| Literature DB >> 21582655 |
Jun Dai, Juan Yang, Xiaobing An.
Abstract
The reaction of lead(II) acetate and 3-methyl-benzoic acid (MBA) in aqueous solution yielded the title polymer, [Pb(C(8)H(7)O(2))(2)(H(2)O)](n). The asymmetric unit contains two Pb(II) atoms, four MBA ligands and two water mol-ecules. Each Pb(II) cation is hepta-coordinated and chelated by four carboxyl-ate O atoms from two MBA ligands. The Pb atoms are bridged through the carboxyl-ate O atoms from another two MBA ligands, leading to a central Pb(2)O(2) core. The Pb-O bond lengths are in the range 2.325 (3)-2.757 (4) Å. The intra- and inter-dimer Pb⋯Pb distances are 4.2942 (3) and 4.2283 (3) Å, respectively, indicating little direct metal-metal inter-action. The coordinating water mol-ecules and carboxyl-ate O atoms are involved in extensive O-H⋯O hydrogen-bonding inter-actions. The complex has an extended ladder-like chain structure and the chains are assembled by hydrogen bonds and π-π inter-actions [centroid-centroid distance = 3.6246 (3) Å] into a three-dimensional supra-molecular structure.Entities:
Year: 2009 PMID: 21582655 PMCID: PMC2969469 DOI: 10.1107/S1600536809019771
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Pb(C8H7O2)2(H2O)] | |
| Monoclinic, | Mo |
| Hall symbol: -P 2yn | Cell parameters from 7418 reflections |
| θ = 2.4–25.2° | |
| µ = 10.29 mm−1 | |
| β = 90.765 (1)° | Block, colourless |
| 0.36 × 0.17 × 0.12 mm | |
| Bruker APEXII CCD area-detector diffractometer | 8096 independent reflections |
| Radiation source: fine-focus sealed tube | 6265 reflections with |
| graphite | |
| φ and ω scans | θmax = 28.2°, θmin = 1.9° |
| Absorption correction: multi-scan ( | |
| 40611 measured reflections |
| Refinement on | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| H-atom parameters constrained | |
| (Δ/σ)max = 0.001 | |
| 8096 reflections | Δρmax = 0.87 e Å−3 |
| 397 parameters | Δρmin = −1.00 e Å−3 |
| 0 restraints | Extinction correction: |
| Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.082 |
| Pb1 | 0.12243 (2) | 0.097018 (5) | 0.352944 (18) | 0.03251 (6) | |
| Pb2 | 0.63079 (2) | 0.136517 (5) | 0.498730 (18) | 0.03285 (6) | |
| O1 | 0.0014 (5) | 0.06035 (8) | 0.5043 (3) | 0.0425 (9) | |
| O2 | 0.2904 (5) | 0.04888 (8) | 0.4562 (3) | 0.0422 (9) | |
| O3 | −0.0208 (5) | 0.12954 (8) | 0.5322 (3) | 0.0417 (9) | |
| O4 | 0.2740 (4) | 0.11793 (8) | 0.5341 (3) | 0.0382 (8) | |
| O5 | 0.4697 (5) | 0.10648 (9) | 0.2967 (3) | 0.0431 (9) | |
| O6 | 0.7648 (4) | 0.11863 (8) | 0.3157 (3) | 0.0361 (8) | |
| O7 | 0.7820 (5) | 0.18516 (8) | 0.4032 (4) | 0.0456 (9) | |
| O8 | 0.4875 (5) | 0.17631 (9) | 0.3567 (4) | 0.0532 (11) | |
| O9 | 0.1259 (5) | 0.15838 (9) | 0.2844 (4) | 0.0536 (11) | |
| H9A | 0.2336 | 0.1648 | 0.2856 | 0.064* | |
| H9B | 0.0480 | 0.1635 | 0.3359 | 0.064* | |
| O10 | 0.6329 (5) | 0.07555 (8) | 0.5507 (3) | 0.0435 (9) | |
| H10B | 0.5587 | 0.0665 | 0.5043 | 0.052* | |
| H10A | 0.7351 | 0.0704 | 0.5243 | 0.052* | |
| C1 | 0.1464 (7) | 0.04397 (11) | 0.5191 (5) | 0.0350 (12) | |
| C2 | 0.1449 (7) | 0.01859 (11) | 0.6140 (5) | 0.0327 (11) | |
| C3 | −0.0085 (7) | 0.01413 (12) | 0.6892 (5) | 0.0419 (13) | |
| H3A | −0.1126 | 0.0268 | 0.6775 | 0.050* | |
| C4 | −0.0118 (8) | −0.00864 (13) | 0.7814 (5) | 0.0449 (14) | |
| C5 | 0.1437 (9) | −0.02741 (13) | 0.7950 (6) | 0.0501 (15) | |
| H5A | 0.1450 | −0.0428 | 0.8563 | 0.060* | |
| C6 | 0.2948 (8) | −0.02395 (13) | 0.7213 (6) | 0.0483 (15) | |
| H6A | 0.3966 | −0.0372 | 0.7319 | 0.058* | |
| C7 | 0.2988 (8) | −0.00088 (12) | 0.6303 (5) | 0.0416 (13) | |
| H7A | 0.4032 | 0.0016 | 0.5807 | 0.050* | |
| C8 | −0.1813 (10) | −0.01275 (18) | 0.8623 (7) | 0.080 (2) | |
| H8A | −0.1591 | −0.0294 | 0.9210 | 0.121* | |
| H8B | −0.2874 | −0.0178 | 0.8107 | 0.121* | |
| H8C | −0.2050 | 0.0063 | 0.9066 | 0.121* | |
| C9 | 0.1354 (7) | 0.13040 (11) | 0.5855 (4) | 0.0297 (11) | |
| C10 | 0.1578 (7) | 0.14561 (12) | 0.7091 (5) | 0.0367 (12) | |
| C11 | 0.0214 (9) | 0.16600 (13) | 0.7525 (6) | 0.0514 (15) | |
| H11A | −0.0821 | 0.1705 | 0.7024 | 0.062* | |
| C12 | 0.0388 (12) | 0.17949 (16) | 0.8690 (7) | 0.072 (2) | |
| C13 | 0.1933 (15) | 0.1719 (2) | 0.9412 (7) | 0.093 (3) | |
| H13A | 0.2058 | 0.1805 | 1.0205 | 0.111* | |
| C14 | 0.3266 (12) | 0.1524 (2) | 0.8998 (7) | 0.081 (2) | |
| H14A | 0.4297 | 0.1481 | 0.9505 | 0.097* | |
| C15 | 0.3122 (9) | 0.13865 (15) | 0.7832 (5) | 0.0563 (17) | |
| H15A | 0.4040 | 0.1251 | 0.7551 | 0.068* | |
| C16 | −0.1079 (14) | 0.2018 (2) | 0.9145 (9) | 0.131 (4) | |
| H16A | −0.0742 | 0.2091 | 0.9965 | 0.197* | |
| H16B | −0.2258 | 0.1912 | 0.9175 | 0.197* | |
| H16C | −0.1171 | 0.2193 | 0.8586 | 0.197* | |
| C17 | 0.6265 (6) | 0.10896 (11) | 0.2509 (5) | 0.0296 (11) | |
| C18 | 0.6596 (7) | 0.10073 (11) | 0.1176 (5) | 0.0308 (11) | |
| C19 | 0.5301 (8) | 0.08355 (12) | 0.0511 (5) | 0.0425 (13) | |
| H19A | 0.4204 | 0.0776 | 0.0896 | 0.051* | |
| C20 | 0.5586 (10) | 0.07500 (14) | −0.0711 (6) | 0.0558 (17) | |
| C21 | 0.7238 (11) | 0.08378 (15) | −0.1256 (6) | 0.0634 (19) | |
| H21A | 0.7476 | 0.0777 | −0.2072 | 0.076* | |
| C22 | 0.8544 (10) | 0.10140 (15) | −0.0611 (6) | 0.0612 (18) | |
| H22A | 0.9636 | 0.1076 | −0.0999 | 0.073* | |
| C23 | 0.8229 (8) | 0.10979 (13) | 0.0606 (5) | 0.0420 (13) | |
| H23A | 0.9110 | 0.1215 | 0.1045 | 0.050* | |
| C24 | 0.4110 (11) | 0.05680 (17) | −0.1440 (7) | 0.090 (3) | |
| H24A | 0.4543 | 0.0528 | −0.2269 | 0.135* | |
| H24B | 0.2980 | 0.0688 | −0.1483 | 0.135* | |
| H24C | 0.3875 | 0.0373 | −0.1027 | 0.135* | |
| C25 | 0.6358 (8) | 0.19171 (13) | 0.3421 (5) | 0.0413 (13) | |
| C26 | 0.6358 (8) | 0.21833 (13) | 0.2526 (5) | 0.0437 (14) | |
| C27 | 0.7935 (9) | 0.23678 (13) | 0.2416 (5) | 0.0500 (15) | |
| H27A | 0.8980 | 0.2324 | 0.2908 | 0.060* | |
| C28 | 0.7986 (11) | 0.26149 (15) | 0.1590 (6) | 0.0643 (19) | |
| C29 | 0.6435 (15) | 0.26682 (19) | 0.0853 (7) | 0.091 (3) | |
| H29A | 0.6446 | 0.2832 | 0.0283 | 0.109* | |
| C30 | 0.4891 (14) | 0.2487 (2) | 0.0936 (8) | 0.095 (3) | |
| H30A | 0.3868 | 0.2526 | 0.0417 | 0.114* | |
| C31 | 0.4833 (10) | 0.22464 (17) | 0.1785 (7) | 0.069 (2) | |
| H31A | 0.3758 | 0.2126 | 0.1857 | 0.083* | |
| C32 | 0.9668 (12) | 0.28192 (18) | 0.1483 (8) | 0.107 (3) | |
| H32A | 0.9438 | 0.2978 | 0.0865 | 0.161* | |
| H32B | 1.0717 | 0.2695 | 0.1242 | 0.161* | |
| H32C | 0.9928 | 0.2916 | 0.2274 | 0.161* |
| Pb1 | 0.02451 (10) | 0.04213 (12) | 0.03088 (11) | −0.00082 (8) | 0.00003 (7) | −0.00184 (9) |
| Pb2 | 0.02385 (9) | 0.04156 (12) | 0.03319 (11) | 0.00000 (8) | 0.00229 (8) | −0.00581 (9) |
| O1 | 0.034 (2) | 0.042 (2) | 0.052 (2) | 0.0036 (17) | 0.0058 (18) | 0.0068 (18) |
| O2 | 0.0285 (19) | 0.049 (2) | 0.050 (2) | −0.0036 (16) | 0.0087 (17) | 0.0043 (18) |
| O3 | 0.034 (2) | 0.053 (2) | 0.038 (2) | 0.0047 (17) | −0.0067 (17) | −0.0090 (18) |
| O4 | 0.0249 (18) | 0.049 (2) | 0.041 (2) | −0.0005 (16) | 0.0056 (16) | −0.0044 (18) |
| O5 | 0.0280 (19) | 0.059 (2) | 0.042 (2) | −0.0028 (17) | 0.0080 (17) | −0.0055 (19) |
| O6 | 0.0273 (18) | 0.050 (2) | 0.031 (2) | −0.0020 (16) | −0.0003 (15) | −0.0068 (17) |
| O7 | 0.037 (2) | 0.042 (2) | 0.058 (3) | −0.0016 (17) | −0.0059 (19) | 0.0046 (19) |
| O8 | 0.039 (2) | 0.052 (2) | 0.068 (3) | −0.0060 (19) | −0.012 (2) | 0.005 (2) |
| O9 | 0.035 (2) | 0.069 (3) | 0.057 (3) | −0.007 (2) | 0.0047 (19) | 0.001 (2) |
| O10 | 0.033 (2) | 0.053 (2) | 0.045 (2) | 0.0014 (17) | 0.0021 (17) | −0.0025 (18) |
| C1 | 0.032 (3) | 0.034 (3) | 0.039 (3) | −0.005 (2) | 0.000 (2) | −0.004 (2) |
| C2 | 0.036 (3) | 0.030 (3) | 0.033 (3) | −0.005 (2) | −0.001 (2) | −0.004 (2) |
| C3 | 0.034 (3) | 0.041 (3) | 0.051 (4) | −0.003 (2) | 0.002 (3) | −0.006 (3) |
| C4 | 0.047 (3) | 0.044 (3) | 0.044 (4) | −0.010 (3) | 0.003 (3) | 0.001 (3) |
| C5 | 0.069 (4) | 0.034 (3) | 0.047 (4) | −0.003 (3) | −0.007 (3) | 0.005 (3) |
| C6 | 0.052 (4) | 0.038 (3) | 0.055 (4) | 0.008 (3) | −0.002 (3) | 0.005 (3) |
| C7 | 0.041 (3) | 0.037 (3) | 0.047 (4) | 0.008 (2) | 0.004 (3) | −0.005 (3) |
| C8 | 0.069 (5) | 0.098 (6) | 0.074 (5) | −0.007 (4) | 0.018 (4) | 0.030 (4) |
| C9 | 0.028 (3) | 0.035 (3) | 0.026 (3) | −0.002 (2) | −0.002 (2) | 0.002 (2) |
| C10 | 0.041 (3) | 0.039 (3) | 0.031 (3) | −0.007 (2) | −0.004 (2) | 0.004 (2) |
| C11 | 0.064 (4) | 0.046 (3) | 0.044 (4) | 0.005 (3) | 0.003 (3) | −0.008 (3) |
| C12 | 0.111 (6) | 0.056 (4) | 0.049 (4) | −0.004 (4) | 0.008 (4) | −0.013 (4) |
| C13 | 0.151 (9) | 0.081 (6) | 0.045 (5) | −0.023 (6) | −0.015 (5) | −0.022 (4) |
| C14 | 0.105 (7) | 0.093 (6) | 0.044 (4) | −0.022 (5) | −0.029 (4) | 0.003 (4) |
| C15 | 0.058 (4) | 0.073 (4) | 0.038 (4) | −0.003 (3) | −0.016 (3) | 0.004 (3) |
| C16 | 0.178 (10) | 0.098 (7) | 0.119 (8) | 0.041 (7) | 0.035 (7) | −0.058 (6) |
| C17 | 0.025 (2) | 0.034 (3) | 0.030 (3) | 0.002 (2) | 0.002 (2) | 0.001 (2) |
| C18 | 0.031 (3) | 0.027 (3) | 0.034 (3) | 0.004 (2) | 0.005 (2) | 0.002 (2) |
| C19 | 0.056 (4) | 0.041 (3) | 0.030 (3) | −0.006 (3) | −0.001 (3) | 0.001 (2) |
| C20 | 0.086 (5) | 0.044 (4) | 0.037 (4) | −0.009 (3) | −0.008 (3) | −0.008 (3) |
| C21 | 0.106 (6) | 0.052 (4) | 0.033 (4) | −0.005 (4) | 0.020 (4) | −0.005 (3) |
| C22 | 0.073 (5) | 0.066 (4) | 0.046 (4) | −0.005 (4) | 0.026 (3) | 0.005 (3) |
| C23 | 0.043 (3) | 0.045 (3) | 0.038 (3) | −0.002 (3) | 0.003 (3) | 0.004 (3) |
| C24 | 0.139 (8) | 0.079 (5) | 0.052 (5) | −0.039 (5) | −0.021 (5) | −0.021 (4) |
| C25 | 0.039 (3) | 0.040 (3) | 0.046 (4) | 0.000 (3) | −0.002 (3) | −0.005 (3) |
| C26 | 0.053 (4) | 0.038 (3) | 0.040 (3) | 0.007 (3) | −0.004 (3) | −0.007 (3) |
| C27 | 0.065 (4) | 0.043 (3) | 0.042 (4) | 0.007 (3) | 0.005 (3) | 0.000 (3) |
| C28 | 0.101 (6) | 0.045 (4) | 0.047 (4) | 0.013 (4) | 0.018 (4) | 0.002 (3) |
| C29 | 0.148 (9) | 0.069 (5) | 0.057 (5) | 0.025 (6) | 0.020 (6) | 0.025 (4) |
| C30 | 0.107 (7) | 0.104 (7) | 0.074 (6) | 0.021 (6) | −0.022 (5) | 0.034 (5) |
| C31 | 0.064 (5) | 0.077 (5) | 0.065 (5) | 0.000 (4) | −0.014 (4) | 0.011 (4) |
| C32 | 0.132 (8) | 0.070 (5) | 0.120 (8) | −0.018 (5) | 0.045 (6) | 0.028 (5) |
| Pb1—O4 | 2.386 (3) | C10—C15 | 1.387 (7) |
| Pb1—O1 | 2.424 (3) | C10—C11 | 1.395 (7) |
| Pb1—O3 | 2.594 (3) | C11—C12 | 1.380 (8) |
| Pb1—O5 | 2.603 (3) | C11—H11A | 0.9300 |
| Pb1—O2 | 2.622 (4) | C12—C13 | 1.381 (11) |
| Pb1—O9 | 2.724 (4) | C12—C16 | 1.505 (10) |
| Pb1—O6i | 2.751 (3) | C13—C14 | 1.348 (11) |
| Pb2—O6 | 2.325 (3) | C13—H13A | 0.9300 |
| Pb2—O8 | 2.494 (4) | C14—C15 | 1.384 (9) |
| Pb2—O3ii | 2.538 (3) | C14—H14A | 0.9300 |
| Pb2—O7 | 2.565 (4) | C15—H15A | 0.9300 |
| Pb2—O10 | 2.665 (3) | C16—H16A | 0.9600 |
| Pb2—O4 | 2.712 (3) | C16—H16B | 0.9600 |
| Pb2—O5 | 2.757 (4) | C16—H16C | 0.9600 |
| O1—C1 | 1.263 (6) | C17—C18 | 1.493 (7) |
| O2—C1 | 1.258 (6) | C18—C19 | 1.376 (7) |
| O3—C9 | 1.251 (5) | C18—C23 | 1.384 (7) |
| O3—Pb2i | 2.538 (3) | C19—C20 | 1.377 (8) |
| O4—C9 | 1.261 (5) | C19—H19A | 0.9300 |
| O5—C17 | 1.238 (5) | C20—C21 | 1.380 (9) |
| O6—C17 | 1.273 (5) | C20—C24 | 1.521 (8) |
| O6—Pb1ii | 2.751 (3) | C21—C22 | 1.381 (9) |
| O7—C25 | 1.261 (6) | C21—H21A | 0.9300 |
| O8—C25 | 1.263 (6) | C22—C23 | 1.373 (8) |
| O9—H9A | 0.8200 | C22—H22A | 0.9300 |
| O9—H9B | 0.8200 | C23—H23A | 0.9300 |
| O10—H10B | 0.8200 | C24—H24A | 0.9600 |
| O10—H10A | 0.8200 | C24—H24B | 0.9600 |
| C1—C2 | 1.487 (7) | C24—H24C | 0.9600 |
| C2—C3 | 1.386 (7) | C25—C26 | 1.488 (8) |
| C2—C7 | 1.392 (7) | C26—C31 | 1.370 (8) |
| C3—C4 | 1.387 (7) | C26—C27 | 1.386 (8) |
| C3—H3A | 0.9300 | C27—C28 | 1.378 (8) |
| C4—C5 | 1.380 (8) | C27—H27A | 0.9300 |
| C4—C8 | 1.513 (8) | C28—C29 | 1.375 (11) |
| C5—C6 | 1.358 (8) | C28—C32 | 1.495 (10) |
| C5—H5A | 0.9300 | C29—C30 | 1.355 (11) |
| C6—C7 | 1.388 (7) | C29—H29A | 0.9300 |
| C6—H6A | 0.9300 | C30—C31 | 1.375 (10) |
| C7—H7A | 0.9300 | C30—H30A | 0.9300 |
| C8—H8A | 0.9600 | C31—H31A | 0.9300 |
| C8—H8B | 0.9600 | C32—H32A | 0.9600 |
| C8—H8C | 0.9600 | C32—H32B | 0.9600 |
| C9—C10 | 1.482 (7) | C32—H32C | 0.9600 |
| O4—Pb1—O1 | 82.05 (12) | C4—C8—H8B | 109.5 |
| O4—Pb1—O3 | 51.51 (11) | H8A—C8—H8B | 109.5 |
| O1—Pb1—O3 | 72.68 (12) | C4—C8—H8C | 109.5 |
| O4—Pb1—O5 | 72.72 (11) | H8A—C8—H8C | 109.5 |
| O1—Pb1—O5 | 127.44 (12) | H8B—C8—H8C | 109.5 |
| O3—Pb1—O5 | 118.56 (11) | O3—C9—O4 | 119.7 (5) |
| O4—Pb1—O2 | 75.46 (12) | O3—C9—C10 | 120.4 (4) |
| O1—Pb1—O2 | 51.48 (11) | O4—C9—C10 | 119.9 (4) |
| O3—Pb1—O2 | 107.02 (11) | C15—C10—C11 | 120.2 (5) |
| O5—Pb1—O2 | 77.50 (11) | C15—C10—C9 | 119.5 (5) |
| O4—Pb1—O9 | 81.54 (12) | C11—C10—C9 | 120.2 (5) |
| O1—Pb1—O9 | 143.85 (12) | C12—C11—C10 | 120.5 (6) |
| O3—Pb1—O9 | 71.86 (12) | C12—C11—H11A | 119.8 |
| O5—Pb1—O9 | 77.05 (11) | C10—C11—H11A | 119.8 |
| O2—Pb1—O9 | 149.74 (11) | C11—C12—C13 | 118.1 (7) |
| O4—Pb1—O6i | 113.97 (10) | C11—C12—C16 | 120.2 (8) |
| O1—Pb1—O6i | 88.41 (11) | C13—C12—C16 | 121.8 (7) |
| O3—Pb1—O6i | 63.23 (10) | C14—C13—C12 | 121.9 (7) |
| O5—Pb1—O6i | 143.91 (11) | C14—C13—H13A | 119.0 |
| O2—Pb1—O6i | 138.35 (10) | C12—C13—H13A | 119.0 |
| O9—Pb1—O6i | 69.48 (10) | C13—C14—C15 | 121.0 (7) |
| O6—Pb2—O8 | 83.21 (13) | C13—C14—H14A | 119.5 |
| O6—Pb2—O3ii | 70.29 (11) | C15—C14—H14A | 119.5 |
| O8—Pb2—O3ii | 124.28 (12) | C14—C15—C10 | 118.4 (7) |
| O6—Pb2—O7 | 75.42 (12) | C14—C15—H15A | 120.8 |
| O8—Pb2—O7 | 51.46 (12) | C10—C15—H15A | 120.8 |
| O3ii—Pb2—O7 | 74.37 (12) | C12—C16—H16A | 109.5 |
| O6—Pb2—O10 | 81.57 (11) | C12—C16—H16B | 109.5 |
| O8—Pb2—O10 | 142.70 (12) | H16A—C16—H16B | 109.5 |
| O3ii—Pb2—O10 | 81.54 (11) | C12—C16—H16C | 109.5 |
| O7—Pb2—O10 | 151.05 (11) | H16A—C16—H16C | 109.5 |
| O6—Pb2—O4 | 115.06 (11) | H16B—C16—H16C | 109.5 |
| O8—Pb2—O4 | 84.44 (12) | O5—C17—O6 | 121.2 (5) |
| O3ii—Pb2—O4 | 151.11 (11) | O5—C17—C18 | 121.1 (4) |
| O7—Pb2—O4 | 134.31 (11) | O6—C17—C18 | 117.7 (4) |
| O10—Pb2—O4 | 71.75 (10) | C19—C18—C23 | 119.4 (5) |
| O6—Pb2—O5 | 50.10 (10) | C19—C18—C17 | 120.4 (5) |
| O8—Pb2—O5 | 70.96 (12) | C23—C18—C17 | 120.2 (5) |
| O3ii—Pb2—O5 | 117.25 (10) | C18—C19—C20 | 121.8 (6) |
| O7—Pb2—O5 | 103.86 (11) | C18—C19—H19A | 119.1 |
| O10—Pb2—O5 | 73.13 (11) | C20—C19—H19A | 119.1 |
| O4—Pb2—O5 | 65.60 (10) | C19—C20—C21 | 118.0 (6) |
| C1—O1—Pb1 | 98.1 (3) | C19—C20—C24 | 120.8 (6) |
| C1—O2—Pb1 | 88.9 (3) | C21—C20—C24 | 121.2 (6) |
| C9—O3—Pb2i | 159.3 (3) | C20—C21—C22 | 121.2 (6) |
| C9—O3—Pb1 | 89.5 (3) | C20—C21—H21A | 119.4 |
| Pb2i—O3—Pb1 | 110.94 (12) | C22—C21—H21A | 119.4 |
| C9—O4—Pb1 | 99.2 (3) | C23—C22—C21 | 119.9 (6) |
| C9—O4—Pb2 | 133.5 (3) | C23—C22—H22A | 120.1 |
| Pb1—O4—Pb2 | 114.63 (13) | C21—C22—H22A | 120.1 |
| C17—O5—Pb1 | 169.4 (3) | C22—C23—C18 | 119.8 (6) |
| C17—O5—Pb2 | 84.1 (3) | C22—C23—H23A | 120.1 |
| Pb1—O5—Pb2 | 106.44 (12) | C18—C23—H23A | 120.1 |
| C17—O6—Pb2 | 103.8 (3) | C20—C24—H24A | 109.5 |
| C17—O6—Pb1ii | 133.6 (3) | C20—C24—H24B | 109.5 |
| Pb2—O6—Pb1ii | 112.57 (13) | H24A—C24—H24B | 109.5 |
| C25—O7—Pb2 | 91.9 (3) | C20—C24—H24C | 109.5 |
| C25—O8—Pb2 | 95.2 (3) | H24A—C24—H24C | 109.5 |
| Pb1—O9—H9A | 109.2 | H24B—C24—H24C | 109.5 |
| Pb1—O9—H9B | 93.9 | O7—C25—O8 | 121.1 (5) |
| H9A—O9—H9B | 123.4 | O7—C25—C26 | 119.8 (5) |
| Pb2—O10—H10B | 109.3 | O8—C25—C26 | 119.1 (5) |
| Pb2—O10—H10A | 101.0 | C31—C26—C27 | 119.0 (6) |
| H10B—O10—H10A | 103.9 | C31—C26—C25 | 121.1 (6) |
| O2—C1—O1 | 121.4 (5) | C27—C26—C25 | 119.8 (5) |
| O2—C1—C2 | 120.1 (5) | C28—C27—C26 | 121.3 (6) |
| O1—C1—C2 | 118.5 (5) | C28—C27—H27A | 119.4 |
| C3—C2—C7 | 118.7 (5) | C26—C27—H27A | 119.4 |
| C3—C2—C1 | 120.7 (5) | C29—C28—C27 | 117.9 (7) |
| C7—C2—C1 | 120.6 (5) | C29—C28—C32 | 120.4 (7) |
| C2—C3—C4 | 122.1 (5) | C27—C28—C32 | 121.7 (7) |
| C2—C3—H3A | 118.9 | C30—C29—C28 | 121.5 (7) |
| C4—C3—H3A | 118.9 | C30—C29—H29A | 119.2 |
| C5—C4—C3 | 117.5 (5) | C28—C29—H29A | 119.2 |
| C5—C4—C8 | 121.8 (6) | C29—C30—C31 | 120.2 (8) |
| C3—C4—C8 | 120.7 (5) | C29—C30—H30A | 119.9 |
| C6—C5—C4 | 121.7 (6) | C31—C30—H30A | 119.9 |
| C6—C5—H5A | 119.1 | C26—C31—C30 | 120.0 (7) |
| C4—C5—H5A | 119.1 | C26—C31—H31A | 120.0 |
| C5—C6—C7 | 120.7 (5) | C30—C31—H31A | 120.0 |
| C5—C6—H6A | 119.6 | C28—C32—H32A | 109.5 |
| C7—C6—H6A | 119.6 | C28—C32—H32B | 109.5 |
| C6—C7—C2 | 119.3 (5) | H32A—C32—H32B | 109.5 |
| C6—C7—H7A | 120.4 | C28—C32—H32C | 109.5 |
| C2—C7—H7A | 120.4 | H32A—C32—H32C | 109.5 |
| C4—C8—H8A | 109.5 | H32B—C32—H32C | 109.5 |
| H··· | ||||
| O9—H9A···O8 | 0.82 | 2.03 | 2.805 (5) | 158 |
| O9—H9B···O7i | 0.82 | 2.25 | 3.017 (5) | 156 |
| O10—H10B···O2 | 0.82 | 2.12 | 2.881 (5) | 153 |
| O10—H10A···O1ii | 0.82 | 1.97 | 2.774 (5) | 166 |
Selected bond lengths (Å)
| Pb1—O4 | 2.386 (3) |
| Pb1—O1 | 2.424 (3) |
| Pb1—O3 | 2.594 (3) |
| Pb1—O5 | 2.603 (3) |
| Pb1—O2 | 2.622 (4) |
| Pb1—O9 | 2.724 (4) |
| Pb1—O6i | 2.751 (3) |
| Pb2—O6 | 2.325 (3) |
| Pb2—O8 | 2.494 (4) |
| Pb2—O3ii | 2.538 (3) |
| Pb2—O7 | 2.565 (4) |
| Pb2—O10 | 2.665 (3) |
| Pb2—O4 | 2.712 (3) |
| Pb2—O5 | 2.757 (4) |
Symmetry codes: (i) ; (ii) .
Hydrogen-bond geometry (Å, °)
| H⋯ | ||||
|---|---|---|---|---|
| O9—H9 | 0.82 | 2.03 | 2.805 (5) | 158 |
| O9—H9 | 0.82 | 2.25 | 3.017 (5) | 156 |
| O10—H10 | 0.82 | 2.12 | 2.881 (5) | 153 |
| O10—H10 | 0.82 | 1.97 | 2.774 (5) | 166 |
Symmetry codes: (i) ; (ii) .