| Literature DB >> 22219756 |
Abstract
In the title compound, {[Ag(3)(C(10)H(8)N(2))(3)](ClO(4))(3)·2H(2)O}(n), one of the Ag(I) ions, one of the 4,4'-bipyridine (bipy) ligands and one of the perchlorate anions are each situated on a twofold rotation axis. Each Ag(I) ion is coordinated by two N atoms from two bridging bipy ligands, forming chains along [101]. π-π inter-actions between the pyridine rings [centroid-centroid distances = 3.638 (8) and 3.688 (8) Å] connect the chains. Inter-molecular O-H⋯O hydrogen bonds link the uncoord-inated water mol-ecules and the perchlorate anions.Entities:
Year: 2011 PMID: 22219756 PMCID: PMC3246936 DOI: 10.1107/S1600536811040153
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Ag3(C10H8N2)3](ClO4)3·2H2O | |
| Monoclinic, | Mo |
| Hall symbol: -C 2yc | Cell parameters from 2263 reflections |
| θ = 3.1–29.0° | |
| µ = 1.90 mm−1 | |
| β = 148.768 (5)° | Block, colorless |
| 0.21 × 0.20 × 0.19 mm | |
| Bruker APEXII CCD diffractometer | 3145 independent reflections |
| Radiation source: fine-focus sealed tube | 2229 reflections with |
| graphite | |
| φ and ω scans | θmax = 25.0°, θmin = 3.2° |
| Absorption correction: multi-scan ( | |
| 7095 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-atom parameters constrained | |
| 3145 reflections | (Δ/σ)max = 0.001 |
| 254 parameters | Δρmax = 1.87 e Å−3 |
| 0 restraints | Δρmin = −1.07 e Å−3 |
| Ag1 | 0.0000 | 0.45375 (5) | −0.2500 | 0.0566 (3) | |
| Ag2 | 0.59795 (4) | 0.05250 (4) | 0.68999 (4) | 0.0558 (3) | |
| O1 | 0.9612 (11) | 0.3396 (11) | 0.2576 (10) | 0.320 (11) | |
| O2 | 1.0878 (12) | 0.2447 (7) | 0.3549 (11) | 0.225 (6) | |
| O3 | 0.2999 (8) | 0.2382 (7) | 0.1888 (9) | 0.183 (5) | |
| O4 | 0.4471 (17) | 0.2642 (6) | 0.3825 (14) | 0.279 (8) | |
| O5 | 0.4822 (10) | 0.2063 (8) | 0.3197 (13) | 0.240 (6) | |
| O6 | 0.3993 (6) | 0.1309 (6) | 0.3237 (6) | 0.147 (3) | |
| O1W | 0.1272 (4) | 0.2966 (4) | 0.1401 (5) | 0.0789 (16) | |
| H1WB | 0.0798 | 0.2751 | 0.0713 | 0.118* | |
| H1WA | 0.2000 | 0.2788 | 0.2016 | 0.118* | |
| N1 | 0.1878 (5) | 0.4546 (3) | −0.0596 (5) | 0.0465 (14) | |
| N2 | 0.4098 (5) | 0.0531 (3) | 0.4983 (5) | 0.0404 (12) | |
| N3 | −0.2117 (4) | 0.0492 (3) | −0.1224 (5) | 0.0410 (13) | |
| C1 | 0.2488 (6) | 0.5264 (4) | −0.0009 (6) | 0.0390 (14) | |
| H1 | 0.2081 | 0.5774 | −0.0424 | 0.047* | |
| C2 | 0.3715 (6) | 0.5285 (4) | 0.1205 (6) | 0.0386 (14) | |
| H2 | 0.4115 | 0.5803 | 0.1582 | 0.046* | |
| C3 | 0.4347 (5) | 0.4539 (4) | 0.1856 (5) | 0.0318 (13) | |
| C4 | 0.3680 (6) | 0.3788 (4) | 0.1220 (7) | 0.0522 (17) | |
| H4 | 0.4053 | 0.3266 | 0.1612 | 0.063* | |
| C5 | 0.2469 (6) | 0.3825 (5) | 0.0010 (6) | 0.0560 (19) | |
| H5 | 0.2044 | 0.3319 | −0.0402 | 0.067* | |
| C6 | 0.3549 (6) | −0.0171 (4) | 0.4321 (6) | 0.0480 (16) | |
| H6 | 0.3989 | −0.0675 | 0.4706 | 0.058* | |
| C7 | 0.2379 (5) | −0.0197 (4) | 0.3112 (5) | 0.0459 (16) | |
| H7 | 0.2051 | −0.0703 | 0.2679 | 0.055* | |
| C8 | 0.1676 (5) | 0.0518 (3) | 0.2521 (5) | 0.0295 (13) | |
| C9 | 0.2230 (6) | 0.1252 (4) | 0.3215 (6) | 0.0461 (16) | |
| H9 | 0.1792 | 0.1755 | 0.2862 | 0.055* | |
| C10 | 0.3441 (6) | 0.1232 (4) | 0.4441 (6) | 0.0524 (17) | |
| H10 | 0.3805 | 0.1729 | 0.4900 | 0.063* | |
| C11 | 0.0359 (5) | 0.0509 (3) | 0.1213 (5) | 0.0279 (12) | |
| C12 | −0.0267 (5) | −0.0238 (4) | 0.0584 (5) | 0.0318 (13) | |
| H12 | 0.0135 | −0.0754 | 0.0971 | 0.038* | |
| C13 | −0.1494 (5) | −0.0225 (4) | −0.0625 (5) | 0.0382 (14) | |
| H13 | −0.1898 | −0.0737 | −0.1032 | 0.046* | |
| C14 | −0.1510 (6) | 0.1215 (4) | −0.0627 (6) | 0.0534 (18) | |
| H14 | −0.1926 | 0.1725 | −0.1033 | 0.064* | |
| C15 | −0.0293 (5) | 0.1237 (4) | 0.0570 (6) | 0.0490 (17) | |
| H15 | 0.0094 | 0.1759 | 0.0948 | 0.059* | |
| Cl1 | 1.0000 | 0.28764 (14) | 0.2500 | 0.0493 (6) | |
| Cl2 | 0.41235 (16) | 0.21081 (11) | 0.30907 (16) | 0.0539 (5) |
| Ag1 | 0.0280 (4) | 0.0644 (6) | 0.0340 (5) | 0.000 | 0.0197 (4) | 0.000 |
| Ag2 | 0.0251 (3) | 0.0706 (5) | 0.0256 (3) | 0.0006 (2) | 0.0144 (3) | 0.0007 (2) |
| O1 | 0.233 (13) | 0.47 (2) | 0.132 (8) | 0.233 (16) | 0.137 (10) | 0.076 (12) |
| O2 | 0.310 (15) | 0.146 (9) | 0.195 (10) | 0.143 (9) | 0.212 (11) | 0.116 (7) |
| O3 | 0.136 (6) | 0.223 (12) | 0.165 (8) | 0.107 (8) | 0.125 (7) | 0.141 (8) |
| O4 | 0.51 (2) | 0.090 (7) | 0.279 (15) | −0.072 (11) | 0.343 (19) | −0.066 (9) |
| O5 | 0.218 (9) | 0.225 (13) | 0.388 (15) | 0.090 (10) | 0.277 (12) | 0.107 (12) |
| O6 | 0.101 (5) | 0.110 (7) | 0.090 (5) | −0.024 (5) | 0.060 (5) | 0.013 (4) |
| O1W | 0.069 (3) | 0.069 (4) | 0.076 (4) | 0.002 (3) | 0.058 (3) | 0.003 (3) |
| N1 | 0.033 (3) | 0.048 (4) | 0.035 (3) | 0.002 (2) | 0.025 (3) | 0.002 (3) |
| N2 | 0.027 (3) | 0.040 (3) | 0.032 (3) | 0.000 (2) | 0.022 (3) | 0.003 (2) |
| N3 | 0.017 (2) | 0.051 (4) | 0.020 (3) | 0.001 (2) | 0.010 (2) | 0.006 (2) |
| C1 | 0.037 (3) | 0.034 (3) | 0.039 (3) | −0.001 (3) | 0.032 (3) | −0.003 (3) |
| C2 | 0.042 (3) | 0.030 (3) | 0.038 (3) | 0.001 (3) | 0.033 (3) | −0.001 (3) |
| C3 | 0.027 (3) | 0.041 (4) | 0.030 (3) | 0.000 (2) | 0.024 (3) | 0.000 (3) |
| C4 | 0.040 (3) | 0.031 (4) | 0.051 (4) | 0.000 (3) | 0.033 (3) | 0.001 (3) |
| C5 | 0.043 (4) | 0.042 (4) | 0.043 (4) | −0.006 (4) | 0.030 (4) | −0.007 (4) |
| C6 | 0.035 (3) | 0.043 (4) | 0.034 (3) | 0.012 (3) | 0.024 (3) | 0.004 (3) |
| C7 | 0.032 (3) | 0.043 (4) | 0.027 (3) | 0.003 (3) | 0.019 (3) | −0.006 (3) |
| C8 | 0.023 (3) | 0.033 (3) | 0.023 (3) | −0.002 (2) | 0.018 (3) | 0.000 (2) |
| C9 | 0.038 (3) | 0.023 (3) | 0.039 (4) | −0.007 (3) | 0.027 (3) | −0.001 (3) |
| C10 | 0.034 (3) | 0.037 (4) | 0.037 (4) | −0.009 (3) | 0.022 (3) | −0.006 (3) |
| C11 | 0.022 (3) | 0.028 (3) | 0.019 (3) | −0.004 (2) | 0.015 (3) | −0.002 (2) |
| C12 | 0.024 (3) | 0.031 (3) | 0.029 (3) | 0.005 (2) | 0.020 (3) | 0.003 (3) |
| C13 | 0.026 (3) | 0.041 (3) | 0.022 (3) | −0.004 (3) | 0.017 (3) | −0.007 (3) |
| C14 | 0.029 (3) | 0.035 (4) | 0.027 (3) | 0.004 (3) | 0.013 (3) | 0.010 (3) |
| C15 | 0.036 (3) | 0.031 (4) | 0.029 (3) | −0.004 (3) | 0.020 (3) | 0.005 (3) |
| Cl1 | 0.0637 (15) | 0.0265 (11) | 0.0578 (15) | 0.000 | 0.0520 (14) | 0.000 |
| Cl2 | 0.0567 (11) | 0.0389 (9) | 0.0568 (11) | 0.0052 (8) | 0.0470 (10) | 0.0060 (8) |
| Ag1—N1 | 2.149 (6) | C3—C4 | 1.400 (8) |
| Ag1—N1i | 2.149 (6) | C3—C3iii | 1.475 (12) |
| Ag2—N3ii | 2.151 (5) | C4—C5 | 1.378 (10) |
| Ag2—N2 | 2.158 (6) | C4—H4 | 0.9300 |
| O1—Cl1 | 1.27 (3) | C5—H5 | 0.9300 |
| O2—Cl1 | 1.325 (9) | C6—C7 | 1.353 (8) |
| O3—Cl2 | 1.396 (8) | C6—H6 | 0.9300 |
| O4—Cl2 | 1.295 (10) | C7—C8 | 1.368 (8) |
| O5—Cl2 | 1.30 (3) | C7—H7 | 0.9300 |
| O6—Cl2 | 1.379 (8) | C8—C9 | 1.383 (8) |
| O1W—H1WB | 0.8500 | C8—C11 | 1.492 (8) |
| O1W—H1WA | 0.8500 | C9—C10 | 1.385 (9) |
| N1—C1 | 1.323 (8) | C9—H9 | 0.9300 |
| N1—C5 | 1.324 (9) | C10—H10 | 0.9300 |
| N2—C6 | 1.320 (8) | C11—C15 | 1.364 (8) |
| N2—C10 | 1.323 (8) | C11—C12 | 1.377 (8) |
| N3—C13 | 1.328 (8) | C12—C13 | 1.386 (7) |
| N3—C14 | 1.329 (8) | C12—H12 | 0.9300 |
| C1—C2 | 1.389 (9) | C13—H13 | 0.9300 |
| C1—H1 | 0.9300 | C14—C15 | 1.374 (8) |
| C2—C3 | 1.383 (8) | C14—H14 | 0.9300 |
| C2—H2 | 0.9300 | C15—H15 | 0.9300 |
| N1—Ag1—N1i | 179.3 (3) | C9—C8—C11 | 120.8 (5) |
| N3ii—Ag2—N2 | 176.36 (19) | C8—C9—C10 | 119.5 (6) |
| H1WB—O1W—H1WA | 115.0 | C8—C9—H9 | 120.3 |
| C1—N1—C5 | 118.1 (6) | C10—C9—H9 | 120.3 |
| C1—N1—Ag1 | 121.3 (4) | N2—C10—C9 | 122.4 (6) |
| C5—N1—Ag1 | 120.5 (5) | N2—C10—H10 | 118.8 |
| C6—N2—C10 | 117.6 (6) | C9—C10—H10 | 118.8 |
| C6—N2—Ag2 | 121.2 (4) | C15—C11—C12 | 116.1 (6) |
| C10—N2—Ag2 | 121.1 (4) | C15—C11—C8 | 122.1 (5) |
| C13—N3—C14 | 117.3 (5) | C12—C11—C8 | 121.7 (5) |
| C13—N3—Ag2iv | 123.0 (4) | C11—C12—C13 | 120.3 (6) |
| C14—N3—Ag2iv | 119.7 (4) | C11—C12—H12 | 119.9 |
| N1—C1—C2 | 122.4 (6) | C13—C12—H12 | 119.9 |
| N1—C1—H1 | 118.8 | N3—C13—C12 | 122.5 (6) |
| C2—C1—H1 | 118.8 | N3—C13—H13 | 118.7 |
| C3—C2—C1 | 120.4 (6) | C12—C13—H13 | 118.7 |
| C3—C2—H2 | 119.8 | N3—C14—C15 | 122.5 (6) |
| C1—C2—H2 | 119.8 | N3—C14—H14 | 118.8 |
| C2—C3—C4 | 116.2 (6) | C15—C14—H14 | 118.8 |
| C2—C3—C3iii | 121.7 (4) | C11—C15—C14 | 121.2 (6) |
| C4—C3—C3iii | 122.1 (4) | C11—C15—H15 | 119.4 |
| C5—C4—C3 | 119.6 (6) | C14—C15—H15 | 119.4 |
| C5—C4—H4 | 120.2 | O1v—Cl1—O1 | 99.3 (17) |
| C3—C4—H4 | 120.2 | O1v—Cl1—O2v | 105.5 (7) |
| N1—C5—C4 | 123.3 (6) | O1—Cl1—O2v | 113.2 (9) |
| N1—C5—H5 | 118.4 | O1v—Cl1—O2 | 113.2 (9) |
| C4—C5—H5 | 118.4 | O1—Cl1—O2 | 105.5 (7) |
| N2—C6—C7 | 123.4 (6) | O2v—Cl1—O2 | 118.6 (12) |
| N2—C6—H6 | 118.3 | O4—Cl2—O5 | 115.0 (10) |
| C7—C6—H6 | 118.3 | O4—Cl2—O6 | 110.4 (7) |
| C6—C7—C8 | 120.5 (6) | O5—Cl2—O6 | 109.2 (6) |
| C6—C7—H7 | 119.8 | O4—Cl2—O3 | 107.5 (9) |
| C8—C7—H7 | 119.8 | O5—Cl2—O3 | 105.6 (7) |
| C7—C8—C9 | 116.7 (6) | O6—Cl2—O3 | 108.9 (5) |
| C7—C8—C11 | 122.5 (5) | ||
| C5—N1—C1—C2 | 0.5 (10) | C6—N2—C10—C9 | −2.1 (10) |
| Ag1—N1—C1—C2 | −177.1 (4) | Ag2—N2—C10—C9 | −179.5 (5) |
| N1—C1—C2—C3 | −0.8 (9) | C8—C9—C10—N2 | −0.1 (10) |
| C1—C2—C3—C4 | 0.2 (9) | C7—C8—C11—C15 | −169.4 (6) |
| C1—C2—C3—C3iii | 179.6 (6) | C9—C8—C11—C15 | 14.1 (9) |
| C2—C3—C4—C5 | 0.8 (10) | C7—C8—C11—C12 | 10.0 (9) |
| C3iii—C3—C4—C5 | −178.7 (7) | C9—C8—C11—C12 | −166.5 (5) |
| C1—N1—C5—C4 | 0.5 (11) | C15—C11—C12—C13 | −1.4 (8) |
| Ag1—N1—C5—C4 | 178.1 (6) | C8—C11—C12—C13 | 179.1 (5) |
| C3—C4—C5—N1 | −1.1 (11) | C14—N3—C13—C12 | 1.3 (9) |
| C10—N2—C6—C7 | 4.0 (10) | Ag2iv—N3—C13—C12 | 179.9 (4) |
| Ag2—N2—C6—C7 | −178.7 (5) | C11—C12—C13—N3 | −0.1 (9) |
| N2—C6—C7—C8 | −3.6 (11) | C13—N3—C14—C15 | −1.0 (10) |
| C6—C7—C8—C9 | 1.2 (9) | Ag2iv—N3—C14—C15 | −179.7 (5) |
| C6—C7—C8—C11 | −175.4 (6) | C12—C11—C15—C14 | 1.7 (9) |
| C7—C8—C9—C10 | 0.5 (9) | C8—C11—C15—C14 | −178.8 (6) |
| C11—C8—C9—C10 | 177.2 (6) | N3—C14—C15—C11 | −0.5 (11) |
| H··· | ||||
| O1W—H1WB···O4vi | 0.85 | 2.21 | 3.060 (15) | 173 |
| O1W—H1WA···O3 | 0.85 | 2.44 | 2.99 (3) | 123 |
Hydrogen-bond geometry (Å, °)
| H⋯ | ||||
|---|---|---|---|---|
| O1 | 0.85 | 2.21 | 3.060 (15) | 173 |
| O1 | 0.85 | 2.44 | 2.99 (3) | 123 |
Symmetry code: (i) .