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
CCDC reference: 251576
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (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
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 = 1243.14 | F(000) = 592 |
Triclinic, P1 | Dx = 2.211 Mg m−3 |
Hall symbol: -P1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.2520 (11) Å | Cell parameters from 3935 reflections |
b = 10.2384 (13) Å | θ = 2.5–25.2° |
c = 11.3422 (15) Å | µ = 9.19 mm−1 |
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 tube | 3126 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.015 |
φ and ω scans | θmax = 25.2°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −9→9 |
Tmin = 0.073, Tmax = 0.161 | k = −12→12 |
4971 measured reflections | l = −5→13 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.021 | H 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 reflections | Δρmax = 0.74 e Å−3 |
279 parameters | Δρmin = −0.86 e Å−3 |
3 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction 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 | x | y | z | Uiso*/Ueq | |
Pb1 | 0.942373 (16) | 0.200026 (13) | 0.341781 (12) | 0.03049 (9) | |
S1 | 0.67198 (13) | −0.02934 (11) | −0.25115 (9) | 0.0360 (2) | |
O1 | 0.7446 (4) | 0.2699 (3) | 0.2022 (3) | 0.0443 (7) | |
O2 | 0.8808 (4) | 0.0689 (4) | 0.1611 (3) | 0.0516 (8) | |
O3 | 0.4876 (4) | 0.3760 (3) | 0.0980 (3) | 0.0461 (7) | |
H3 | 0.5567 | 0.3678 | 0.1466 | 0.069* | |
O4 | 0.7666 (4) | −0.1509 (3) | −0.2005 (3) | 0.0478 (8) | |
O5 | 0.5205 (5) | −0.0505 (5) | −0.2936 (4) | 0.0847 (15) | |
O6 | 0.7743 (5) | 0.0337 (3) | −0.3410 (3) | 0.0559 (9) | |
O7 | 0.6879 (5) | 0.1137 (4) | 0.4338 (3) | 0.0546 (9) | |
N1 | 0.9867 (4) | 0.4350 (3) | 0.2615 (3) | 0.0320 (7) | |
N2 | 0.7929 (4) | 0.3944 (3) | 0.4683 (3) | 0.0315 (7) | |
C1 | 0.6663 (5) | 0.1743 (4) | 0.0373 (3) | 0.0296 (8) | |
C2 | 0.5306 (5) | 0.2777 (4) | 0.0231 (3) | 0.0335 (9) | |
C3 | 0.4359 (6) | 0.2797 (5) | −0.0721 (4) | 0.0460 (11) | |
H3A | 0.3437 | 0.3469 | −0.0814 | 0.055* | |
C4 | 0.4769 (5) | 0.1841 (4) | −0.1522 (4) | 0.0408 (10) | |
H4 | 0.4132 | 0.1872 | −0.2160 | 0.049* | |
C5 | 0.6130 (5) | 0.0825 (4) | −0.1390 (3) | 0.0302 (8) | |
C6 | 0.7065 (5) | 0.0768 (4) | −0.0438 (3) | 0.0287 (8) | |
H6 | 0.7963 | 0.0077 | −0.0338 | 0.034* | |
C7 | 0.7719 (5) | 0.1670 (4) | 0.1397 (3) | 0.0341 (9) | |
C8 | 1.0789 (5) | 0.4546 (4) | 0.1620 (4) | 0.0403 (10) | |
H8 | 1.1315 | 0.3811 | 0.1212 | 0.048* | |
C9 | 1.1004 (6) | 0.5821 (5) | 0.1155 (4) | 0.0478 (11) | |
H9 | 1.1638 | 0.5927 | 0.0442 | 0.057* | |
C10 | 1.0276 (6) | 0.6905 (5) | 0.1760 (4) | 0.0448 (11) | |
H10 | 1.0420 | 0.7755 | 0.1463 | 0.054* | |
C11 | 0.9312 (5) | 0.6738 (4) | 0.2828 (4) | 0.0338 (9) | |
C12 | 0.8551 (5) | 0.7824 (4) | 0.3520 (4) | 0.0408 (10) | |
H12 | 0.8692 | 0.8687 | 0.3263 | 0.049* | |
C13 | 0.7627 (5) | 0.7609 (4) | 0.4548 (4) | 0.0377 (9) | |
H13 | 0.7128 | 0.8331 | 0.4982 | 0.045* | |
C14 | 0.7403 (5) | 0.6303 (4) | 0.4977 (4) | 0.0326 (8) | |
C15 | 0.6464 (5) | 0.6056 (4) | 0.6036 (4) | 0.0395 (10) | |
H15 | 0.5946 | 0.6760 | 0.6486 | 0.047* | |
C16 | 0.6307 (6) | 0.4779 (5) | 0.6411 (4) | 0.0427 (10) | |
H16 | 0.5716 | 0.4599 | 0.7128 | 0.051* | |
C17 | 0.7048 (5) | 0.3748 (4) | 0.5702 (4) | 0.0388 (10) | |
H17 | 0.6917 | 0.2883 | 0.5955 | 0.047* | |
C18 | 0.8129 (4) | 0.5215 (4) | 0.4319 (3) | 0.0273 (8) | |
C19 | 0.9130 (4) | 0.5431 (4) | 0.3223 (3) | 0.0288 (8) | |
H7A | 0.628 (5) | 0.092 (4) | 0.389 (3) | 0.035* | |
H7B | 0.684 (5) | 0.079 (4) | 0.5018 (19) | 0.035* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pb1 | 0.03444 (11) | 0.02586 (11) | 0.03144 (11) | −0.00315 (6) | −0.00357 (6) | −0.00788 (6) |
S1 | 0.0367 (5) | 0.0418 (6) | 0.0304 (5) | −0.0036 (4) | −0.0028 (4) | −0.0159 (4) |
O1 | 0.064 (2) | 0.0395 (17) | 0.0348 (16) | −0.0152 (14) | −0.0102 (15) | −0.0115 (13) |
O2 | 0.0453 (18) | 0.066 (2) | 0.0423 (18) | 0.0047 (16) | −0.0138 (15) | −0.0196 (16) |
O3 | 0.061 (2) | 0.0391 (17) | 0.0352 (17) | 0.0021 (15) | 0.0013 (14) | −0.0163 (14) |
O4 | 0.064 (2) | 0.0324 (16) | 0.0437 (18) | −0.0067 (14) | 0.0093 (15) | −0.0073 (13) |
O5 | 0.049 (2) | 0.126 (4) | 0.089 (3) | −0.005 (2) | −0.020 (2) | −0.072 (3) |
O6 | 0.077 (2) | 0.0463 (19) | 0.0333 (17) | 0.0083 (17) | 0.0125 (16) | −0.0024 (14) |
O7 | 0.071 (2) | 0.068 (2) | 0.0358 (18) | −0.0419 (19) | −0.0113 (17) | 0.0037 (16) |
N1 | 0.0337 (17) | 0.0301 (17) | 0.0321 (18) | −0.0057 (13) | 0.0016 (14) | −0.0063 (14) |
N2 | 0.0390 (18) | 0.0267 (17) | 0.0282 (17) | −0.0062 (14) | 0.0028 (14) | −0.0041 (13) |
C1 | 0.034 (2) | 0.036 (2) | 0.0202 (18) | −0.0121 (16) | 0.0024 (16) | −0.0031 (15) |
C2 | 0.044 (2) | 0.031 (2) | 0.025 (2) | −0.0055 (17) | 0.0059 (17) | −0.0055 (16) |
C3 | 0.042 (2) | 0.047 (3) | 0.043 (3) | 0.011 (2) | −0.008 (2) | −0.009 (2) |
C4 | 0.038 (2) | 0.053 (3) | 0.029 (2) | 0.0050 (19) | −0.0081 (18) | −0.012 (2) |
C5 | 0.0333 (19) | 0.032 (2) | 0.025 (2) | −0.0059 (16) | −0.0010 (16) | −0.0058 (16) |
C6 | 0.0268 (18) | 0.030 (2) | 0.029 (2) | −0.0058 (15) | −0.0007 (15) | −0.0043 (16) |
C7 | 0.039 (2) | 0.044 (2) | 0.023 (2) | −0.0146 (19) | 0.0010 (17) | −0.0054 (17) |
C8 | 0.044 (2) | 0.040 (2) | 0.034 (2) | −0.0066 (19) | 0.0082 (19) | −0.0049 (18) |
C9 | 0.051 (3) | 0.056 (3) | 0.035 (2) | −0.015 (2) | 0.011 (2) | 0.002 (2) |
C10 | 0.047 (2) | 0.038 (2) | 0.049 (3) | −0.013 (2) | 0.001 (2) | 0.005 (2) |
C11 | 0.036 (2) | 0.031 (2) | 0.036 (2) | −0.0076 (17) | −0.0044 (17) | −0.0029 (17) |
C12 | 0.046 (2) | 0.025 (2) | 0.053 (3) | −0.0082 (18) | −0.007 (2) | −0.0044 (19) |
C13 | 0.045 (2) | 0.026 (2) | 0.041 (2) | −0.0017 (17) | −0.005 (2) | −0.0081 (17) |
C14 | 0.0293 (19) | 0.032 (2) | 0.037 (2) | −0.0018 (15) | −0.0038 (17) | −0.0094 (17) |
C15 | 0.044 (2) | 0.033 (2) | 0.038 (2) | 0.0016 (18) | 0.0057 (19) | −0.0136 (18) |
C16 | 0.049 (3) | 0.041 (2) | 0.036 (2) | −0.007 (2) | 0.011 (2) | −0.0119 (19) |
C17 | 0.048 (2) | 0.032 (2) | 0.036 (2) | −0.0099 (18) | 0.0046 (19) | −0.0071 (18) |
C18 | 0.0282 (18) | 0.0235 (18) | 0.031 (2) | −0.0039 (14) | −0.0065 (15) | −0.0025 (15) |
C19 | 0.0289 (18) | 0.029 (2) | 0.029 (2) | −0.0039 (15) | −0.0039 (15) | −0.0041 (15) |
Geometric parameters (Å, º) top
Pb1—O1 | 2.354 (3) | C3—H3A | 0.9300 |
Pb1—O7 | 2.530 (3) | C4—C5 | 1.388 (6) |
Pb1—N1 | 2.577 (3) | C4—H4 | 0.9300 |
Pb1—N2 | 2.599 (3) | C5—C6 | 1.378 (5) |
Pb1—O2 | 2.684 (3) | C6—H6 | 0.9300 |
Pb1—O4i | 2.742 (3) | C8—C9 | 1.400 (6) |
S1—O4 | 1.442 (3) | C8—H8 | 0.9300 |
S1—O5 | 1.443 (4) | C9—C10 | 1.365 (7) |
S1—O6 | 1.447 (3) | C9—H9 | 0.9300 |
S1—C5 | 1.757 (4) | C10—C11 | 1.399 (6) |
O1—C7 | 1.293 (5) | C10—H10 | 0.9300 |
O2—C7 | 1.237 (5) | C11—C19 | 1.405 (5) |
O3—C2 | 1.347 (5) | C11—C12 | 1.427 (6) |
O3—H3 | 0.8200 | C12—C13 | 1.355 (6) |
O4—Pb1i | 2.742 (3) | C12—H12 | 0.9300 |
O7—H7A | 0.810 (18) | C13—C14 | 1.422 (6) |
O7—H7B | 0.820 (18) | C13—H13 | 0.9300 |
N1—C8 | 1.321 (5) | C14—C15 | 1.396 (6) |
N1—C19 | 1.366 (5) | C14—C18 | 1.401 (5) |
N2—C17 | 1.325 (5) | C15—C16 | 1.366 (6) |
N2—C18 | 1.366 (5) | C15—H15 | 0.9300 |
C1—C6 | 1.388 (6) | C16—C17 | 1.393 (6) |
C1—C2 | 1.397 (6) | C16—H16 | 0.9300 |
C1—C7 | 1.507 (5) | C17—H17 | 0.9300 |
C2—C3 | 1.390 (6) | C18—C19 | 1.448 (5) |
C3—C4 | 1.367 (6) | | |
| | | |
O1—Pb1—O7 | 75.64 (11) | C6—C5—C4 | 119.9 (4) |
O1—Pb1—N1 | 75.07 (10) | C6—C5—S1 | 121.1 (3) |
O7—Pb1—N1 | 131.98 (12) | C4—C5—S1 | 118.7 (3) |
O1—Pb1—N2 | 88.59 (10) | C5—C6—C1 | 119.9 (4) |
O7—Pb1—N2 | 77.80 (11) | C5—C6—H6 | 120.0 |
N1—Pb1—N2 | 64.31 (10) | C1—C6—H6 | 120.0 |
O1—Pb1—O2 | 51.60 (10) | O2—C7—O1 | 122.0 (4) |
O7—Pb1—O2 | 80.31 (11) | O2—C7—C1 | 121.6 (4) |
N1—Pb1—O2 | 108.80 (11) | O1—C7—C1 | 116.4 (4) |
N2—Pb1—O2 | 138.34 (10) | N1—C8—C9 | 122.4 (4) |
O1—Pb1—O4i | 102.56 (11) | N1—C8—H8 | 118.8 |
O7—Pb1—O4i | 147.10 (11) | C9—C8—H8 | 118.8 |
N1—Pb1—O4i | 76.65 (9) | C10—C9—C8 | 119.4 (4) |
N2—Pb1—O4i | 135.05 (9) | C10—C9—H9 | 120.3 |
O2—Pb1—O4i | 73.83 (10) | C8—C9—H9 | 120.3 |
O4—S1—O5 | 112.1 (3) | C9—C10—C11 | 119.9 (4) |
O4—S1—O6 | 110.2 (2) | C9—C10—H10 | 120.0 |
O5—S1—O6 | 113.1 (3) | C11—C10—H10 | 120.0 |
O4—S1—C5 | 108.39 (18) | C10—C11—C19 | 117.3 (4) |
O5—S1—C5 | 106.3 (2) | C10—C11—C12 | 122.8 (4) |
O6—S1—C5 | 106.45 (19) | C19—C11—C12 | 120.0 (4) |
C7—O1—Pb1 | 100.2 (2) | C13—C12—C11 | 120.5 (4) |
C7—O2—Pb1 | 86.2 (2) | C13—C12—H12 | 119.8 |
C2—O3—H3 | 109.5 | C11—C12—H12 | 119.8 |
S1—O4—Pb1i | 106.09 (16) | C12—C13—C14 | 121.4 (4) |
Pb1—O7—H7A | 117 (3) | C12—C13—H13 | 119.3 |
Pb1—O7—H7B | 121 (3) | C14—C13—H13 | 119.3 |
H7A—O7—H7B | 117 (3) | C15—C14—C18 | 118.0 (4) |
C8—N1—C19 | 118.5 (3) | C15—C14—C13 | 122.4 (4) |
C8—N1—Pb1 | 121.8 (3) | C18—C14—C13 | 119.6 (4) |
C19—N1—Pb1 | 119.7 (2) | C16—C15—C14 | 119.8 (4) |
C17—N2—C18 | 118.3 (3) | C16—C15—H15 | 120.1 |
C17—N2—Pb1 | 122.7 (3) | C14—C15—H15 | 120.1 |
C18—N2—Pb1 | 118.8 (2) | C15—C16—C17 | 119.0 (4) |
C6—C1—C2 | 120.2 (3) | C15—C16—H16 | 120.5 |
C6—C1—C7 | 118.9 (3) | C17—C16—H16 | 120.5 |
C2—C1—C7 | 120.9 (4) | N2—C17—C16 | 123.0 (4) |
O3—C2—C3 | 118.4 (4) | N2—C17—H17 | 118.5 |
O3—C2—C1 | 122.7 (4) | C16—C17—H17 | 118.5 |
C3—C2—C1 | 118.9 (4) | N2—C18—C14 | 121.8 (4) |
C4—C3—C2 | 120.7 (4) | N2—C18—C19 | 118.6 (3) |
C4—C3—H3A | 119.7 | C14—C18—C19 | 119.5 (3) |
C2—C3—H3A | 119.7 | N1—C19—C11 | 122.5 (4) |
C3—C4—C5 | 120.4 (4) | N1—C19—C18 | 118.5 (3) |
C3—C4—H4 | 119.8 | C11—C19—C18 | 119.0 (3) |
C5—C4—H4 | 119.8 | | |
Symmetry code: (i) −x+2, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O1 | 0.82 | 1.81 | 2.542 (4) | 147 |
O7—H7A···O5ii | 0.81 (2) | 1.84 (2) | 2.653 (5) | 176 (5) |
O7—H7B···O6iii | 0.82 (2) | 1.98 (2) | 2.733 (5) | 152 (4) |
Symmetry codes: (ii) −x+1, −y, −z; (iii) x, y, z+1. |