| Literature DB >> 21588188 |
Gholamhossein Mohammadnezhad, Ali Reza Ghanbarpour, Mostafa M Amini, Seik Weng Ng.
Abstract
The dinuclear title compound, [Pb(2)(C(10)H(6)NO(2))(2)(CH(3)COO)(2)(CH(3)OH)(2)], lies across an inversion center. The methanol-coordinated Pb(II) atom is chelated by the acetate anion as well as by the quinoline-2-carboxyl-ate anion. One O atom of the quinoline-2-carboxyl-ate anion bridges two symmetry-related Pb(II) atoms, forming the dinuclear compound. Aside from the six atoms connected to the Pb(II) atom by regular coordination bonds, the structure features a long Pb⋯O inter-action [3.145 (3) Å] that gives rise to a distorted Ψ-square-anti-prismatic geometry at the metal center. The H atom of the methanol is hydrogen bonded to an O atom of the acetate.Entities:
Year: 2010 PMID: 21588188 PMCID: PMC3007209 DOI: 10.1107/S1600536810027777
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Pb2(C10H6NO2)2(C2H3O2)2(CH4O)2] | |
| Monoclinic, | Mo |
| Hall symbol: -P 2ybc | Cell parameters from 8885 reflections |
| θ = 2.6–28.3° | |
| µ = 11.91 mm−1 | |
| β = 90.397 (1)° | Block, colorless |
| 0.25 × 0.15 × 0.10 mm | |
| Bruker SMART APEX diffractometer | 3267 independent reflections |
| Radiation source: fine-focus sealed tube | 3055 reflections with |
| graphite | |
| ω scans | θmax = 27.5°, θmin = 1.8° |
| Absorption correction: multi-scan ( | |
| 13298 measured reflections |
| Refinement on | Primary atom site location: structure-invariant direct methods |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| Hydrogen site location: inferred from neighbouring sites | |
| H atoms treated by a mixture of independent and constrained refinement | |
| 3267 reflections | (Δ/σ)max = 0.001 |
| 186 parameters | Δρmax = 1.65 e Å−3 |
| 1 restraint | Δρmin = −1.43 e Å−3 |
| Pb1 | 0.271223 (16) | 0.534286 (15) | 0.449130 (5) | 0.01353 (5) | |
| O1 | 0.5946 (3) | 0.5505 (3) | 0.45723 (11) | 0.0199 (5) | |
| O2 | 0.8654 (3) | 0.6518 (3) | 0.43362 (11) | 0.0240 (6) | |
| O3 | 0.3648 (4) | 0.2628 (4) | 0.43453 (12) | 0.0313 (7) | |
| O4 | 0.1736 (4) | 0.3174 (3) | 0.36464 (12) | 0.0294 (6) | |
| O5 | 0.3561 (4) | 0.8211 (4) | 0.49639 (12) | 0.0284 (6) | |
| H5 | 0.454 (4) | 0.818 (7) | 0.515 (2) | 0.043* | |
| N1 | 0.4435 (4) | 0.6512 (3) | 0.35907 (12) | 0.0142 (5) | |
| C1 | 0.7022 (4) | 0.6278 (4) | 0.42410 (14) | 0.0158 (7) | |
| C2 | 0.6171 (4) | 0.6881 (4) | 0.36843 (14) | 0.0154 (6) | |
| C3 | 0.7256 (5) | 0.7731 (5) | 0.32939 (16) | 0.0212 (7) | |
| H3 | 0.8477 | 0.8020 | 0.3389 | 0.025* | |
| C4 | 0.6514 (5) | 0.8138 (5) | 0.27705 (17) | 0.0247 (8) | |
| H4 | 0.7230 | 0.8689 | 0.2495 | 0.030* | |
| C5 | 0.4697 (5) | 0.7735 (4) | 0.26467 (15) | 0.0185 (7) | |
| C6 | 0.3834 (5) | 0.8108 (5) | 0.21153 (16) | 0.0252 (8) | |
| H6 | 0.4512 | 0.8628 | 0.1823 | 0.030* | |
| C7 | 0.2051 (6) | 0.7731 (5) | 0.20205 (15) | 0.0251 (8) | |
| H7 | 0.1489 | 0.8001 | 0.1665 | 0.030* | |
| C8 | 0.1033 (5) | 0.6945 (5) | 0.24449 (15) | 0.0238 (8) | |
| H8 | −0.0207 | 0.6672 | 0.2371 | 0.029* | |
| C9 | 0.1807 (5) | 0.6563 (5) | 0.29670 (15) | 0.0200 (7) | |
| H9 | 0.1099 | 0.6046 | 0.3253 | 0.024* | |
| C10 | 0.3661 (5) | 0.6944 (4) | 0.30758 (14) | 0.0152 (6) | |
| C11 | 0.2681 (5) | 0.2208 (5) | 0.39130 (15) | 0.0213 (7) | |
| C12 | 0.2797 (8) | 0.0481 (5) | 0.3721 (2) | 0.0366 (11) | |
| H12A | 0.1787 | 0.0246 | 0.3456 | 0.055* | |
| H12B | 0.2717 | −0.0229 | 0.4056 | 0.055* | |
| H12C | 0.3962 | 0.0302 | 0.3527 | 0.055* | |
| C13 | 0.2189 (7) | 0.8980 (7) | 0.5289 (2) | 0.0478 (13) | |
| H13A | 0.0984 | 0.8608 | 0.5160 | 0.072* | |
| H13B | 0.2276 | 1.0148 | 0.5237 | 0.072* | |
| H13C | 0.2356 | 0.8717 | 0.5696 | 0.072* |
| Pb1 | 0.00951 (7) | 0.01915 (8) | 0.01191 (7) | 0.00240 (5) | −0.00103 (4) | 0.00037 (5) |
| O1 | 0.0138 (12) | 0.0310 (15) | 0.0148 (12) | 0.0017 (10) | −0.0010 (9) | 0.0060 (10) |
| O2 | 0.0141 (12) | 0.0336 (15) | 0.0244 (13) | −0.0003 (11) | −0.0035 (10) | 0.0041 (11) |
| O3 | 0.0334 (16) | 0.0291 (15) | 0.0313 (15) | 0.0141 (13) | −0.0169 (12) | −0.0117 (12) |
| O4 | 0.0368 (16) | 0.0248 (14) | 0.0264 (14) | 0.0051 (13) | −0.0145 (12) | −0.0018 (12) |
| O5 | 0.0276 (15) | 0.0275 (14) | 0.0300 (15) | 0.0107 (12) | −0.0137 (12) | −0.0051 (12) |
| N1 | 0.0136 (13) | 0.0167 (14) | 0.0123 (13) | 0.0012 (11) | −0.0002 (10) | 0.0004 (11) |
| C1 | 0.0140 (15) | 0.0187 (17) | 0.0147 (15) | 0.0024 (13) | −0.0004 (12) | −0.0010 (13) |
| C2 | 0.0140 (15) | 0.0158 (16) | 0.0164 (16) | 0.0025 (13) | 0.0001 (12) | −0.0024 (13) |
| C3 | 0.0126 (16) | 0.0240 (18) | 0.0270 (19) | −0.0014 (14) | 0.0025 (14) | 0.0049 (15) |
| C4 | 0.0204 (18) | 0.0270 (19) | 0.0269 (19) | 0.0012 (16) | 0.0050 (15) | 0.0112 (16) |
| C5 | 0.0208 (17) | 0.0197 (17) | 0.0151 (16) | 0.0040 (14) | 0.0011 (13) | 0.0045 (13) |
| C6 | 0.029 (2) | 0.030 (2) | 0.0169 (17) | 0.0070 (17) | 0.0022 (15) | 0.0094 (15) |
| C7 | 0.028 (2) | 0.034 (2) | 0.0130 (17) | 0.0087 (17) | −0.0044 (14) | 0.0041 (15) |
| C8 | 0.0205 (18) | 0.033 (2) | 0.0176 (17) | 0.0043 (16) | −0.0045 (14) | −0.0012 (15) |
| C9 | 0.0181 (17) | 0.0249 (18) | 0.0171 (16) | 0.0017 (14) | −0.0004 (13) | 0.0005 (14) |
| C10 | 0.0163 (16) | 0.0159 (16) | 0.0135 (15) | 0.0049 (13) | 0.0007 (12) | −0.0016 (12) |
| C11 | 0.0220 (18) | 0.0237 (19) | 0.0182 (17) | 0.0009 (15) | −0.0047 (14) | 0.0001 (14) |
| C12 | 0.055 (3) | 0.023 (2) | 0.032 (2) | 0.0088 (19) | −0.012 (2) | −0.0055 (17) |
| C13 | 0.047 (3) | 0.047 (3) | 0.049 (3) | 0.022 (3) | −0.006 (2) | −0.013 (3) |
| Pb1—O1 | 2.377 (3) | C4—C5 | 1.400 (5) |
| Pb1—O1i | 2.490 (2) | C4—H4 | 0.9500 |
| Pb1—O2ii | 3.145 (3) | C5—C10 | 1.421 (5) |
| Pb1—O3 | 2.382 (3) | C5—C6 | 1.422 (5) |
| Pb1—O4 | 2.761 (3) | C6—C7 | 1.359 (6) |
| Pb1—O5 | 2.696 (3) | C6—H6 | 0.9500 |
| Pb1—N1 | 2.643 (3) | C7—C8 | 1.404 (5) |
| O1—C1 | 1.280 (4) | C7—H7 | 0.9500 |
| O2—C1 | 1.230 (4) | C8—C9 | 1.376 (5) |
| O3—C11 | 1.276 (4) | C8—H8 | 0.9500 |
| O4—C11 | 1.226 (4) | C9—C10 | 1.415 (5) |
| O5—C13 | 1.416 (6) | C9—H9 | 0.9500 |
| O5—H5 | 0.84 (4) | C11—C12 | 1.505 (5) |
| N1—C2 | 1.324 (4) | C12—H12A | 0.9800 |
| N1—C10 | 1.372 (4) | C12—H12B | 0.9800 |
| C1—C2 | 1.521 (5) | C12—H12C | 0.9800 |
| C2—C3 | 1.403 (5) | C13—H13A | 0.9800 |
| C3—C4 | 1.375 (5) | C13—H13B | 0.9800 |
| C3—H3 | 0.9500 | C13—H13C | 0.9800 |
| O1—Pb1—O3 | 77.17 (10) | C4—C3—H3 | 120.7 |
| O1—Pb1—O1i | 63.88 (10) | C2—C3—H3 | 120.7 |
| O3—Pb1—O1i | 75.27 (9) | C3—C4—C5 | 119.6 (3) |
| O1—Pb1—N1 | 64.02 (8) | C3—C4—H4 | 120.2 |
| O3—Pb1—N1 | 95.46 (10) | C5—C4—H4 | 120.2 |
| O1i—Pb1—N1 | 127.85 (8) | C4—C5—C10 | 118.4 (3) |
| O1—Pb1—O5 | 71.99 (9) | C4—C5—C6 | 122.9 (3) |
| O3—Pb1—O5 | 146.04 (8) | C10—C5—C6 | 118.6 (3) |
| O1i—Pb1—O5 | 78.63 (8) | C7—C6—C5 | 120.8 (4) |
| N1—Pb1—O5 | 83.70 (9) | C7—C6—H6 | 119.6 |
| O1—Pb1—O4 | 110.27 (9) | C5—C6—H6 | 119.6 |
| O3—Pb1—O4 | 49.71 (8) | C6—C7—C8 | 120.4 (3) |
| O1i—Pb1—O4 | 122.70 (8) | C6—C7—H7 | 119.8 |
| N1—Pb1—O4 | 78.17 (9) | C8—C7—H7 | 119.8 |
| O5—Pb1—O4 | 157.89 (8) | C9—C8—C7 | 120.9 (4) |
| O1—Pb1—O2i | 105.53 (7) | C9—C8—H8 | 119.5 |
| O3—Pb1—O2i | 76.37 (9) | C7—C8—H8 | 119.5 |
| O1i—Pb1—O2i | 42.37 (7) | C8—C9—C10 | 119.7 (3) |
| N1—Pb1—O2i | 168.31 (8) | C8—C9—H9 | 120.2 |
| O5—Pb1—O2i | 98.35 (8) | C10—C9—H9 | 120.2 |
| O4—Pb1—O2i | 101.97 (8) | N1—C10—C9 | 119.2 (3) |
| C1—O1—Pb1 | 126.7 (2) | N1—C10—C5 | 121.2 (3) |
| C1—O1—Pb1i | 115.5 (2) | C9—C10—C5 | 119.5 (3) |
| Pb1—O1—Pb1i | 116.12 (10) | O4—C11—O3 | 122.0 (4) |
| C11—O3—Pb1 | 102.3 (2) | O4—C11—C12 | 120.4 (3) |
| C11—O4—Pb1 | 85.6 (2) | O3—C11—C12 | 117.6 (3) |
| C13—O5—Pb1 | 117.1 (3) | C11—C12—H12A | 109.5 |
| C13—O5—H5 | 110 (4) | C11—C12—H12B | 109.5 |
| Pb1—O5—H5 | 112 (4) | H12A—C12—H12B | 109.5 |
| C2—N1—C10 | 118.3 (3) | C11—C12—H12C | 109.5 |
| C2—N1—Pb1 | 114.6 (2) | H12A—C12—H12C | 109.5 |
| C10—N1—Pb1 | 126.5 (2) | H12B—C12—H12C | 109.5 |
| O2—C1—O1 | 125.0 (3) | O5—C13—H13A | 109.5 |
| O2—C1—C2 | 119.5 (3) | O5—C13—H13B | 109.5 |
| O1—C1—C2 | 115.5 (3) | H13A—C13—H13B | 109.5 |
| N1—C2—C3 | 123.8 (3) | O5—C13—H13C | 109.5 |
| N1—C2—C1 | 116.9 (3) | H13A—C13—H13C | 109.5 |
| C3—C2—C1 | 119.3 (3) | H13B—C13—H13C | 109.5 |
| C4—C3—C2 | 118.6 (3) | ||
| O3—Pb1—O1—C1 | 116.0 (3) | O5—Pb1—N1—C10 | −110.9 (3) |
| O1i—Pb1—O1—C1 | −164.3 (3) | O4—Pb1—N1—C10 | 56.4 (3) |
| N1—Pb1—O1—C1 | 13.3 (3) | O2i—Pb1—N1—C10 | 148.3 (3) |
| O5—Pb1—O1—C1 | −78.4 (3) | Pb1—O1—C1—O2 | 169.7 (3) |
| O4—Pb1—O1—C1 | 78.3 (3) | Pb1i—O1—C1—O2 | 5.3 (4) |
| O2i—Pb1—O1—C1 | −172.3 (3) | Pb1—O1—C1—C2 | −12.1 (4) |
| O3—Pb1—O1—Pb1i | −79.70 (12) | Pb1i—O1—C1—C2 | −176.6 (2) |
| O1i—Pb1—O1—Pb1i | 0.0 | C10—N1—C2—C3 | 2.0 (5) |
| N1—Pb1—O1—Pb1i | 177.62 (15) | Pb1—N1—C2—C3 | −170.2 (3) |
| O5—Pb1—O1—Pb1i | 85.90 (12) | C10—N1—C2—C1 | −175.7 (3) |
| O4—Pb1—O1—Pb1i | −117.41 (11) | Pb1—N1—C2—C1 | 12.1 (4) |
| O2i—Pb1—O1—Pb1i | −8.01 (13) | O2—C1—C2—N1 | 176.4 (3) |
| O1—Pb1—O3—C11 | −134.9 (3) | O1—C1—C2—N1 | −1.8 (5) |
| O1i—Pb1—O3—C11 | 159.2 (3) | O2—C1—C2—C3 | −1.3 (5) |
| N1—Pb1—O3—C11 | −73.1 (3) | O1—C1—C2—C3 | −179.6 (3) |
| O5—Pb1—O3—C11 | −159.9 (2) | N1—C2—C3—C4 | −3.5 (6) |
| O4—Pb1—O3—C11 | −3.6 (2) | C1—C2—C3—C4 | 174.1 (3) |
| O2i—Pb1—O3—C11 | 115.4 (3) | C2—C3—C4—C5 | 1.7 (6) |
| O1—Pb1—O4—C11 | 55.1 (2) | C3—C4—C5—C10 | 1.4 (6) |
| O3—Pb1—O4—C11 | 3.7 (2) | C3—C4—C5—C6 | −179.8 (4) |
| O1i—Pb1—O4—C11 | −16.2 (3) | C4—C5—C6—C7 | −178.2 (4) |
| N1—Pb1—O4—C11 | 111.5 (2) | C10—C5—C6—C7 | 0.6 (6) |
| O5—Pb1—O4—C11 | 147.1 (3) | C5—C6—C7—C8 | −0.8 (6) |
| O2i—Pb1—O4—C11 | −56.6 (2) | C6—C7—C8—C9 | 1.0 (6) |
| O1—Pb1—O5—C13 | −157.6 (3) | C7—C8—C9—C10 | −1.0 (6) |
| O3—Pb1—O5—C13 | −131.9 (3) | C2—N1—C10—C9 | −180.0 (3) |
| O1i—Pb1—O5—C13 | −91.6 (3) | Pb1—N1—C10—C9 | −8.8 (4) |
| N1—Pb1—O5—C13 | 137.7 (3) | C2—N1—C10—C5 | 1.4 (5) |
| O4—Pb1—O5—C13 | 102.7 (4) | Pb1—N1—C10—C5 | 172.5 (2) |
| O2i—Pb1—O5—C13 | −53.9 (3) | C8—C9—C10—N1 | −177.9 (3) |
| O1—Pb1—N1—C2 | −12.5 (2) | C8—C9—C10—C5 | 0.8 (5) |
| O3—Pb1—N1—C2 | −85.3 (2) | C4—C5—C10—N1 | −3.0 (5) |
| O1i—Pb1—N1—C2 | −9.8 (3) | C6—C5—C10—N1 | 178.1 (3) |
| O5—Pb1—N1—C2 | 60.5 (2) | C4—C5—C10—C9 | 178.3 (3) |
| O4—Pb1—N1—C2 | −132.2 (2) | C6—C5—C10—C9 | −0.6 (5) |
| O2i—Pb1—N1—C2 | −40.3 (5) | Pb1—O4—C11—O3 | −6.2 (4) |
| O1—Pb1—N1—C10 | 176.1 (3) | Pb1—O4—C11—C12 | 176.4 (4) |
| O3—Pb1—N1—C10 | 103.2 (3) | Pb1—O3—C11—O4 | 7.4 (5) |
| O1i—Pb1—N1—C10 | 178.8 (2) | Pb1—O3—C11—C12 | −175.2 (3) |
| H··· | ||||
| O5—H5···O3i | 0.84 (4) | 1.89 (4) | 2.685 (4) | 158 (5) |
Selected bond lengths (Å)
| Pb1—O1 | 2.377 (3) |
| Pb1—O1i | 2.490 (2) |
| Pb1—O2ii | 3.145 (3) |
| Pb1—O3 | 2.382 (3) |
| Pb1—O4 | 2.761 (3) |
| Pb1—O5 | 2.696 (3) |
| Pb1—N1 | 2.643 (3) |
Symmetry codes: (i) ; (ii) .
Hydrogen-bond geometry (Å, °)
| H⋯ | ||||
|---|---|---|---|---|
| O5—H5⋯O3i | 0.84 (4) | 1.89 (4) | 2.685 (4) | 158 (5) |
Symmetry code: (i) .