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In the title compound, [Pb2(C7H4O6S)2(C12H8N2)2(H2O)2], two [Pb(phen)(H2O)] moieties are connected together by two Hssa anions, resulting in a centrosymmetric dimer (phen is 1,10-phenanthroline and Hssa is the hydrogen 5-sulfosalicyl­ate dianion). Each PbII cation is surrounded by O atoms from a carboxyl­ate group in a chelating fashion, a sulfonate group in a monodentate mode, a water mol­ecule, and two N atoms from a phen ligand, forming a distorted PbO4N2 octahedron.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804018483/ob6398sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804018483/ob6398Isup2.hkl
Contains datablock I

CCDC reference: 251576

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.021
  • wR factor = 0.053
  • Data-to-parameter ratio = 11.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pb1 - O1 .. 7.13 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pb1 - O2 .. 5.00 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pb1 - O4_a .. 6.69 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Pb1 - O6_a .. 8.77 su PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for O2 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for S1 PLAT731_ALERT_1_C Bond Calc 0.81(4), Rep 0.810(18) ...... 2.22 su-Rat O7 -H7A 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.81(4), Rep 0.810(18) ...... 2.22 su-Rat O7 -H7A 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.84(4), Rep 1.844(19) ...... 2.11 su-Rat H7A -O5 1.555 2.655
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 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

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Bruker, 2002); software used to prepare material for publication: SHELXL97.

Bis(µ-hydrogen 5-sulfosalicylate)bis[aqua(1,10-phenanthroline)lead(II)] top
Crystal data top
[Pb2(C7H4O6S)2(C12H8N2)2(H2O)2]Z = 1
Mr = 1243.14F(000) = 592
Triclinic, P1Dx = 2.211 Mg m3
Hall symbol: -P1Mo Kα radiation, λ = 0.71073 Å
a = 8.2520 (11) ÅCell parameters from 3935 reflections
b = 10.2384 (13) Åθ = 2.5–25.2°
c = 11.3422 (15) ŵ = 9.19 mm1
α = 84.979 (2)°T = 298 K
β = 84.407 (2)°Block, colourless
γ = 78.970 (2)°0.32 × 0.27 × 0.20 mm
V = 933.8 (2) Å3
Data collection top
Bruker APEX CCD area-detector
diffractometer
3307 independent reflections
Radiation source: fine-focus sealed tube3126 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.015
φ and ω scansθmax = 25.2°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 99
Tmin = 0.073, Tmax = 0.161k = 1212
4971 measured reflectionsl = 513
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)] = 0.021H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.053 w = 1/[σ2(Fo2) + (0.0335P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
3307 reflectionsΔρmax = 0.74 e Å3
279 parametersΔρmin = 0.86 e Å3
3 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0189 (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
Pb10.942373 (16)0.200026 (13)0.341781 (12)0.03049 (9)
S10.67198 (13)0.02934 (11)0.25115 (9)0.0360 (2)
O10.7446 (4)0.2699 (3)0.2022 (3)0.0443 (7)
O20.8808 (4)0.0689 (4)0.1611 (3)0.0516 (8)
O30.4876 (4)0.3760 (3)0.0980 (3)0.0461 (7)
H30.55670.36780.14660.069*
O40.7666 (4)0.1509 (3)0.2005 (3)0.0478 (8)
O50.5205 (5)0.0505 (5)0.2936 (4)0.0847 (15)
O60.7743 (5)0.0337 (3)0.3410 (3)0.0559 (9)
O70.6879 (5)0.1137 (4)0.4338 (3)0.0546 (9)
N10.9867 (4)0.4350 (3)0.2615 (3)0.0320 (7)
N20.7929 (4)0.3944 (3)0.4683 (3)0.0315 (7)
C10.6663 (5)0.1743 (4)0.0373 (3)0.0296 (8)
C20.5306 (5)0.2777 (4)0.0231 (3)0.0335 (9)
C30.4359 (6)0.2797 (5)0.0721 (4)0.0460 (11)
H3A0.34370.34690.08140.055*
C40.4769 (5)0.1841 (4)0.1522 (4)0.0408 (10)
H40.41320.18720.21600.049*
C50.6130 (5)0.0825 (4)0.1390 (3)0.0302 (8)
C60.7065 (5)0.0768 (4)0.0438 (3)0.0287 (8)
H60.79630.00770.03380.034*
C70.7719 (5)0.1670 (4)0.1397 (3)0.0341 (9)
C81.0789 (5)0.4546 (4)0.1620 (4)0.0403 (10)
H81.13150.38110.12120.048*
C91.1004 (6)0.5821 (5)0.1155 (4)0.0478 (11)
H91.16380.59270.04420.057*
C101.0276 (6)0.6905 (5)0.1760 (4)0.0448 (11)
H101.04200.77550.14630.054*
C110.9312 (5)0.6738 (4)0.2828 (4)0.0338 (9)
C120.8551 (5)0.7824 (4)0.3520 (4)0.0408 (10)
H120.86920.86870.32630.049*
C130.7627 (5)0.7609 (4)0.4548 (4)0.0377 (9)
H130.71280.83310.49820.045*
C140.7403 (5)0.6303 (4)0.4977 (4)0.0326 (8)
C150.6464 (5)0.6056 (4)0.6036 (4)0.0395 (10)
H150.59460.67600.64860.047*
C160.6307 (6)0.4779 (5)0.6411 (4)0.0427 (10)
H160.57160.45990.71280.051*
C170.7048 (5)0.3748 (4)0.5702 (4)0.0388 (10)
H170.69170.28830.59550.047*
C180.8129 (4)0.5215 (4)0.4319 (3)0.0273 (8)
C190.9130 (4)0.5431 (4)0.3223 (3)0.0288 (8)
H7A0.628 (5)0.092 (4)0.389 (3)0.035*
H7B0.684 (5)0.079 (4)0.5018 (19)0.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.03444 (11)0.02586 (11)0.03144 (11)0.00315 (6)0.00357 (6)0.00788 (6)
S10.0367 (5)0.0418 (6)0.0304 (5)0.0036 (4)0.0028 (4)0.0159 (4)
O10.064 (2)0.0395 (17)0.0348 (16)0.0152 (14)0.0102 (15)0.0115 (13)
O20.0453 (18)0.066 (2)0.0423 (18)0.0047 (16)0.0138 (15)0.0196 (16)
O30.061 (2)0.0391 (17)0.0352 (17)0.0021 (15)0.0013 (14)0.0163 (14)
O40.064 (2)0.0324 (16)0.0437 (18)0.0067 (14)0.0093 (15)0.0073 (13)
O50.049 (2)0.126 (4)0.089 (3)0.005 (2)0.020 (2)0.072 (3)
O60.077 (2)0.0463 (19)0.0333 (17)0.0083 (17)0.0125 (16)0.0024 (14)
O70.071 (2)0.068 (2)0.0358 (18)0.0419 (19)0.0113 (17)0.0037 (16)
N10.0337 (17)0.0301 (17)0.0321 (18)0.0057 (13)0.0016 (14)0.0063 (14)
N20.0390 (18)0.0267 (17)0.0282 (17)0.0062 (14)0.0028 (14)0.0041 (13)
C10.034 (2)0.036 (2)0.0202 (18)0.0121 (16)0.0024 (16)0.0031 (15)
C20.044 (2)0.031 (2)0.025 (2)0.0055 (17)0.0059 (17)0.0055 (16)
C30.042 (2)0.047 (3)0.043 (3)0.011 (2)0.008 (2)0.009 (2)
C40.038 (2)0.053 (3)0.029 (2)0.0050 (19)0.0081 (18)0.012 (2)
C50.0333 (19)0.032 (2)0.025 (2)0.0059 (16)0.0010 (16)0.0058 (16)
C60.0268 (18)0.030 (2)0.029 (2)0.0058 (15)0.0007 (15)0.0043 (16)
C70.039 (2)0.044 (2)0.023 (2)0.0146 (19)0.0010 (17)0.0054 (17)
C80.044 (2)0.040 (2)0.034 (2)0.0066 (19)0.0082 (19)0.0049 (18)
C90.051 (3)0.056 (3)0.035 (2)0.015 (2)0.011 (2)0.002 (2)
C100.047 (2)0.038 (2)0.049 (3)0.013 (2)0.001 (2)0.005 (2)
C110.036 (2)0.031 (2)0.036 (2)0.0076 (17)0.0044 (17)0.0029 (17)
C120.046 (2)0.025 (2)0.053 (3)0.0082 (18)0.007 (2)0.0044 (19)
C130.045 (2)0.026 (2)0.041 (2)0.0017 (17)0.005 (2)0.0081 (17)
C140.0293 (19)0.032 (2)0.037 (2)0.0018 (15)0.0038 (17)0.0094 (17)
C150.044 (2)0.033 (2)0.038 (2)0.0016 (18)0.0057 (19)0.0136 (18)
C160.049 (3)0.041 (2)0.036 (2)0.007 (2)0.011 (2)0.0119 (19)
C170.048 (2)0.032 (2)0.036 (2)0.0099 (18)0.0046 (19)0.0071 (18)
C180.0282 (18)0.0235 (18)0.031 (2)0.0039 (14)0.0065 (15)0.0025 (15)
C190.0289 (18)0.029 (2)0.029 (2)0.0039 (15)0.0039 (15)0.0041 (15)
Geometric parameters (Å, º) top
Pb1—O12.354 (3)C3—H3A0.9300
Pb1—O72.530 (3)C4—C51.388 (6)
Pb1—N12.577 (3)C4—H40.9300
Pb1—N22.599 (3)C5—C61.378 (5)
Pb1—O22.684 (3)C6—H60.9300
Pb1—O4i2.742 (3)C8—C91.400 (6)
S1—O41.442 (3)C8—H80.9300
S1—O51.443 (4)C9—C101.365 (7)
S1—O61.447 (3)C9—H90.9300
S1—C51.757 (4)C10—C111.399 (6)
O1—C71.293 (5)C10—H100.9300
O2—C71.237 (5)C11—C191.405 (5)
O3—C21.347 (5)C11—C121.427 (6)
O3—H30.8200C12—C131.355 (6)
O4—Pb1i2.742 (3)C12—H120.9300
O7—H7A0.810 (18)C13—C141.422 (6)
O7—H7B0.820 (18)C13—H130.9300
N1—C81.321 (5)C14—C151.396 (6)
N1—C191.366 (5)C14—C181.401 (5)
N2—C171.325 (5)C15—C161.366 (6)
N2—C181.366 (5)C15—H150.9300
C1—C61.388 (6)C16—C171.393 (6)
C1—C21.397 (6)C16—H160.9300
C1—C71.507 (5)C17—H170.9300
C2—C31.390 (6)C18—C191.448 (5)
C3—C41.367 (6)
O1—Pb1—O775.64 (11)C6—C5—C4119.9 (4)
O1—Pb1—N175.07 (10)C6—C5—S1121.1 (3)
O7—Pb1—N1131.98 (12)C4—C5—S1118.7 (3)
O1—Pb1—N288.59 (10)C5—C6—C1119.9 (4)
O7—Pb1—N277.80 (11)C5—C6—H6120.0
N1—Pb1—N264.31 (10)C1—C6—H6120.0
O1—Pb1—O251.60 (10)O2—C7—O1122.0 (4)
O7—Pb1—O280.31 (11)O2—C7—C1121.6 (4)
N1—Pb1—O2108.80 (11)O1—C7—C1116.4 (4)
N2—Pb1—O2138.34 (10)N1—C8—C9122.4 (4)
O1—Pb1—O4i102.56 (11)N1—C8—H8118.8
O7—Pb1—O4i147.10 (11)C9—C8—H8118.8
N1—Pb1—O4i76.65 (9)C10—C9—C8119.4 (4)
N2—Pb1—O4i135.05 (9)C10—C9—H9120.3
O2—Pb1—O4i73.83 (10)C8—C9—H9120.3
O4—S1—O5112.1 (3)C9—C10—C11119.9 (4)
O4—S1—O6110.2 (2)C9—C10—H10120.0
O5—S1—O6113.1 (3)C11—C10—H10120.0
O4—S1—C5108.39 (18)C10—C11—C19117.3 (4)
O5—S1—C5106.3 (2)C10—C11—C12122.8 (4)
O6—S1—C5106.45 (19)C19—C11—C12120.0 (4)
C7—O1—Pb1100.2 (2)C13—C12—C11120.5 (4)
C7—O2—Pb186.2 (2)C13—C12—H12119.8
C2—O3—H3109.5C11—C12—H12119.8
S1—O4—Pb1i106.09 (16)C12—C13—C14121.4 (4)
Pb1—O7—H7A117 (3)C12—C13—H13119.3
Pb1—O7—H7B121 (3)C14—C13—H13119.3
H7A—O7—H7B117 (3)C15—C14—C18118.0 (4)
C8—N1—C19118.5 (3)C15—C14—C13122.4 (4)
C8—N1—Pb1121.8 (3)C18—C14—C13119.6 (4)
C19—N1—Pb1119.7 (2)C16—C15—C14119.8 (4)
C17—N2—C18118.3 (3)C16—C15—H15120.1
C17—N2—Pb1122.7 (3)C14—C15—H15120.1
C18—N2—Pb1118.8 (2)C15—C16—C17119.0 (4)
C6—C1—C2120.2 (3)C15—C16—H16120.5
C6—C1—C7118.9 (3)C17—C16—H16120.5
C2—C1—C7120.9 (4)N2—C17—C16123.0 (4)
O3—C2—C3118.4 (4)N2—C17—H17118.5
O3—C2—C1122.7 (4)C16—C17—H17118.5
C3—C2—C1118.9 (4)N2—C18—C14121.8 (4)
C4—C3—C2120.7 (4)N2—C18—C19118.6 (3)
C4—C3—H3A119.7C14—C18—C19119.5 (3)
C2—C3—H3A119.7N1—C19—C11122.5 (4)
C3—C4—C5120.4 (4)N1—C19—C18118.5 (3)
C3—C4—H4119.8C11—C19—C18119.0 (3)
C5—C4—H4119.8
Symmetry code: (i) x+2, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O10.821.812.542 (4)147
O7—H7A···O5ii0.81 (2)1.84 (2)2.653 (5)176 (5)
O7—H7B···O6iii0.82 (2)1.98 (2)2.733 (5)152 (4)
Symmetry codes: (ii) x+1, y, z; (iii) x, y, z+1.
 

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