in vacuo over P4O10 for 48 h. Single crystals suitable for X-ray structural analysis was obtained by slowly evaporating from methanol at room temperature, which afforded colourless crystals.

Refinement top

The H atoms were placed geometrically [C—H = 0.93 Å, O—H = 0.82 and 0.85 Å] and refined as riding with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(hydroxy and water O).

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); 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 molecular structure of (I) showing 50% displacement ellipsoids.
Pentaaquabis[4-(2-hydroxybenzylideneamino)benzenesulfonato]lead(II) top
Crystal data top
[Pb(C13H10NO4S)2(H2O)5]F(000) = 1672
Mr = 849.83Dx = 1.882 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7854 reflections
a = 35.618 (4) Åθ = 2.3–28.2°
b = 7.3407 (10) ŵ = 5.83 mm1
c = 11.6218 (18) ÅT = 298 K
β = 99.146 (2)°Block, colourless
V = 3000.0 (7) Å30.50 × 0.40 × 0.38 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
5264 independent reflections
Radiation source: fine-focus sealed tube4635 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.045
ϕ and ω scansθmax = 25.0°, θmin = 2.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 3842
Tmin = 0.159, Tmax = 0.215k = 88
14411 measured reflectionsl = 1213
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)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.129H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0518P)2 + 32.8197P]
where P = (Fo2 + 2Fc2)/3
5264 reflections(Δ/σ)max = 0.001
397 parametersΔρmax = 1.95 e Å3
0 restraintsΔρmin = 4.10 e Å3
Crystal data top
[Pb(C13H10NO4S)2(H2O)5]V = 3000.0 (7) Å3
Mr = 849.83Z = 4
Monoclinic, P21/cMo Kα radiation
a = 35.618 (4) ŵ = 5.83 mm1
b = 7.3407 (10) ÅT = 298 K
c = 11.6218 (18) Å0.50 × 0.40 × 0.38 mm
β = 99.146 (2)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
5264 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
4635 reflections with I > 2σ(I)
Tmin = 0.159, Tmax = 0.215Rint = 0.045
14411 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0510 restraints
wR(F2) = 0.129H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0518P)2 + 32.8197P]
where P = (Fo2 + 2Fc2)/3
5264 reflectionsΔρmax = 1.95 e Å3
397 parametersΔρmin = 4.10 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.254090 (10)0.60871 (5)0.70033 (3)0.02876 (13)
N10.4786 (2)0.3808 (10)0.7656 (6)0.0272 (17)
N20.0183 (2)0.8703 (10)0.7901 (6)0.0300 (18)
O10.29367 (18)0.3019 (11)0.6522 (7)0.0485 (19)
O20.3039 (2)0.5492 (12)0.5314 (8)0.059 (2)
O30.3111 (2)0.2452 (14)0.4657 (8)0.071 (3)
O40.53202 (17)0.4584 (10)0.9417 (5)0.0378 (16)
H40.51030.44810.90620.057*
O50.20067 (17)0.7699 (8)0.7789 (5)0.0307 (14)
O60.18530 (18)1.0295 (9)0.6507 (5)0.0316 (14)
O70.19465 (18)1.0692 (9)0.8588 (6)0.0359 (15)
O80.03384 (18)0.9558 (10)0.9153 (5)0.0377 (16)
H80.01230.93620.90130.057*
O90.2255 (3)0.7960 (11)0.5263 (6)0.063 (2)
H9A0.20620.85620.53970.076*
H9B0.21940.73070.46580.076*
O100.2010 (2)0.4078 (9)0.5991 (5)0.0408 (17)
H10A0.20250.30120.62800.049*
H10B0.20160.40100.52640.049*
O110.2377 (2)0.3831 (9)0.8548 (6)0.0445 (18)
H11A0.25710.32150.88370.053*
H11B0.22020.31060.82530.053*
O120.3084 (2)0.6237 (10)0.8910 (6)0.052 (2)
H12A0.30890.52570.93020.062*
H12B0.30460.71290.93440.062*
O130.2833 (2)0.9472 (11)0.7455 (8)0.058 (2)
H13A0.28180.98430.81390.069*
H13B0.27401.02550.69510.069*
S10.31440 (6)0.3667 (3)0.56240 (19)0.0272 (5)
S20.18201 (6)0.9476 (3)0.76156 (17)0.0231 (4)
C10.3629 (2)0.3685 (11)0.6230 (7)0.0237 (18)
C20.3894 (3)0.4201 (13)0.5545 (7)0.028 (2)
H20.38120.45210.47710.034*
C30.4275 (2)0.4250 (13)0.5985 (7)0.030 (2)
H30.44510.46160.55180.036*
C40.4396 (2)0.3745 (12)0.7138 (8)0.0269 (19)
C50.4133 (2)0.3274 (13)0.7839 (7)0.0269 (19)
H50.42150.29990.86200.032*
C60.3745 (2)0.3204 (13)0.7387 (7)0.030 (2)
H60.35690.28430.78520.036*
C70.5050 (3)0.3422 (13)0.7080 (8)0.029 (2)
H70.49830.30240.63150.035*
C80.5449 (2)0.3570 (12)0.7553 (7)0.0233 (18)
C90.5573 (2)0.4157 (12)0.8698 (7)0.0258 (19)
C100.5957 (2)0.4223 (13)0.9124 (7)0.029 (2)
H100.60390.45940.98880.035*
C110.6218 (3)0.3746 (13)0.8431 (9)0.035 (2)
H110.64760.38200.87250.042*
C120.6104 (3)0.3158 (14)0.7307 (8)0.034 (2)
H120.62840.28370.68450.041*
C130.5724 (3)0.3050 (12)0.6873 (8)0.029 (2)
H130.56470.26260.61180.035*
C140.1336 (2)0.9073 (11)0.7639 (7)0.0232 (18)
C150.1065 (2)0.9479 (12)0.6678 (7)0.0259 (19)
H150.11430.98610.59890.031*
C160.0686 (3)0.9325 (13)0.6734 (8)0.029 (2)
H160.05070.96220.60880.035*
C170.0565 (2)0.8722 (11)0.7757 (7)0.0233 (18)
C180.0838 (2)0.8274 (13)0.8711 (7)0.0268 (19)
H180.07610.78550.93920.032*
C190.1220 (2)0.8443 (13)0.8661 (7)0.0263 (19)
H190.14000.81390.93030.032*
C200.0091 (3)0.8373 (12)0.7066 (8)0.0279 (19)
H200.00290.79850.63580.034*
C210.0482 (2)0.8562 (12)0.7154 (7)0.0249 (19)
C220.0593 (3)0.9194 (12)0.8203 (7)0.0264 (19)
C230.0983 (3)0.9433 (13)0.8238 (8)0.031 (2)
H230.10620.98600.89150.037*
C240.1247 (3)0.9040 (13)0.7285 (9)0.035 (2)
H240.15030.92070.73270.042*
C250.1145 (3)0.8408 (14)0.6267 (9)0.037 (2)
H250.13300.81450.56280.045*
C260.0766 (3)0.8169 (13)0.6208 (8)0.032 (2)
H260.06950.77360.55210.039*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.0247 (2)0.0297 (2)0.03319 (19)0.00055 (15)0.00855 (13)0.00043 (15)
N10.024 (4)0.032 (5)0.024 (3)0.000 (3)0.000 (3)0.001 (3)
N20.020 (4)0.033 (5)0.038 (4)0.001 (3)0.008 (3)0.002 (3)
O10.020 (3)0.059 (5)0.068 (5)0.004 (3)0.010 (3)0.007 (4)
O20.023 (4)0.064 (6)0.087 (6)0.011 (4)0.003 (4)0.022 (5)
O30.022 (4)0.099 (7)0.086 (6)0.004 (4)0.006 (4)0.060 (6)
O40.018 (3)0.064 (5)0.031 (3)0.004 (3)0.003 (3)0.007 (3)
O50.027 (3)0.026 (3)0.042 (3)0.006 (3)0.014 (3)0.008 (3)
O60.033 (4)0.029 (4)0.035 (3)0.000 (3)0.014 (3)0.010 (3)
O70.030 (4)0.036 (4)0.043 (4)0.004 (3)0.010 (3)0.004 (3)
O80.024 (3)0.060 (5)0.030 (3)0.005 (3)0.008 (3)0.008 (3)
O90.106 (7)0.050 (5)0.033 (4)0.023 (5)0.010 (4)0.002 (4)
O100.053 (5)0.037 (4)0.029 (3)0.008 (3)0.004 (3)0.005 (3)
O110.043 (4)0.038 (4)0.049 (4)0.008 (3)0.002 (3)0.012 (3)
O120.061 (5)0.046 (5)0.044 (4)0.009 (4)0.005 (4)0.003 (3)
O130.054 (5)0.040 (5)0.076 (5)0.012 (4)0.001 (4)0.003 (4)
S10.0165 (10)0.0292 (13)0.0351 (11)0.0024 (9)0.0015 (9)0.0059 (9)
S20.0201 (10)0.0231 (11)0.0276 (10)0.0001 (9)0.0078 (8)0.0026 (9)
C10.021 (4)0.020 (5)0.030 (4)0.001 (4)0.005 (3)0.007 (4)
C20.028 (5)0.034 (5)0.021 (4)0.003 (4)0.000 (4)0.003 (4)
C30.019 (4)0.040 (6)0.031 (5)0.002 (4)0.005 (4)0.006 (4)
C40.021 (4)0.024 (5)0.034 (5)0.004 (4)0.001 (4)0.003 (4)
C50.020 (4)0.037 (5)0.024 (4)0.006 (4)0.002 (3)0.001 (4)
C60.022 (5)0.036 (5)0.032 (5)0.002 (4)0.008 (4)0.009 (4)
C70.029 (5)0.028 (5)0.029 (4)0.001 (4)0.002 (4)0.001 (4)
C80.019 (4)0.021 (5)0.029 (4)0.003 (4)0.001 (3)0.002 (3)
C90.021 (4)0.029 (5)0.028 (4)0.000 (4)0.008 (4)0.004 (4)
C100.024 (5)0.038 (6)0.026 (4)0.004 (4)0.003 (4)0.000 (4)
C110.022 (5)0.032 (6)0.051 (6)0.000 (4)0.002 (4)0.009 (4)
C120.022 (5)0.040 (6)0.044 (5)0.006 (4)0.013 (4)0.001 (5)
C130.033 (5)0.024 (5)0.032 (5)0.006 (4)0.008 (4)0.002 (4)
C140.023 (4)0.019 (4)0.030 (4)0.003 (4)0.011 (3)0.002 (3)
C150.026 (5)0.029 (5)0.024 (4)0.004 (4)0.007 (3)0.005 (4)
C160.025 (5)0.031 (5)0.030 (4)0.004 (4)0.005 (4)0.002 (4)
C170.017 (4)0.018 (5)0.037 (5)0.003 (3)0.011 (4)0.002 (4)
C180.025 (5)0.031 (5)0.026 (4)0.004 (4)0.008 (4)0.004 (4)
C190.025 (5)0.031 (5)0.022 (4)0.005 (4)0.003 (3)0.004 (4)
C200.031 (5)0.024 (5)0.030 (4)0.003 (4)0.010 (4)0.000 (4)
C210.022 (4)0.021 (5)0.032 (4)0.001 (4)0.007 (4)0.004 (4)
C220.030 (5)0.020 (5)0.029 (4)0.006 (4)0.006 (4)0.001 (4)
C230.025 (5)0.036 (5)0.035 (5)0.000 (4)0.013 (4)0.000 (4)
C240.027 (5)0.030 (5)0.050 (6)0.006 (4)0.012 (4)0.006 (4)
C250.036 (6)0.033 (6)0.042 (5)0.019 (5)0.005 (4)0.003 (4)
C260.040 (6)0.030 (5)0.028 (4)0.004 (5)0.008 (4)0.001 (4)
Geometric parameters (Å, º) top
Pb1—O92.523 (7)C3—H30.9300
Pb1—O52.531 (6)C4—C51.378 (12)
Pb1—O102.534 (7)C5—C61.400 (12)
Pb1—O112.576 (7)C5—H50.9300
Pb1—O122.702 (7)C6—H60.9300
Pb1—O132.713 (8)C7—C81.443 (12)
Pb1—O12.761 (8)C7—H70.9300
Pb1—O22.882 (8)C8—C91.402 (12)
N1—C71.268 (11)C8—C131.407 (12)
N1—C41.426 (11)C9—C101.380 (12)
N2—C201.284 (12)C10—C111.369 (13)
N2—C171.398 (11)C10—H100.9300
O1—S11.452 (7)C11—C121.373 (14)
O2—S11.421 (9)C11—H110.9300
O3—S11.425 (8)C12—C131.370 (13)
O4—C91.358 (10)C12—H120.9300
O4—H40.8200C13—H130.9300
O5—S21.463 (6)C14—C151.386 (12)
O6—S21.443 (6)C14—C191.397 (12)
O7—S21.454 (7)C15—C161.369 (12)
O8—C221.340 (10)C15—H150.9300
O8—H80.8200C16—C171.399 (12)
O9—H9A0.8501C16—H160.9300
O9—H9B0.8500C17—C181.392 (12)
O10—H10A0.8500C18—C191.377 (12)
O10—H10B0.8500C18—H180.9300
O11—H11A0.8500C19—H190.9300
O11—H11B0.8501C20—C211.422 (12)
O12—H12A0.8500C20—H200.9300
O12—H12B0.8500C21—C261.399 (12)
O13—H13A0.8500C21—C221.418 (12)
O13—H13B0.8500C22—C231.407 (12)
S1—C11.759 (9)C23—C241.364 (13)
S2—C141.754 (9)C23—H230.9300
C1—C21.379 (12)C24—C251.372 (14)
C1—C61.388 (12)C24—H240.9300
C2—C31.376 (12)C25—C261.376 (14)
C2—H20.9300C25—H250.9300
C3—C41.391 (12)C26—H260.9300
O9—Pb1—O578.7 (2)C4—C3—H3120.5
O9—Pb1—O1076.6 (3)C5—C4—C3120.2 (8)
O5—Pb1—O1083.8 (2)C5—C4—N1117.8 (8)
O9—Pb1—O11143.3 (3)C3—C4—N1121.9 (8)
O5—Pb1—O1177.4 (2)C4—C5—C6120.6 (8)
O10—Pb1—O1173.4 (2)C4—C5—H5119.7
O9—Pb1—O12141.3 (3)C6—C5—H5119.7
O5—Pb1—O1299.5 (2)C1—C6—C5118.6 (8)
O10—Pb1—O12142.0 (2)C1—C6—H6120.7
O11—Pb1—O1270.5 (2)C5—C6—H6120.7
O9—Pb1—O1375.5 (3)N1—C7—C8123.3 (8)
O5—Pb1—O1377.9 (2)N1—C7—H7118.4
O10—Pb1—O13149.1 (2)C8—C7—H7118.4
O11—Pb1—O13125.2 (2)C9—C8—C13118.2 (8)
O12—Pb1—O1366.5 (2)C9—C8—C7121.8 (8)
O9—Pb1—O1115.9 (2)C13—C8—C7119.9 (8)
O5—Pb1—O1153.1 (2)O4—C9—C10119.1 (8)
O10—Pb1—O178.4 (2)O4—C9—C8121.0 (8)
O11—Pb1—O178.2 (2)C10—C9—C8119.8 (8)
O12—Pb1—O183.0 (2)C11—C10—C9120.4 (8)
O13—Pb1—O1126.4 (2)C11—C10—H10119.8
O9—Pb1—O275.6 (2)C9—C10—H10119.8
O5—Pb1—O2153.7 (2)C10—C11—C12121.0 (9)
O10—Pb1—O295.2 (2)C10—C11—H11119.5
O11—Pb1—O2127.6 (2)C12—C11—H11119.5
O12—Pb1—O297.3 (2)C13—C12—C11119.5 (9)
O13—Pb1—O290.7 (3)C13—C12—H12120.2
O1—Pb1—O249.4 (2)C11—C12—H12120.2
C7—N1—C4121.6 (7)C12—C13—C8121.0 (8)
C20—N2—C17123.3 (8)C12—C13—H13119.5
S1—O1—Pb1102.3 (4)C8—C13—H13119.5
S1—O2—Pb197.8 (4)C15—C14—C19119.6 (8)
C9—O4—H4109.5C15—C14—S2120.7 (6)
S2—O5—Pb1135.9 (3)C19—C14—S2119.5 (7)
C22—O8—H8109.5C16—C15—C14120.7 (8)
Pb1—O9—H9A111.8C16—C15—H15119.7
Pb1—O9—H9B111.9C14—C15—H15119.7
H9A—O9—H9B109.8C15—C16—C17120.3 (8)
Pb1—O10—H10A111.0C15—C16—H16119.8
Pb1—O10—H10B111.2C17—C16—H16119.8
H10A—O10—H10B109.2C18—C17—N2118.2 (7)
Pb1—O11—H11A110.9C18—C17—C16118.8 (8)
Pb1—O11—H11B110.8N2—C17—C16122.7 (8)
H11A—O11—H11B109.0C19—C18—C17121.0 (8)
Pb1—O12—H12A110.9C19—C18—H18119.5
Pb1—O12—H12B110.9C17—C18—H18119.5
H12A—O12—H12B109.0C18—C19—C14119.5 (8)
Pb1—O13—H13A113.2C18—C19—H19120.2
Pb1—O13—H13B113.0C14—C19—H19120.2
H13A—O13—H13B110.6N2—C20—C21124.2 (8)
O2—S1—O3113.8 (6)N2—C20—H20117.9
O2—S1—O1110.4 (5)C21—C20—H20117.9
O3—S1—O1112.0 (5)C26—C21—C22118.6 (8)
O2—S1—C1107.2 (4)C26—C21—C20121.1 (8)
O3—S1—C1105.9 (4)C22—C21—C20120.3 (8)
O1—S1—C1107.1 (4)O8—C22—C23119.6 (8)
O6—S2—O7112.3 (4)O8—C22—C21121.9 (8)
O6—S2—O5113.3 (4)C23—C22—C21118.5 (8)
O7—S2—O5111.2 (4)C24—C23—C22120.4 (8)
O6—S2—C14107.7 (4)C24—C23—H23119.8
O7—S2—C14106.0 (4)C22—C23—H23119.8
O5—S2—C14105.9 (4)C23—C24—C25122.0 (9)
C2—C1—C6120.2 (8)C23—C24—H24119.0
C2—C1—S1119.2 (7)C25—C24—H24119.0
C6—C1—S1120.5 (7)C24—C25—C26118.8 (9)
C3—C2—C1121.2 (8)C24—C25—H25120.6
C3—C2—H2119.4C26—C25—H25120.6
C1—C2—H2119.4C25—C26—C21121.7 (9)
C2—C3—C4119.1 (8)C25—C26—H26119.1
C2—C3—H3120.5C21—C26—H26119.1
O9—Pb1—O1—S141.2 (5)C4—C5—C6—C12.4 (14)
O5—Pb1—O1—S1159.5 (3)C4—N1—C7—C8176.4 (8)
O10—Pb1—O1—S1110.0 (4)N1—C7—C8—C90.1 (14)
O11—Pb1—O1—S1174.8 (4)N1—C7—C8—C13177.6 (9)
O12—Pb1—O1—S1103.3 (4)C13—C8—C9—O4176.4 (8)
O13—Pb1—O1—S149.5 (5)C7—C8—C9—O41.1 (13)
O2—Pb1—O1—S12.6 (3)C13—C8—C9—C100.4 (13)
O9—Pb1—O2—S1147.3 (5)C7—C8—C9—C10178.0 (8)
O5—Pb1—O2—S1158.9 (4)O4—C9—C10—C11178.0 (9)
O10—Pb1—O2—S172.5 (4)C8—C9—C10—C111.0 (14)
O11—Pb1—O2—S10.5 (5)C9—C10—C11—C121.3 (15)
O12—Pb1—O2—S171.5 (4)C10—C11—C12—C130.1 (15)
O13—Pb1—O2—S1137.9 (4)C11—C12—C13—C81.4 (15)
O1—Pb1—O2—S12.7 (3)C9—C8—C13—C121.7 (14)
O9—Pb1—O5—S233.1 (5)C7—C8—C13—C12179.3 (9)
O10—Pb1—O5—S2110.6 (5)O6—S2—C14—C152.0 (8)
O11—Pb1—O5—S2175.1 (6)O7—S2—C14—C15122.4 (7)
O12—Pb1—O5—S2107.6 (5)O5—S2—C14—C15119.4 (7)
O13—Pb1—O5—S244.4 (5)O6—S2—C14—C19173.9 (7)
O1—Pb1—O5—S2159.1 (4)O7—S2—C14—C1953.6 (8)
O2—Pb1—O5—S221.5 (9)O5—S2—C14—C1964.7 (8)
Pb1—O2—S1—O3131.0 (4)C19—C14—C15—C162.1 (13)
Pb1—O2—S1—O14.1 (5)S2—C14—C15—C16173.9 (7)
Pb1—O2—S1—C1112.2 (3)C14—C15—C16—C171.1 (14)
Pb1—O1—S1—O24.3 (5)C20—N2—C17—C18151.5 (9)
Pb1—O1—S1—O3132.3 (4)C20—N2—C17—C1634.4 (13)
Pb1—O1—S1—C1112.1 (3)C15—C16—C17—C180.4 (13)
Pb1—O5—S2—O624.2 (7)C15—C16—C17—N2173.7 (8)
Pb1—O5—S2—O7103.3 (5)N2—C17—C18—C19173.4 (8)
Pb1—O5—S2—C14142.0 (5)C16—C17—C18—C190.9 (14)
O2—S1—C1—C263.3 (8)C17—C18—C19—C140.0 (14)
O3—S1—C1—C258.5 (9)C15—C14—C19—C181.5 (13)
O1—S1—C1—C2178.2 (7)S2—C14—C19—C18174.5 (7)
O2—S1—C1—C6116.0 (8)C17—N2—C20—C21172.0 (8)
O3—S1—C1—C6122.1 (8)N2—C20—C21—C26179.7 (9)
O1—S1—C1—C62.5 (9)N2—C20—C21—C221.6 (14)
C6—C1—C2—C30.1 (14)C26—C21—C22—O8178.5 (8)
S1—C1—C2—C3179.4 (7)C20—C21—C22—O82.9 (13)
C1—C2—C3—C40.9 (14)C26—C21—C22—C231.2 (13)
C2—C3—C4—C52.6 (14)C20—C21—C22—C23177.4 (8)
C2—C3—C4—N1178.4 (8)O8—C22—C23—C24178.9 (9)
C7—N1—C4—C5148.1 (9)C21—C22—C23—C240.8 (14)
C7—N1—C4—C336.0 (13)C22—C23—C24—C250.0 (15)
C3—C4—C5—C63.4 (14)C23—C24—C25—C260.2 (15)
N1—C4—C5—C6179.4 (8)C24—C25—C26—C210.3 (15)
C2—C1—C6—C50.7 (14)C22—C21—C26—C251.0 (14)
S1—C1—C6—C5178.7 (7)C20—C21—C26—C25177.6 (9)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H4···N10.821.902.626 (9)147
O4—H4···O4i0.822.592.897 (9)104
O8—H8···N20.821.882.611 (10)147
O8—H8···O8ii0.822.602.933 (9)106
O9—H9A···O60.852.042.781 (11)146
O9—H9B···O5iii0.852.172.911 (9)146
O10—H10A···O6iv0.852.122.914 (9)156
O10—H10B···O7iii0.851.942.771 (9)167
O11—H11A···O3v0.852.072.883 (11)162
O11—H11B···O7iv0.852.062.772 (9)141
O12—H12A···O3v0.852.032.841 (13)159
O12—H12B···O2vi0.852.082.922 (11)170
O13—H13A···O2vi0.852.543.287 (13)148
O13—H13B···O1vii0.852.232.867 (11)132
C6—H6···O10.932.522.898 (10)104
C15—H15···O60.932.522.907 (10)105
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+2, z+2; (iii) x, y+1/2, z3/2; (iv) x, y1, z; (v) x, y1/2, z1/2; (vi) x, y+1/2, z1/2; (vii) x, y+1, z.

Experimental details

Crystal data
Chemical formula[Pb(C13H10NO4S)2(H2O)5]
Mr849.83
Crystal system, space groupMonoclinic, P21/c
Temperature (K)298
a, b, c (Å)35.618 (4), 7.3407 (10), 11.6218 (18)
β (°) 99.146 (2)
V3)3000.0 (7)
Z4
Radiation typeMo Kα
µ (mm1)5.83
Crystal size (mm)0.50 × 0.40 × 0.38
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2000)
Tmin, Tmax0.159, 0.215
No. of measured, independent and
observed [I > 2σ(I)] reflections
14411, 5264, 4635
Rint0.045
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.051, 0.129, 1.09
No. of reflections5264
No. of parameters397
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0518P)2 + 32.8197P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.95, 4.10

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Pb1—O92.523 (7)Pb1—O122.702 (7)
Pb1—O52.531 (6)Pb1—O132.713 (8)
Pb1—O102.534 (7)Pb1—O12.761 (8)
Pb1—O112.576 (7)Pb1—O22.882 (8)
S1—O1—Pb1102.3 (4)S1—O2—Pb197.8 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H4···N10.82001.90002.626 (9)147.00
O4—H4···O4i0.82002.59002.897 (9)104.00
O8—H8···N20.82001.88002.611 (10)147.00
O8—H8···O8ii0.82002.60002.933 (9)106.00
O9—H9A···O60.85002.04002.781 (11)146.00
O9—H9B···O5iii0.85002.17002.911 (9)146.00
O10—H10A···O6iv0.85002.12002.914 (9)156.00
O10—H10B···O7iii0.85001.94002.771 (9)167.00
O11—H11A···O3v0.85002.07002.883 (11)162.00
O11—H11B···O7iv0.85002.06002.772 (9)141.00
O12—H12A···O3v0.85002.03002.841 (13)159.00
O12—H12B···O2vi0.85002.08002.922 (11)170.00
O13—H13A···O2vi0.85002.54003.287 (13)148.00
O13—H13B···O1vii0.85002.23002.867 (11)132.00
C6—H6···O10.93002.52002.898 (10)104.00
C15—H15···O60.93002.52002.907 (10)105.00
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+2, z+2; (iii) x, y+1/2, z3/2; (iv) x, y1, z; (v) x, y1/2, z1/2; (vi) x, y+1/2, z1/2; (vii) x, y+1, z.
 

Acknowledgements

The authors thank the National Natural Science Foundation of China (grant No. 20671073), the Natural Science Foundation of Shandong (grant No. Y2007B60), the Science and Technology Foundation of Weifang, and Weifang University for a research grant.

References

First citationBruker (2000). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationTai, X.-S., Feng, Y.-M. & Kong, F.-Y. (2008). Acta Cryst. E64, o750.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationTai, X. S., Yin, J. & Feng, Y. M. (2007). Z. Kristallogr. New Cryst. Struct. 222, 343–344.  CAS Google Scholar
First citationTai, X. S., Yin, J. & Kong, F. Y. (2007). Z. Kristallogr. New Cryst. Struct. 222, 401–402.  CAS Google Scholar
First citationTai, X.-S., Yin, X.-H., Tan, M.-Y. & Li, Y.-Z. (2003). Acta Cryst. E59, o681–o682.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationXi-Shi, T. & Yi-Min, F. (2008). Acta Cryst. E64, o707.  Web of Science CSD CrossRef IUCr Journals Google Scholar

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Volume 65| Part 3| March 2009| Pages m275-m276
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