| Literature DB >> 21577472 |
Michael I Kahn, James A Golen, Arnold L Rheingold, Linda H Doerrer.
Abstract
The crystal structure of the title compound, [PtBr(C(15)H(11)N(3))][AuBr(2)]·(CH(3))(2)SO, exhibits infinite chains of {PtAuPt}(∞) metallophilic inter-actions along the b axis. Two cations and one anion stack in a trimer with a unique Pt⋯Au distance of 3.3361 (5) Å and Pt⋯Pt contacts of 3.4335 (6) Å. The remaining [AuBr(2)](-) anion forms no close contacts.Entities:
Year: 2009 PMID: 21577472 PMCID: PMC2970032 DOI: 10.1107/S1600536809033248
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [PtBr(C15H11N3)][AuBr2]·C2H6OS | |
| Triclinic, | |
| Hall symbol: -P 1 | Mo |
| Cell parameters from 5521 reflections | |
| θ = 2.5–28.2° | |
| µ = 19.31 mm−1 | |
| α = 81.905 (2)° | |
| β = 87.675 (2)° | Block, red |
| γ = 68.532 (3)° | 0.30 × 0.20 × 0.15 mm |
| Bruker SMART CCD area-detector diffractometer | 4826 independent reflections |
| Radiation source: fine-focus sealed tube | 4312 reflections with |
| graphite | |
| φ and ω scans | θmax = 28.2°, θmin = 1.5° |
| Absorption correction: multi-scan ( | |
| 7511 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 | |
| 4826 reflections | (Δ/σ)max = 0.001 |
| 249 parameters | Δρmax = 2.01 e Å−3 |
| 0 restraints | Δρmin = −4.13 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 |
| Au1 | 1.0000 | 0.5000 | 1.0000 | 0.03631 (12) | |
| Au2 | 0.5000 | 0.5000 | 0.5000 | 0.03754 (12) | |
| Pt1 | 0.01155 (3) | 0.82805 (2) | −0.005856 (15) | 0.02023 (9) | |
| Br1 | −0.25578 (8) | 0.87221 (7) | 0.08893 (5) | 0.03042 (15) | |
| Br2 | 0.98737 (9) | 0.44194 (7) | 1.17203 (6) | 0.03918 (18) | |
| Br3 | 0.75978 (12) | 0.32173 (10) | 0.45033 (6) | 0.0514 (2) | |
| S1 | 0.3410 (3) | 1.1786 (2) | 0.55776 (14) | 0.0477 (5) | |
| N1 | 0.1935 (6) | 0.7291 (5) | 0.1004 (4) | 0.0220 (10) | |
| N3 | −0.0990 (6) | 0.9177 (5) | −0.1372 (4) | 0.0212 (9) | |
| N2 | 0.2244 (6) | 0.7937 (5) | −0.0823 (4) | 0.0196 (9) | |
| O1 | 0.3110 (10) | 1.0395 (7) | 0.5756 (6) | 0.079 (2) | |
| C1 | 0.1657 (9) | 0.6989 (7) | 0.1947 (5) | 0.0292 (13) | |
| H1A | 0.0493 | 0.7257 | 0.2172 | 0.035* | |
| C2 | 0.3038 (10) | 0.6292 (8) | 0.2598 (5) | 0.0363 (15) | |
| H2A | 0.2809 | 0.6086 | 0.3256 | 0.044* | |
| C3 | 0.4751 (10) | 0.5900 (8) | 0.2277 (5) | 0.0356 (15) | |
| H3A | 0.5700 | 0.5420 | 0.2713 | 0.043* | |
| C4 | 0.5057 (9) | 0.6221 (7) | 0.1305 (5) | 0.0313 (14) | |
| H4A | 0.6216 | 0.5976 | 0.1072 | 0.038* | |
| C5 | 0.3634 (8) | 0.6908 (6) | 0.0682 (4) | 0.0239 (12) | |
| C6 | 0.3808 (8) | 0.7276 (7) | −0.0365 (5) | 0.0275 (13) | |
| C7 | 0.5327 (8) | 0.7028 (6) | −0.0895 (5) | 0.0274 (13) | |
| H7A | 0.6440 | 0.6568 | −0.0592 | 0.033* | |
| C8 | 0.5184 (8) | 0.7467 (7) | −0.1880 (5) | 0.0307 (14) | |
| H8A | 0.6215 | 0.7295 | −0.2249 | 0.037* | |
| C9 | 0.3560 (8) | 0.8153 (7) | −0.2337 (4) | 0.0270 (12) | |
| H9A | 0.3475 | 0.8453 | −0.3008 | 0.032* | |
| C10 | 0.2060 (8) | 0.8385 (6) | −0.1780 (4) | 0.0237 (12) | |
| C11 | 0.0209 (8) | 0.9105 (6) | −0.2094 (4) | 0.0241 (12) | |
| C12 | −0.0334 (9) | 0.9673 (7) | −0.3032 (5) | 0.0306 (14) | |
| H12A | 0.0508 | 0.9637 | −0.3519 | 0.037* | |
| C13 | −0.2089 (9) | 1.0288 (7) | −0.3261 (5) | 0.0344 (15) | |
| H13A | −0.2470 | 1.0662 | −0.3903 | 0.041* | |
| C14 | −0.3288 (9) | 1.0348 (8) | −0.2530 (5) | 0.0356 (15) | |
| H14A | −0.4502 | 1.0775 | −0.2672 | 0.043* | |
| C15 | −0.2725 (8) | 0.9788 (6) | −0.1592 (5) | 0.0270 (13) | |
| H15A | −0.3559 | 0.9833 | −0.1100 | 0.032* | |
| C16 | 0.2828 (11) | 1.2500 (9) | 0.4364 (5) | 0.0473 (19) | |
| H16A | 0.3572 | 1.1838 | 0.3945 | 0.071* | |
| H16B | 0.2987 | 1.3414 | 0.4222 | 0.071* | |
| H16C | 0.1603 | 1.2642 | 0.4255 | 0.071* | |
| C17 | 0.1620 (13) | 1.3074 (11) | 0.6114 (7) | 0.063 (3) | |
| H17A | 0.1799 | 1.2924 | 0.6809 | 0.094* | |
| H17B | 0.0525 | 1.2965 | 0.5969 | 0.094* | |
| H17C | 0.1560 | 1.4035 | 0.5856 | 0.094* |
| Au1 | 0.02295 (18) | 0.0324 (2) | 0.0533 (3) | −0.00747 (15) | −0.00103 (16) | −0.01197 (17) |
| Au2 | 0.0434 (2) | 0.0484 (2) | 0.0243 (2) | −0.02176 (18) | −0.00643 (16) | 0.00001 (16) |
| Pt1 | 0.01865 (13) | 0.02448 (13) | 0.01805 (14) | −0.00871 (9) | 0.00074 (9) | −0.00222 (9) |
| Br1 | 0.0254 (3) | 0.0345 (3) | 0.0311 (3) | −0.0109 (3) | 0.0069 (2) | −0.0054 (3) |
| Br2 | 0.0306 (3) | 0.0323 (3) | 0.0542 (5) | −0.0095 (3) | −0.0011 (3) | −0.0097 (3) |
| Br3 | 0.0499 (5) | 0.0579 (5) | 0.0436 (5) | −0.0160 (4) | −0.0025 (4) | −0.0072 (4) |
| S1 | 0.0383 (9) | 0.0678 (13) | 0.0308 (10) | −0.0188 (9) | −0.0043 (8) | 0.0137 (9) |
| N1 | 0.021 (2) | 0.027 (2) | 0.019 (2) | −0.0096 (19) | −0.0004 (19) | −0.0027 (19) |
| N3 | 0.017 (2) | 0.022 (2) | 0.022 (2) | −0.0041 (18) | −0.0033 (18) | −0.0013 (19) |
| N2 | 0.018 (2) | 0.021 (2) | 0.020 (2) | −0.0077 (18) | 0.0020 (18) | −0.0030 (19) |
| O1 | 0.081 (5) | 0.057 (4) | 0.079 (5) | −0.020 (4) | 0.013 (4) | 0.033 (4) |
| C1 | 0.034 (3) | 0.035 (3) | 0.021 (3) | −0.017 (3) | 0.003 (3) | −0.002 (3) |
| C2 | 0.042 (4) | 0.045 (4) | 0.023 (3) | −0.020 (3) | −0.001 (3) | 0.005 (3) |
| C3 | 0.039 (4) | 0.038 (4) | 0.029 (4) | −0.015 (3) | −0.012 (3) | 0.006 (3) |
| C4 | 0.030 (3) | 0.034 (3) | 0.032 (4) | −0.013 (3) | −0.004 (3) | −0.004 (3) |
| C5 | 0.023 (3) | 0.025 (3) | 0.024 (3) | −0.011 (2) | 0.000 (2) | −0.001 (2) |
| C6 | 0.024 (3) | 0.030 (3) | 0.028 (3) | −0.010 (2) | −0.001 (2) | −0.003 (3) |
| C7 | 0.023 (3) | 0.029 (3) | 0.029 (3) | −0.008 (2) | −0.002 (2) | −0.004 (3) |
| C8 | 0.024 (3) | 0.036 (3) | 0.032 (4) | −0.011 (3) | 0.007 (3) | −0.005 (3) |
| C9 | 0.027 (3) | 0.035 (3) | 0.020 (3) | −0.013 (3) | 0.002 (2) | −0.002 (2) |
| C10 | 0.025 (3) | 0.023 (3) | 0.025 (3) | −0.010 (2) | 0.001 (2) | −0.003 (2) |
| C11 | 0.022 (3) | 0.026 (3) | 0.025 (3) | −0.008 (2) | −0.001 (2) | −0.007 (2) |
| C12 | 0.036 (3) | 0.029 (3) | 0.026 (3) | −0.013 (3) | −0.003 (3) | 0.001 (3) |
| C13 | 0.035 (3) | 0.036 (3) | 0.029 (4) | −0.010 (3) | −0.009 (3) | 0.001 (3) |
| C14 | 0.027 (3) | 0.042 (4) | 0.035 (4) | −0.010 (3) | −0.010 (3) | 0.002 (3) |
| C15 | 0.022 (3) | 0.030 (3) | 0.029 (3) | −0.009 (2) | −0.003 (2) | −0.003 (3) |
| C16 | 0.057 (5) | 0.060 (5) | 0.028 (4) | −0.025 (4) | 0.001 (3) | −0.001 (3) |
| C17 | 0.070 (6) | 0.084 (7) | 0.049 (5) | −0.040 (5) | 0.016 (5) | −0.025 (5) |
| Au1—Br2i | 2.3981 (9) | C4—H4A | 0.9400 |
| Au1—Br2 | 2.3981 (9) | C5—C6 | 1.471 (9) |
| Au2—Br3 | 2.3753 (9) | C6—C7 | 1.375 (9) |
| Au2—Br3ii | 2.3753 (9) | C7—C8 | 1.381 (9) |
| Pt1—N2 | 1.944 (5) | C7—H7A | 0.9400 |
| Pt1—N3 | 2.015 (5) | C8—C9 | 1.383 (9) |
| Pt1—N1 | 2.018 (5) | C8—H8A | 0.9400 |
| Pt1—Br1 | 2.4320 (7) | C9—C10 | 1.385 (8) |
| S1—O1 | 1.497 (7) | C9—H9A | 0.9400 |
| S1—C16 | 1.757 (8) | C10—C11 | 1.468 (8) |
| S1—C17 | 1.782 (9) | C11—C12 | 1.376 (9) |
| N1—C1 | 1.338 (8) | C12—C13 | 1.365 (9) |
| N1—C5 | 1.369 (7) | C12—H12A | 0.9400 |
| N3—C15 | 1.348 (7) | C13—C14 | 1.376 (10) |
| N3—C11 | 1.366 (8) | C13—H13A | 0.9400 |
| N2—C6 | 1.342 (7) | C14—C15 | 1.376 (9) |
| N2—C10 | 1.345 (8) | C14—H14A | 0.9400 |
| C1—C2 | 1.382 (10) | C15—H15A | 0.9400 |
| C1—H1A | 0.9400 | C16—H16A | 0.9700 |
| C2—C3 | 1.379 (10) | C16—H16B | 0.9700 |
| C2—H2A | 0.9400 | C16—H16C | 0.9700 |
| C3—C4 | 1.385 (9) | C17—H17A | 0.9700 |
| C3—H3A | 0.9400 | C17—H17B | 0.9700 |
| C4—C5 | 1.380 (9) | C17—H17C | 0.9700 |
| Br2i—Au1—Br2 | 180.0 | C6—C7—H7A | 120.7 |
| Br3—Au2—Br3ii | 180.000 (1) | C8—C7—H7A | 120.7 |
| N2—Pt1—N3 | 80.7 (2) | C7—C8—C9 | 121.5 (6) |
| N2—Pt1—N1 | 80.8 (2) | C7—C8—H8A | 119.2 |
| N3—Pt1—N1 | 161.5 (2) | C9—C8—H8A | 119.2 |
| N2—Pt1—Br1 | 179.63 (16) | C8—C9—C10 | 118.2 (6) |
| N3—Pt1—Br1 | 98.95 (14) | C8—C9—H9A | 120.9 |
| N1—Pt1—Br1 | 99.58 (14) | C10—C9—H9A | 120.9 |
| O1—S1—C16 | 107.0 (4) | N2—C10—C9 | 118.9 (5) |
| O1—S1—C17 | 106.8 (4) | N2—C10—C11 | 113.0 (5) |
| C16—S1—C17 | 97.3 (4) | C9—C10—C11 | 128.2 (6) |
| C1—N1—C5 | 118.9 (5) | N3—C11—C12 | 120.8 (6) |
| C1—N1—Pt1 | 127.8 (4) | N3—C11—C10 | 114.7 (5) |
| C5—N1—Pt1 | 113.3 (4) | C12—C11—C10 | 124.4 (6) |
| C15—N3—C11 | 119.1 (5) | C13—C12—C11 | 120.3 (7) |
| C15—N3—Pt1 | 127.2 (4) | C13—C12—H12A | 119.8 |
| C11—N3—Pt1 | 113.6 (4) | C11—C12—H12A | 119.8 |
| C6—N2—C10 | 123.9 (5) | C12—C13—C14 | 118.4 (6) |
| C6—N2—Pt1 | 118.2 (4) | C12—C13—H13A | 120.8 |
| C10—N2—Pt1 | 117.9 (4) | C14—C13—H13A | 120.8 |
| N1—C1—C2 | 121.7 (6) | C13—C14—C15 | 120.6 (6) |
| N1—C1—H1A | 119.2 | C13—C14—H14A | 119.7 |
| C2—C1—H1A | 119.2 | C15—C14—H14A | 119.7 |
| C3—C2—C1 | 119.7 (6) | N3—C15—C14 | 120.7 (6) |
| C3—C2—H2A | 120.1 | N3—C15—H15A | 119.7 |
| C1—C2—H2A | 120.1 | C14—C15—H15A | 119.7 |
| C2—C3—C4 | 119.2 (6) | S1—C16—H16A | 109.5 |
| C2—C3—H3A | 120.4 | S1—C16—H16B | 109.5 |
| C4—C3—H3A | 120.4 | H16A—C16—H16B | 109.5 |
| C5—C4—C3 | 118.9 (6) | S1—C16—H16C | 109.5 |
| C5—C4—H4A | 120.5 | H16A—C16—H16C | 109.5 |
| C3—C4—H4A | 120.5 | H16B—C16—H16C | 109.5 |
| N1—C5—C4 | 121.6 (6) | S1—C17—H17A | 109.5 |
| N1—C5—C6 | 115.0 (5) | S1—C17—H17B | 109.5 |
| C4—C5—C6 | 123.4 (6) | H17A—C17—H17B | 109.5 |
| N2—C6—C7 | 119.0 (6) | S1—C17—H17C | 109.5 |
| N2—C6—C5 | 112.7 (5) | H17A—C17—H17C | 109.5 |
| C7—C6—C5 | 128.3 (6) | H17B—C17—H17C | 109.5 |
| C6—C7—C8 | 118.6 (6) |
| Cl | Br | I | |||
| Au—Pt | 3.2684 (1) | 3.3361 (5) | 4.2546 (4) | ||
| Pt—X | 2.305 (3) | 2.4319 (8) | 2.5930 (5) | ||
| Au—X | 2.271 (3) | 2.3984 (9) | 2.5581 (5) | ||
| Pt—Pt | 3.4535 (7) | 3.4335 (6) | 3.5278 (3) | ||
| Cl | Br | ||||
| X2—Au1—Pt1 | 88.63 (7) | 81.70 (2) | |||
| 91.37 (7) | 98.30 (2) | ||||
| X1—Pt1—Au1 | 97.62 (7) | 84.08 (2) | |||
| Au1—Pt1—Pt1(1-x, 2-y, -z) | 165.10 (2) | 173.94 (1) |
Selected geometric parameters (Å, °) in [Pt(tpy)X][AuX 2], X = Cl, Br, I
| Cl | Br | I | |||
|---|---|---|---|---|---|
| Au—Pt | 3.2684 (1) | 3.3361 (5) | 4.2546 (4) | ||
| Pt— | 2.305 (3) | 2.4319 (8) | 2.5930 (5) | ||
| Au— | 2.271 (3) | 2.3984 (9) | 2.5581 (5) | ||
| Pt—Pt | 3.4535 (7) | 3.4335 (6) | 3.5278 (3) | ||
| Cl | Br | ||||
| 88.63 (7) | 81.70 (2) | ||||
| 91.37 (7) | 98.30 (2) | ||||
| 97.62 (7) | 84.08 (2) | ||||
| Au1—Pt1—Pt1(1 − | 165.10 (2) | 173.94 (1) |