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The title compound, [Pb(C7H4O5S)(H2O)2]·C10H8N2, crystallizes as a two-dimensional coordination polymer. Double sheets are formed by Pb2+ ions which are connected by μ4-bridging 3-sulfonatobenzoate groups. The coordination around the Pb atoms comprises three O atoms from carboxyl­ate groups, two O atoms from the sulfonate group and additionally two water mol­ecules. As a result of hydrogen bonds between 4,4′-bipyridine and water mol­ecules attached to Pb2+ the double layer structure is extended to give a three-dimensional supra­molecular architecture.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806051270/tk2103sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806051270/tk2103Isup2.hkl
Contains datablock I

CCDC reference: 634063

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.019
  • wR factor = 0.056
  • Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 4000 Deg. PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1 PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.841(19) ...... 2.11 su-Ra O6 -H6 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.855(19) ...... 2.11 su-Ra O6 -H5 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(5), Rep 0.844(19) ...... 2.63 su-Ra O7 -H7 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.846(19) ...... 2.11 su-Ra O7 -H8 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.842(19) ...... 2.11 su-Ra O6 -H6 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.846(19) ...... 2.11 su-Ra O7 -H8 1.555 1.555
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT804_ALERT_5_G ARU-Pack Problem in PLATON Analysis ............ 1 Times
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Computing details top

Data collection: STADI-4 (Stoe & Cie, 1996); cell refinement: STADI-4; data reduction: STADI-4; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97.

Poly[[diaqua(µ4-3-sulfonatobenzoato)lead(II)] 4,4'-bipyridine] top
Crystal data top
[Pb(C7H4O5S)(H2O)2]·C10H8N2Z = 2
Mr = 599.57F(000) = 572
Triclinic, P1Dx = 2.080 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.178 (5) ÅCell parameters from 24 reflections
b = 9.483 (4) Åθ = 7.7–11.0°
c = 12.790 (6) ŵ = 8.96 mm1
α = 89.19 (4)°T = 293 K
β = 80.73 (4)°Needle, colourless
γ = 78.05 (4)°0.38 × 0.09 × 0.09 mm
V = 957.5 (9) Å3
Data collection top
Stoe Stadi-4
diffractometer
3236 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.031
Graphite monochromatorθmax = 25.0°, θmin = 1.6°
ω–2θ scansh = 99
Absorption correction: ψ scan
(X-RED32; Stoe & Cie, 1996)
k = 1111
Tmin = 0.054, Tmax = 0.445l = 1515
6715 measured reflections2 standard reflections every 60 min
3380 independent reflections intensity decay: random variation +5%
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)] = 0.019H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.056 w = 1/[σ2(Fo2) + (0.0311P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.19(Δ/σ)max < 0.001
3380 reflectionsΔρmax = 0.98 e Å3
270 parametersΔρmin = 0.79 e Å3
6 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0110 (6)
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
C10.2082 (5)0.8695 (4)0.8971 (3)0.0272 (7)
C20.1912 (5)1.0093 (4)0.8775 (3)0.0289 (8)
H10.08871.03560.88070.035*
C30.3275 (5)1.1109 (4)0.8530 (3)0.0268 (7)
C40.4814 (5)1.0731 (4)0.8480 (3)0.0323 (8)
H20.57171.14120.83050.039*
C50.4990 (5)0.9339 (5)0.8691 (3)0.0357 (9)
H30.60200.90810.86630.043*
C60.3634 (5)0.8310 (4)0.8948 (3)0.0326 (8)
H40.37640.73740.91020.039*
C70.0566 (5)0.7582 (4)0.9169 (3)0.0310 (8)
C80.1887 (6)1.0826 (5)0.5183 (3)0.0369 (9)
C90.1455 (7)1.0637 (6)0.6272 (4)0.0488 (12)
H90.06551.13360.66850.059*
C100.2226 (8)0.9409 (7)0.6726 (4)0.0568 (14)
H100.19240.93070.74510.068*
C110.3794 (7)0.8532 (6)0.5155 (4)0.0525 (12)
H110.46090.78170.47680.063*
C120.3080 (7)0.9717 (6)0.4620 (4)0.0453 (11)
H120.33920.97750.38920.054*
C130.1063 (6)1.2131 (5)0.4656 (3)0.0372 (10)
C140.0538 (6)1.2910 (5)0.5067 (3)0.0424 (10)
H130.10991.26630.57130.051*
C150.1294 (6)1.4050 (5)0.4514 (4)0.0468 (11)
H140.23811.45390.47950.056*
C160.1007 (7)1.3789 (6)0.3226 (3)0.0505 (12)
H150.15581.41000.25980.061*
C170.1860 (7)1.2625 (5)0.3714 (3)0.0450 (11)
H160.29551.21720.34190.054*
N10.3383 (6)0.8352 (5)0.6193 (4)0.0552 (11)
N20.0555 (6)1.4495 (4)0.3597 (3)0.0477 (10)
O10.0872 (4)0.7877 (3)0.8987 (3)0.0461 (7)
O20.0770 (4)0.6341 (3)0.9488 (3)0.0420 (7)
O30.4341 (4)1.3750 (3)0.9185 (2)0.0398 (7)
O40.3510 (5)1.3319 (3)0.7294 (2)0.0487 (8)
O50.1396 (4)1.3006 (4)0.8471 (3)0.0538 (8)
O60.4130 (5)0.6056 (4)0.7615 (3)0.0545 (9)
H60.402 (7)0.668 (4)0.714 (3)0.060 (17)*
H50.484 (6)0.531 (4)0.735 (4)0.064 (18)*
O70.1772 (4)0.3802 (4)0.8005 (2)0.0416 (7)
H70.086 (5)0.352 (7)0.819 (4)0.09 (2)*
H80.174 (6)0.423 (6)0.742 (3)0.057 (16)*
S0.30985 (12)1.29300 (10)0.83358 (7)0.0309 (2)
Pb0.243824 (15)0.539897 (14)0.933755 (10)0.02885 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0266 (19)0.0212 (18)0.0304 (17)0.0007 (15)0.0027 (14)0.0036 (14)
C20.0214 (18)0.027 (2)0.0369 (18)0.0021 (15)0.0028 (15)0.0001 (15)
C30.0268 (19)0.0226 (19)0.0283 (16)0.0003 (15)0.0038 (15)0.0018 (14)
C40.030 (2)0.031 (2)0.0345 (18)0.0006 (17)0.0082 (16)0.0045 (15)
C50.031 (2)0.034 (2)0.043 (2)0.0071 (18)0.0088 (17)0.0002 (17)
C60.036 (2)0.027 (2)0.0352 (18)0.0069 (18)0.0060 (16)0.0037 (16)
C70.032 (2)0.024 (2)0.0325 (18)0.0022 (17)0.0045 (16)0.0045 (15)
C80.042 (2)0.038 (2)0.036 (2)0.017 (2)0.0103 (18)0.0083 (17)
C90.054 (3)0.058 (3)0.034 (2)0.010 (3)0.008 (2)0.010 (2)
C100.062 (3)0.072 (4)0.043 (2)0.021 (3)0.020 (2)0.021 (3)
C110.051 (3)0.043 (3)0.066 (3)0.012 (2)0.014 (2)0.005 (2)
C120.054 (3)0.043 (3)0.040 (2)0.014 (2)0.006 (2)0.0041 (19)
C130.045 (3)0.041 (2)0.0309 (18)0.019 (2)0.0114 (18)0.0023 (17)
C140.046 (3)0.046 (3)0.038 (2)0.019 (2)0.0057 (19)0.0053 (19)
C150.044 (3)0.046 (3)0.053 (2)0.012 (2)0.012 (2)0.002 (2)
C160.069 (4)0.050 (3)0.034 (2)0.018 (3)0.007 (2)0.007 (2)
C170.054 (3)0.044 (3)0.034 (2)0.008 (2)0.002 (2)0.0064 (18)
N10.060 (3)0.053 (3)0.061 (2)0.021 (2)0.025 (2)0.022 (2)
N20.061 (3)0.039 (2)0.049 (2)0.014 (2)0.020 (2)0.0062 (17)
O10.0273 (15)0.0363 (17)0.0702 (19)0.0005 (13)0.0038 (14)0.0216 (15)
O20.0375 (16)0.0268 (16)0.0602 (17)0.0043 (13)0.0086 (14)0.0175 (13)
O30.0415 (17)0.0300 (16)0.0413 (15)0.0044 (14)0.0019 (13)0.0053 (12)
O40.071 (2)0.0335 (17)0.0364 (14)0.0017 (16)0.0045 (15)0.0094 (12)
O50.0338 (17)0.0342 (18)0.094 (2)0.0098 (14)0.0102 (17)0.0125 (17)
O60.054 (2)0.038 (2)0.059 (2)0.0069 (18)0.0040 (17)0.0206 (17)
O70.0358 (17)0.0441 (19)0.0461 (17)0.0118 (15)0.0066 (14)0.0067 (14)
S0.0295 (5)0.0208 (5)0.0383 (5)0.0010 (4)0.0022 (4)0.0039 (4)
Pb0.02344 (11)0.02329 (11)0.03851 (11)0.00113 (6)0.00640 (6)0.00609 (6)
Geometric parameters (Å, º) top
C1—C21.376 (5)C13—C171.398 (6)
C1—C61.397 (5)C14—C151.376 (7)
C1—C71.505 (5)C14—H130.9300
C2—C31.389 (5)C15—N21.335 (6)
C2—H10.9300C15—H140.9300
C3—C41.390 (6)C16—N21.329 (7)
C3—S1.773 (4)C16—C171.377 (7)
C4—C51.375 (6)C16—H150.9300
C4—H20.9300C17—H160.9300
C5—C61.396 (6)Pb—O12.504 (3)
C5—H30.9300Pb—O22.567 (4)
C6—H40.9300Pb—O2i2.654 (3)
C7—O11.250 (5)Pb—O3ii2.749 (4)
C7—O21.275 (5)Pb—O3iii2.856 (3)
C8—C121.395 (7)O2—Pbi2.654 (3)
C8—C91.400 (6)O3—S1.469 (3)
C8—C131.489 (6)O3—Pbiv2.749 (4)
C9—C101.373 (8)O4—S1.451 (3)
C9—H90.9300O5—S1.447 (3)
C10—N11.335 (8)Pb—O62.549 (4)
C10—H100.9300O6—H60.841 (19)
C11—N11.334 (7)O6—H50.855 (19)
C11—C121.380 (7)Pb—O72.492 (3)
C11—H110.9300O7—H70.844 (19)
C12—H120.9300O7—H80.846 (19)
C13—C141.388 (7)O3—Pbiv2.749 (4)
C2—C1—C6120.0 (4)N2—C16—H15118.0
C2—C1—C7119.4 (3)C17—C16—H15118.0
C6—C1—C7120.6 (3)C16—C17—C13119.3 (5)
C1—C2—C3119.8 (3)C16—C17—H16120.3
C1—C2—H1120.1C13—C17—H16120.3
C3—C2—H1120.1C11—N1—C10116.5 (5)
C2—C3—C4120.7 (4)C16—N2—C15116.6 (4)
C2—C3—S120.1 (3)C7—O1—Pb95.4 (2)
C4—C3—S119.1 (3)C7—O2—Pb91.8 (2)
C5—C4—C3119.4 (4)C7—O2—Pbi152.7 (3)
C5—C4—H2120.3Pb—O2—Pbi110.41 (11)
C3—C4—H2120.3S—O3—Pbiv135.60 (17)
C4—C5—C6120.5 (4)Pb—O6—H6139 (4)
C4—C5—H3119.8Pb—O6—H5109 (3)
C6—C5—H3119.8H6—O6—H5108 (3)
C5—C6—C1119.5 (4)Pb—O7—H7114 (5)
C5—C6—H4120.2Pb—O7—H8110 (4)
C1—C6—H4120.2H7—O7—H8109 (3)
O1—C7—O2121.3 (4)O5—S—O4114.8 (2)
O1—C7—C1119.5 (4)O5—S—O3110.5 (2)
O2—C7—C1119.3 (4)O4—S—O3112.0 (2)
C12—C8—C9116.7 (5)O5—S—C3106.67 (19)
C12—C8—C13122.2 (4)O4—S—C3107.18 (18)
C9—C8—C13121.1 (4)O3—S—C3105.05 (18)
C10—C9—C8119.3 (5)O1—Pb—O251.41 (10)
C10—C9—H9120.4O1—Pb—O2i118.59 (11)
C8—C9—H9120.4O1—Pb—O3ii141.79 (10)
N1—C10—C9124.3 (5)O1—Pb—O3iii96.80 (11)
N1—C10—H10117.9O1—Pb—O676.72 (12)
C9—C10—H10117.9O1—Pb—O7105.00 (11)
N1—C11—C12123.9 (6)O2—Pb—O2i69.59 (11)
N1—C11—H11118.1O2—Pb—O3ii166.11 (10)
C12—C11—H11118.1O2—Pb—O3iii121.90 (10)
C11—C12—C8119.4 (5)O2—Pb—O6113.72 (12)
C11—C12—H12120.3O2—Pb—O779.65 (11)
C8—C12—H12120.3O2i—Pb—O3ii98.79 (10)
C14—C13—C17116.6 (4)O2i—Pb—O3iii100.95 (10)
C14—C13—C8121.9 (4)O2i—Pb—O6152.37 (12)
C17—C13—C8121.5 (4)O2i—Pb—O776.48 (11)
C15—C14—C13119.7 (4)O3ii—Pb—O3iii66.64 (11)
C15—C14—H13120.1O3ii—Pb—O672.88 (11)
C13—C14—H13120.1O3ii—Pb—O790.41 (11)
N2—C15—C14123.7 (5)O3iii—Pb—O699.63 (12)
N2—C15—H14118.1O3iii—Pb—O7156.45 (10)
C14—C15—H14118.1O6—Pb—O777.27 (13)
N2—C16—C17123.9 (5)
C6—C1—C2—C31.5 (5)O2—C7—O1—Pb3.8 (4)
C7—C1—C2—C3176.2 (3)C1—C7—O1—Pb174.0 (3)
C1—C2—C3—C40.0 (5)O1—C7—O2—Pb3.7 (4)
C1—C2—C3—S177.1 (3)C1—C7—O2—Pb174.2 (3)
C2—C3—C4—C51.0 (5)O1—C7—O2—Pbi141.7 (5)
S—C3—C4—C5176.2 (3)C1—C7—O2—Pbi40.5 (7)
C3—C4—C5—C60.4 (6)Pbiv—O3—S—O5145.2 (2)
C4—C5—C6—C11.1 (6)Pbiv—O3—S—O415.9 (3)
C2—C1—C6—C52.0 (5)Pbiv—O3—S—C3100.1 (3)
C7—C1—C6—C5175.6 (3)C2—C3—S—O50.8 (4)
C2—C1—C7—O111.4 (5)C4—C3—S—O5178.0 (3)
C6—C1—C7—O1166.3 (4)C2—C3—S—O4124.1 (3)
C2—C1—C7—O2170.7 (3)C4—C3—S—O458.6 (3)
C6—C1—C7—O211.6 (5)C2—C3—S—O3116.5 (3)
C12—C8—C9—C100.9 (7)C4—C3—S—O360.7 (3)
C13—C8—C9—C10179.1 (5)C7—O1—Pb—O761.1 (3)
C8—C9—C10—N10.2 (9)C7—O1—Pb—O6133.8 (3)
N1—C11—C12—C81.7 (8)C7—O1—Pb—O22.1 (2)
C9—C8—C12—C111.6 (7)C7—O1—Pb—O2i21.5 (3)
C13—C8—C12—C11179.8 (4)C7—O1—Pb—O3ii171.7 (2)
C12—C8—C13—C14152.5 (4)C7—O1—Pb—O3iii127.9 (2)
C9—C8—C13—C1425.5 (6)C7—O2—Pb—O7116.8 (2)
C12—C8—C13—C1726.7 (6)Pbi—O2—Pb—O779.31 (13)
C9—C8—C13—C17155.2 (4)C7—O2—Pb—O12.0 (2)
C17—C13—C14—C153.7 (6)Pbi—O2—Pb—O1161.85 (19)
C8—C13—C14—C15175.6 (4)C7—O2—Pb—O645.8 (3)
C13—C14—C15—N21.8 (7)Pbi—O2—Pb—O6150.34 (13)
N2—C16—C17—C130.1 (8)C7—O2—Pb—O2i163.9 (3)
C14—C13—C17—C162.9 (6)Pbi—O2—Pb—O2i0.0
C8—C13—C17—C16176.4 (4)C7—O2—Pb—O3ii161.7 (3)
C12—C11—N1—C101.0 (8)Pbi—O2—Pb—O3ii34.4 (4)
C9—C10—N1—C110.2 (8)C7—O2—Pb—O3iii73.5 (3)
C17—C16—N2—C151.9 (7)Pbi—O2—Pb—O3iii90.41 (13)
C14—C15—N2—C161.0 (7)
Symmetry codes: (i) x, y+1, z+2; (ii) x+1, y1, z; (iii) x, y+2, z+2; (iv) x1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H6···N10.84 (2)2.02 (2)2.849 (6)170 (5)
O7—H8···N2v0.85 (2)1.99 (3)2.773 (5)153 (5)
Symmetry code: (v) x, y+2, z+1.
 

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