| Literature DB >> 21587457 |
Ryan K Golder1, Christopher M Fitchett, Jan L Wikaira, Peter J Steel.
Abstract
Reaction of 4-amino-pyridine with silver(I) perchlorate leads to a one-dimensional coordination polymer, {[Ag(C(5)H(6)N(2))]ClO(4)}(n), in which the amino-pyridine binds through both N atoms. The perchlorate anion is hydrogen bonded to the amino H atoms and inter-acts weakly with the silver(I) atoms (Ag-O > 2.70 Å), both located on inversion centres, and some aromatic H atoms (O-H > 2.55 ÅA), thereby extending the dimensionality of the assembly. This is the first silver complex in which this ligand acts in a bridging mode.Entities:
Year: 2010 PMID: 21587457 PMCID: PMC2983413 DOI: 10.1107/S1600536810037682
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Ag(C5H6N2)]ClO4 | |
| Triclinic, | |
| Hall symbol: -P 1 | Mo |
| Cell parameters from 6232 reflections | |
| θ = 3.0–26.4° | |
| µ = 2.67 mm−1 | |
| α = 93.198 (2)° | |
| β = 96.992 (2)° | Prism, orange |
| γ = 100.452 (2)° | 0.35 × 0.11 × 0.05 mm |
| Bruker APEXII CCD diffractometer | 1740 independent reflections |
| Radiation source: fine-focus sealed tube | 1591 reflections with |
| graphite | |
| φ and ω scans | θmax = 26.4°, θmin = 2.3° |
| Absorption correction: multi-scan ( | |
| 9107 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 | |
| 1740 reflections | (Δ/σ)max = 0.017 |
| 127 parameters | Δρmax = 0.57 e Å−3 |
| 0 restraints | Δρmin = −0.78 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 | 0.0000 | 0.0000 | 0.5000 | 0.02748 (9) | |
| Ag2 | 0.5000 | −0.5000 | 0.0000 | 0.02716 (9) | |
| Cl1 | −0.04375 (9) | −0.70217 (6) | 0.19452 (5) | 0.02471 (12) | |
| O1 | −0.0156 (4) | −0.81713 (18) | 0.08849 (17) | 0.0372 (4) | |
| O2 | 0.0718 (4) | −0.7384 (2) | 0.32954 (17) | 0.0405 (4) | |
| O3 | 0.0969 (3) | −0.55690 (18) | 0.16137 (19) | 0.0338 (4) | |
| O4 | −0.3233 (3) | −0.6953 (2) | 0.1977 (2) | 0.0530 (6) | |
| N1 | 0.2684 (3) | −0.10407 (19) | 0.38878 (18) | 0.0212 (3) | |
| C2 | 0.3565 (4) | −0.2298 (2) | 0.4306 (2) | 0.0253 (4) | |
| H2A | 0.3003 | −0.2710 | 0.5139 | 0.030* | |
| C3 | 0.5233 (4) | −0.3006 (2) | 0.3584 (2) | 0.0245 (4) | |
| H3A | 0.5804 | −0.3886 | 0.3917 | 0.029* | |
| C4 | 0.6080 (4) | −0.2422 (2) | 0.2358 (2) | 0.0187 (4) | |
| C5 | 0.5244 (4) | −0.1101 (2) | 0.1946 (2) | 0.0224 (4) | |
| H5A | 0.5824 | −0.0647 | 0.1134 | 0.027* | |
| C6 | 0.3576 (4) | −0.0467 (2) | 0.2725 (2) | 0.0246 (4) | |
| H6A | 0.3017 | 0.0430 | 0.2427 | 0.030* | |
| N2 | 0.7619 (3) | −0.3164 (2) | 0.15325 (19) | 0.0218 (3) | |
| H2B | 0.874 (5) | −0.362 (3) | 0.199 (3) | 0.026* | |
| H2C | 0.845 (5) | −0.259 (3) | 0.097 (3) | 0.026* |
| Ag1 | 0.01995 (12) | 0.03359 (15) | 0.02912 (14) | 0.00871 (9) | 0.00516 (9) | −0.01157 (10) |
| Ag2 | 0.02874 (13) | 0.02542 (14) | 0.02684 (14) | 0.00551 (9) | 0.00580 (9) | −0.00782 (9) |
| Cl1 | 0.0227 (2) | 0.0299 (3) | 0.0266 (3) | 0.01105 (19) | 0.00968 (18) | 0.0130 (2) |
| O1 | 0.0491 (10) | 0.0312 (9) | 0.0296 (9) | 0.0013 (7) | 0.0083 (7) | 0.0022 (7) |
| O2 | 0.0520 (10) | 0.0550 (11) | 0.0238 (8) | 0.0281 (9) | 0.0100 (7) | 0.0138 (8) |
| O3 | 0.0347 (8) | 0.0259 (8) | 0.0473 (10) | 0.0105 (6) | 0.0211 (7) | 0.0102 (7) |
| O4 | 0.0238 (9) | 0.0665 (13) | 0.0815 (15) | 0.0196 (8) | 0.0229 (9) | 0.0445 (12) |
| N1 | 0.0193 (8) | 0.0232 (8) | 0.0211 (8) | 0.0061 (6) | 0.0032 (6) | −0.0055 (7) |
| C2 | 0.0309 (11) | 0.0270 (11) | 0.0197 (10) | 0.0059 (8) | 0.0089 (8) | 0.0023 (8) |
| C3 | 0.0322 (11) | 0.0224 (10) | 0.0225 (10) | 0.0112 (8) | 0.0075 (8) | 0.0045 (8) |
| C4 | 0.0167 (9) | 0.0202 (9) | 0.0183 (9) | 0.0031 (7) | 0.0015 (7) | −0.0025 (7) |
| C5 | 0.0276 (10) | 0.0207 (10) | 0.0204 (10) | 0.0058 (8) | 0.0063 (8) | 0.0037 (8) |
| C6 | 0.0270 (10) | 0.0209 (10) | 0.0269 (11) | 0.0088 (8) | 0.0020 (8) | 0.0000 (8) |
| N2 | 0.0212 (8) | 0.0233 (9) | 0.0227 (9) | 0.0069 (7) | 0.0072 (7) | 0.0004 (7) |
| Ag1—N1 | 2.1363 (16) | C2—H2A | 0.9500 |
| Ag1—N1i | 2.1363 (16) | C3—C4 | 1.393 (3) |
| Ag2—N2ii | 2.2582 (18) | C3—H3A | 0.9500 |
| Ag2—N2 | 2.2583 (18) | C4—C5 | 1.394 (3) |
| Cl1—O2 | 1.4301 (16) | C4—N2 | 1.399 (3) |
| Cl1—O4 | 1.4344 (16) | C5—C6 | 1.371 (3) |
| Cl1—O3 | 1.4430 (16) | C5—H5A | 0.9500 |
| Cl1—O1 | 1.4454 (17) | C6—H6A | 0.9500 |
| N1—C6 | 1.344 (3) | N2—H2B | 0.85 (3) |
| N1—C2 | 1.353 (3) | N2—H2C | 0.86 (3) |
| C2—C3 | 1.373 (3) | ||
| N1—Ag1—N1i | 180.00 (5) | C4—C3—H3A | 120.3 |
| N2ii—Ag2—N2 | 180.0 | C5—C4—C3 | 117.63 (18) |
| O2—Cl1—O4 | 109.54 (11) | C5—C4—N2 | 120.84 (18) |
| O2—Cl1—O3 | 109.91 (12) | C3—C4—N2 | 121.47 (18) |
| O4—Cl1—O3 | 108.88 (10) | C6—C5—C4 | 119.20 (19) |
| O2—Cl1—O1 | 108.65 (11) | C6—C5—H5A | 120.4 |
| O4—Cl1—O1 | 110.77 (13) | C4—C5—H5A | 120.4 |
| O3—Cl1—O1 | 109.08 (10) | N1—C6—C5 | 123.77 (19) |
| C6—N1—C2 | 116.76 (17) | N1—C6—H6A | 118.1 |
| C6—N1—Ag1 | 120.93 (13) | C5—C6—H6A | 118.1 |
| C2—N1—Ag1 | 122.31 (13) | C4—N2—Ag2 | 111.91 (12) |
| N1—C2—C3 | 123.15 (19) | C4—N2—H2B | 115.5 (17) |
| N1—C2—H2A | 118.4 | Ag2—N2—H2B | 104.1 (17) |
| C3—C2—H2A | 118.4 | C4—N2—H2C | 113.7 (17) |
| C2—C3—C4 | 119.45 (19) | Ag2—N2—H2C | 101.4 (17) |
| C2—C3—H3A | 120.3 | H2B—N2—H2C | 109 (2) |
| H··· | ||||
| N2—H2C···O1ii | 0.86 (3) | 2.16 (3) | 2.984 (3) | 161 (2) |
| N2—H2B···O3iii | 0.85 (3) | 2.29 (3) | 2.984 (3) | 139 (2) |
Hydrogen-bond geometry (Å, °)
| H⋯ | ||||
|---|---|---|---|---|
| N2—H2 | 0.86 (3) | 2.16 (3) | 2.984 (3) | 161 (2) |
| N2—H2 | 0.85 (3) | 2.29 (3) | 2.984 (3) | 139 (2) |
Symmetry codes: (i) ; (ii) .