| Literature DB >> 23125598 |
Abstract
In the title complex, [Ag(2)(C(12)H(8)N(2)O(4))(C(10)H(8)N(2))(2)]·2H(2)O, the Ag(I) ion is three-coordinated by two N atoms from a chelating 2,2'-bipyridine ligand and one N atom from an imide ligand in a Y-shaped fashion. The imide ligand and the complex lie on a twofold rotation axis. The ligand bridges two Ag(I) ions, forming a dinuclear complex. In the crystal, O-H⋯O hydrogen bonds link the lattice water mol-ecules and the complex mol-ecules into a ribbon-like structure along [001]. π-π inter-actions are observed between the pyridine rings [centroid-centroid distance = 3.8289 (14) Å].Entities:
Year: 2012 PMID: 23125598 PMCID: PMC3470154 DOI: 10.1107/S1600536812038640
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Ag2(C12H8N2O4)(C10H8N2)2]·2H2O | |
| Monoclinic, | Mo |
| Hall symbol: -C 2yc | Cell parameters from 2928 reflections |
| θ = 1.0–26.1° | |
| µ = 1.39 mm−1 | |
| β = 108.376 (1)° | Block, colorless |
| 0.24 × 0.22 × 0.21 mm | |
| Bruker APEXII CCD diffractometer | 2923 independent reflections |
| Radiation source: fine-focus sealed tube | 2588 reflections with |
| Graphite monochromator | |
| φ and ω scans | θmax = 26.1°, θmin = 2.2° |
| Absorption correction: multi-scan ( | |
| 7869 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 | |
| 2923 reflections | (Δ/σ)max = 0.002 |
| 214 parameters | Δρmax = 0.30 e Å−3 |
| 2 restraints | Δρmin = −0.32 e Å−3 |
| 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 |
| Ag1 | 0.301043 (8) | 0.57692 (2) | 0.020063 (9) | 0.02934 (7) | |
| C1 | 0.37168 (10) | 0.7372 (3) | 0.16827 (11) | 0.0247 (5) | |
| C2 | 0.43266 (10) | 0.8225 (3) | 0.21718 (11) | 0.0232 (4) | |
| H2 | 0.4254 | 0.9535 | 0.2282 | 0.028* | |
| C3 | 0.47747 (10) | 0.8155 (3) | 0.17171 (11) | 0.0241 (5) | |
| H3 | 0.4875 | 0.9436 | 0.1601 | 0.029* | |
| C4 | 0.43841 (10) | 0.7149 (3) | 0.10388 (11) | 0.0236 (4) | |
| C5 | 0.46134 (9) | 0.7102 (3) | 0.28753 (11) | 0.0229 (4) | |
| H5 | 0.4321 | 0.7026 | 0.3157 | 0.027* | |
| C6 | 0.47997 (9) | 0.5181 (3) | 0.26895 (11) | 0.0224 (4) | |
| H6 | 0.4646 | 0.4077 | 0.2829 | 0.027* | |
| C7 | 0.17622 (12) | 0.5344 (3) | 0.07607 (13) | 0.0352 (6) | |
| H11 | 0.2008 | 0.6046 | 0.1149 | 0.042* | |
| C8 | 0.11778 (13) | 0.4724 (4) | 0.07644 (15) | 0.0419 (6) | |
| H12 | 0.1026 | 0.5036 | 0.1140 | 0.050* | |
| C9 | 0.08256 (12) | 0.3642 (4) | 0.02055 (15) | 0.0437 (7) | |
| H13 | 0.0432 | 0.3190 | 0.0200 | 0.052* | |
| C10 | 0.10585 (11) | 0.3222 (3) | −0.03534 (14) | 0.0346 (5) | |
| H14 | 0.0826 | 0.2478 | −0.0735 | 0.041* | |
| C11 | 0.16472 (10) | 0.3932 (3) | −0.03348 (12) | 0.0248 (5) | |
| C12 | 0.19220 (10) | 0.3621 (3) | −0.09278 (12) | 0.0254 (5) | |
| C13 | 0.16013 (11) | 0.2632 (3) | −0.15462 (12) | 0.0308 (5) | |
| H17 | 0.1206 | 0.2113 | −0.1596 | 0.037* | |
| C14 | 0.18683 (12) | 0.2423 (4) | −0.20821 (13) | 0.0375 (6) | |
| H18 | 0.1655 | 0.1769 | −0.2499 | 0.045* | |
| C15 | 0.24567 (12) | 0.3190 (4) | −0.19984 (13) | 0.0376 (6) | |
| H19 | 0.2647 | 0.3071 | −0.2355 | 0.045* | |
| C16 | 0.27537 (11) | 0.4139 (3) | −0.13678 (13) | 0.0328 (5) | |
| H20 | 0.3151 | 0.4652 | −0.1307 | 0.039* | |
| N1 | 0.19911 (9) | 0.4976 (3) | 0.02200 (10) | 0.0282 (4) | |
| N2 | 0.25001 (8) | 0.4358 (2) | −0.08404 (10) | 0.0263 (4) | |
| N3 | 0.37858 (8) | 0.6828 (2) | 0.10383 (9) | 0.0239 (4) | |
| O1 | 0.32354 (7) | 0.7175 (2) | 0.18440 (8) | 0.0329 (4) | |
| O2 | 0.45990 (7) | 0.6671 (3) | 0.05599 (8) | 0.0349 (4) | |
| O1W | 0.43224 (10) | 0.5971 (3) | −0.09313 (10) | 0.0525 (5) | |
| H1A | 0.4321 (17) | 0.635 (5) | −0.0542 (13) | 0.079* | |
| H1B | 0.4609 (14) | 0.519 (4) | −0.0847 (19) | 0.079* |
| Ag1 | 0.02316 (10) | 0.03214 (11) | 0.02658 (10) | −0.00518 (7) | −0.00091 (7) | 0.00260 (7) |
| C1 | 0.0213 (11) | 0.0274 (11) | 0.0226 (11) | 0.0055 (9) | 0.0029 (9) | 0.0072 (9) |
| C2 | 0.0231 (10) | 0.0225 (11) | 0.0217 (11) | 0.0036 (9) | 0.0036 (9) | 0.0005 (9) |
| C3 | 0.0217 (10) | 0.0265 (11) | 0.0217 (11) | −0.0047 (9) | 0.0035 (9) | 0.0031 (9) |
| C4 | 0.0239 (11) | 0.0263 (11) | 0.0187 (10) | −0.0007 (9) | 0.0039 (9) | 0.0054 (9) |
| C5 | 0.0185 (10) | 0.0311 (11) | 0.0185 (10) | 0.0023 (9) | 0.0051 (8) | 0.0007 (9) |
| C6 | 0.0194 (10) | 0.0236 (10) | 0.0197 (11) | −0.0024 (9) | −0.0002 (8) | 0.0025 (9) |
| C7 | 0.0360 (13) | 0.0386 (14) | 0.0319 (13) | 0.0003 (11) | 0.0119 (11) | 0.0047 (11) |
| C8 | 0.0434 (15) | 0.0446 (15) | 0.0464 (16) | 0.0039 (12) | 0.0265 (13) | 0.0081 (13) |
| C9 | 0.0305 (13) | 0.0442 (15) | 0.0609 (18) | −0.0012 (12) | 0.0209 (13) | 0.0115 (14) |
| C10 | 0.0236 (11) | 0.0329 (13) | 0.0448 (15) | −0.0022 (10) | 0.0075 (11) | 0.0057 (11) |
| C11 | 0.0213 (11) | 0.0225 (11) | 0.0272 (12) | 0.0007 (9) | 0.0029 (9) | 0.0070 (9) |
| C12 | 0.0217 (10) | 0.0220 (10) | 0.0286 (12) | 0.0022 (9) | 0.0024 (9) | 0.0068 (9) |
| C13 | 0.0263 (12) | 0.0278 (12) | 0.0333 (13) | −0.0018 (10) | 0.0021 (10) | 0.0034 (10) |
| C14 | 0.0417 (14) | 0.0345 (13) | 0.0311 (13) | 0.0000 (11) | 0.0042 (11) | −0.0043 (11) |
| C15 | 0.0434 (14) | 0.0402 (14) | 0.0297 (13) | 0.0053 (12) | 0.0124 (11) | 0.0003 (11) |
| C16 | 0.0276 (12) | 0.0361 (13) | 0.0349 (13) | −0.0011 (10) | 0.0102 (10) | 0.0036 (11) |
| N1 | 0.0256 (10) | 0.0296 (10) | 0.0285 (11) | −0.0012 (8) | 0.0071 (8) | 0.0045 (8) |
| N2 | 0.0215 (9) | 0.0280 (10) | 0.0264 (10) | −0.0010 (8) | 0.0034 (8) | 0.0027 (8) |
| N3 | 0.0208 (9) | 0.0278 (10) | 0.0202 (9) | −0.0011 (8) | 0.0024 (7) | 0.0031 (7) |
| O1 | 0.0215 (8) | 0.0475 (10) | 0.0298 (8) | 0.0024 (7) | 0.0081 (7) | 0.0030 (8) |
| O2 | 0.0268 (8) | 0.0563 (11) | 0.0216 (8) | −0.0040 (8) | 0.0076 (7) | −0.0017 (8) |
| O1W | 0.0568 (13) | 0.0680 (14) | 0.0300 (10) | 0.0172 (11) | 0.0099 (10) | −0.0080 (10) |
| Ag1—N3 | 2.1123 (17) | C7—H11 | 0.9300 |
| Ag1—N2 | 2.2380 (18) | C8—C9 | 1.367 (4) |
| Ag1—N1 | 2.3510 (18) | C8—H12 | 0.9300 |
| Ag1—Ag1i | 3.2716 (4) | C9—C10 | 1.386 (4) |
| C1—O1 | 1.218 (2) | C9—H13 | 0.9300 |
| C1—N3 | 1.377 (3) | C10—C11 | 1.394 (3) |
| C1—C2 | 1.520 (3) | C10—H14 | 0.9300 |
| C2—C3 | 1.535 (3) | C11—N1 | 1.341 (3) |
| C2—C5 | 1.548 (3) | C11—C12 | 1.493 (3) |
| C2—H2 | 0.9800 | C12—N2 | 1.350 (3) |
| C3—C4 | 1.520 (3) | C12—C13 | 1.390 (3) |
| C3—C5ii | 1.539 (3) | C13—C14 | 1.370 (3) |
| C3—H3 | 0.9800 | C13—H17 | 0.9300 |
| C4—O2 | 1.230 (3) | C14—C15 | 1.380 (4) |
| C4—N3 | 1.352 (3) | C14—H18 | 0.9300 |
| C5—C6 | 1.504 (3) | C15—C16 | 1.381 (3) |
| C5—C3ii | 1.539 (3) | C15—H19 | 0.9300 |
| C5—H5 | 0.9800 | C16—N2 | 1.336 (3) |
| C6—C6ii | 1.330 (4) | C16—H20 | 0.9300 |
| C6—H6 | 0.9300 | O1W—H1A | 0.81 (3) |
| C7—N1 | 1.340 (3) | O1W—H1B | 0.82 (3) |
| C7—C8 | 1.376 (3) | ||
| N3—Ag1—N2 | 157.77 (7) | C9—C8—H12 | 120.6 |
| N3—Ag1—N1 | 129.00 (7) | C7—C8—H12 | 120.6 |
| N2—Ag1—N1 | 72.09 (7) | C8—C9—C10 | 119.6 (2) |
| N3—Ag1—Ag1i | 104.80 (5) | C8—C9—H13 | 120.2 |
| N2—Ag1—Ag1i | 90.12 (5) | C10—C9—H13 | 120.2 |
| N1—Ag1—Ag1i | 65.33 (5) | C9—C10—C11 | 119.0 (2) |
| O1—C1—N3 | 124.7 (2) | C9—C10—H14 | 120.5 |
| O1—C1—C2 | 124.46 (19) | C11—C10—H14 | 120.5 |
| N3—C1—C2 | 110.86 (17) | N1—C11—C10 | 120.9 (2) |
| C1—C2—C3 | 103.58 (16) | N1—C11—C12 | 116.48 (18) |
| C1—C2—C5 | 113.16 (18) | C10—C11—C12 | 122.6 (2) |
| C3—C2—C5 | 109.94 (17) | N2—C12—C13 | 120.9 (2) |
| C1—C2—H2 | 110.0 | N2—C12—C11 | 116.92 (19) |
| C3—C2—H2 | 110.0 | C13—C12—C11 | 122.1 (2) |
| C5—C2—H2 | 110.0 | C14—C13—C12 | 119.9 (2) |
| C4—C3—C2 | 103.13 (16) | C14—C13—H17 | 120.1 |
| C4—C3—C5ii | 113.28 (18) | C12—C13—H17 | 120.1 |
| C2—C3—C5ii | 110.16 (16) | C13—C14—C15 | 119.4 (2) |
| C4—C3—H3 | 110.0 | C13—C14—H18 | 120.3 |
| C2—C3—H3 | 110.0 | C15—C14—H18 | 120.3 |
| C5ii—C3—H3 | 110.0 | C14—C15—C16 | 117.9 (2) |
| O2—C4—N3 | 125.1 (2) | C14—C15—H19 | 121.1 |
| O2—C4—C3 | 123.12 (19) | C16—C15—H19 | 121.1 |
| N3—C4—C3 | 111.81 (18) | N2—C16—C15 | 123.5 (2) |
| C6—C5—C3ii | 107.48 (16) | N2—C16—H20 | 118.3 |
| C6—C5—C2 | 108.60 (16) | C15—C16—H20 | 118.3 |
| C3ii—C5—C2 | 105.19 (17) | C7—N1—C11 | 119.3 (2) |
| C6—C5—H5 | 111.8 | C7—N1—Ag1 | 125.20 (16) |
| C3ii—C5—H5 | 111.8 | C11—N1—Ag1 | 115.26 (14) |
| C2—C5—H5 | 111.8 | C16—N2—C12 | 118.4 (2) |
| C6ii—C6—C5 | 114.88 (11) | C16—N2—Ag1 | 122.89 (15) |
| C6ii—C6—H6 | 122.6 | C12—N2—Ag1 | 118.63 (15) |
| C5—C6—H6 | 122.6 | C4—N3—C1 | 110.35 (17) |
| N1—C7—C8 | 122.6 (2) | C4—N3—Ag1 | 128.63 (14) |
| N1—C7—H11 | 118.7 | C1—N3—Ag1 | 120.98 (14) |
| C8—C7—H11 | 118.7 | H1A—O1W—H1B | 105 (4) |
| C9—C8—C7 | 118.7 (2) | ||
| O1—C1—C2—C3 | −179.7 (2) | C12—C11—N1—C7 | 178.35 (19) |
| N3—C1—C2—C3 | 1.2 (2) | C10—C11—N1—Ag1 | 174.03 (16) |
| O1—C1—C2—C5 | 61.3 (3) | C12—C11—N1—Ag1 | −7.3 (2) |
| N3—C1—C2—C5 | −117.83 (19) | N3—Ag1—N1—C7 | 9.0 (2) |
| C1—C2—C3—C4 | −3.7 (2) | N2—Ag1—N1—C7 | −179.1 (2) |
| C5—C2—C3—C4 | 117.52 (18) | Ag1i—Ag1—N1—C7 | −80.37 (18) |
| C1—C2—C3—C5ii | −124.88 (18) | N3—Ag1—N1—C11 | −164.88 (14) |
| C5—C2—C3—C5ii | −3.7 (2) | N2—Ag1—N1—C11 | 7.03 (15) |
| C2—C3—C4—O2 | −173.5 (2) | Ag1i—Ag1—N1—C11 | 105.71 (16) |
| C5ii—C3—C4—O2 | −54.5 (3) | C15—C16—N2—C12 | −0.2 (3) |
| C2—C3—C4—N3 | 5.4 (2) | C15—C16—N2—Ag1 | 176.70 (18) |
| C5ii—C3—C4—N3 | 124.47 (19) | C13—C12—N2—C16 | 1.0 (3) |
| C1—C2—C5—C6 | 64.1 (2) | C11—C12—N2—C16 | −178.63 (19) |
| C3—C2—C5—C6 | −51.2 (2) | C13—C12—N2—Ag1 | −176.10 (16) |
| C1—C2—C5—C3ii | 178.93 (17) | C11—C12—N2—Ag1 | 4.3 (2) |
| C3—C2—C5—C3ii | 63.66 (18) | N3—Ag1—N2—C16 | −19.6 (3) |
| C3ii—C5—C6—C6ii | −56.6 (3) | N1—Ag1—N2—C16 | 177.18 (19) |
| C2—C5—C6—C6ii | 56.7 (3) | Ag1i—Ag1—N2—C16 | 113.25 (17) |
| N1—C7—C8—C9 | 2.1 (4) | N3—Ag1—N2—C12 | 157.30 (17) |
| C7—C8—C9—C10 | −1.0 (4) | N1—Ag1—N2—C12 | −5.89 (15) |
| C8—C9—C10—C11 | −0.6 (4) | Ag1i—Ag1—N2—C12 | −69.82 (15) |
| C9—C10—C11—N1 | 1.2 (3) | O2—C4—N3—C1 | 174.0 (2) |
| C9—C10—C11—C12 | −177.3 (2) | C3—C4—N3—C1 | −4.9 (2) |
| N1—C11—C12—N2 | 2.3 (3) | O2—C4—N3—Ag1 | −8.5 (3) |
| C10—C11—C12—N2 | −179.1 (2) | C3—C4—N3—Ag1 | 172.56 (13) |
| N1—C11—C12—C13 | −177.2 (2) | O1—C1—N3—C4 | −176.8 (2) |
| C10—C11—C12—C13 | 1.4 (3) | C2—C1—N3—C4 | 2.3 (2) |
| N2—C12—C13—C14 | −1.1 (3) | O1—C1—N3—Ag1 | 5.4 (3) |
| C11—C12—C13—C14 | 178.5 (2) | C2—C1—N3—Ag1 | −175.45 (13) |
| C12—C13—C14—C15 | 0.4 (4) | N2—Ag1—N3—C4 | 15.3 (3) |
| C13—C14—C15—C16 | 0.3 (4) | N1—Ag1—N3—C4 | 174.54 (16) |
| C14—C15—C16—N2 | −0.4 (4) | Ag1i—Ag1—N3—C4 | −115.44 (17) |
| C8—C7—N1—C11 | −1.4 (4) | N2—Ag1—N3—C1 | −167.45 (16) |
| C8—C7—N1—Ag1 | −175.12 (18) | N1—Ag1—N3—C1 | −8.19 (19) |
| C10—C11—N1—C7 | −0.3 (3) | Ag1i—Ag1—N3—C1 | 61.83 (16) |
| H··· | ||||
| O1 | 0.81 (3) | 2.07 (2) | 2.839 (2) | 159 (3) |
| O1 | 0.82 (3) | 2.13 (3) | 2.952 (3) | 175 (2) |
Hydrogen-bond geometry (Å, °)
|
|
| H⋯ |
|
|
|---|---|---|---|---|
| O1 | 0.81 (3) | 2.07 (2) | 2.839 (2) | 159 (3) |
| O1 | 0.82 (3) | 2.13 (3) | 2.952 (3) | 175 (2) |
Symmetry code: (i) .