| Literature DB >> 21203079 |
Xing-Cong Wang1, Yan-Li Wu, Xiu-Li You.
Abstract
In the title chain compound, [Ag(NO(3))(C(26)H(24)P(2))](n), the bis-(diphenyl-phosphino)ethane (dppe) units link the Ag(+) ions into chains along [001]. A nitrate anion is coordinated to the Ag atom. There is a centre of symmetry at the mid-point of the ethane C-C bond and a twofold rotation axis passes through the Ag, N and terminal O atoms. Each Ag atom is four-coordinated in a distorted tetra-hedral geometry by two O atoms of the nitrate anion and two P atoms of dppe ligands. The two aromatic rings are oriented at a dihedral angle of 73.77 (3)°.Entities:
Year: 2008 PMID: 21203079 PMCID: PMC2961910 DOI: 10.1107/S1600536808019442
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| [Ag(NO3)(C26H24P2)] | |
| Monoclinic, | Mo |
| Hall symbol: -C 2yc | Cell parameters from 5049 reflections |
| θ = 3.5–25.3º | |
| µ = 0.95 mm−1 | |
| β = 108.33 (3)º | Block, colorless |
| 0.30 × 0.26 × 0.20 mm | |
| Rigaku Mercury diffractometer | 2327 independent reflections |
| Radiation source: fine-focus sealed tube | 2161 reflections with |
| Monochromator: graphite | |
| Detector resolution: 14.6306 pixels mm-1 | θmax = 25.3º |
| θmin = 3.5º | |
| ω scans | |
| Absorption correction: multi-scan(Jacobson, 1998) | |
| 12170 measured reflections |
| Refinement on | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| H-atom parameters constrained | |
| | |
| (Δ/σ)max < 0.001 | |
| 2327 reflections | Δρmax = 0.97 e Å−3 |
| 151 parameters | Δρmin = −0.45 e Å−3 |
| Primary atom site location: structure-invariant direct methods | Extinction correction: none |
| Experimental. no |
| 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 F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
| Ag1 | 0.0000 | 0.33644 (2) | 0.2500 | 0.03718 (14) | |
| P1 | 0.08413 (5) | 0.39847 (5) | 0.13087 (7) | 0.02910 (19) | |
| O1 | 0.06120 (15) | 0.17517 (16) | 0.3151 (2) | 0.0493 (6) | |
| O2 | 0.0000 | 0.0421 (3) | 0.2500 | 0.0783 (13) | |
| N1 | 0.0000 | 0.1292 (3) | 0.2500 | 0.0409 (9) | |
| C1 | 0.18506 (17) | 0.4287 (2) | 0.2384 (3) | 0.0342 (7) | |
| C2 | 0.2341 (2) | 0.5014 (3) | 0.2188 (3) | 0.0486 (8) | |
| H2A | 0.2160 | 0.5381 | 0.1457 | 0.058* | |
| C3 | 0.3100 (2) | 0.5200 (3) | 0.3075 (4) | 0.0635 (11) | |
| H3A | 0.3426 | 0.5693 | 0.2943 | 0.076* | |
| C4 | 0.3370 (2) | 0.4648 (3) | 0.4153 (4) | 0.0633 (11) | |
| H4A | 0.3878 | 0.4771 | 0.4750 | 0.076* | |
| C5 | 0.2902 (2) | 0.3933 (3) | 0.4345 (4) | 0.0612 (11) | |
| H5A | 0.3094 | 0.3560 | 0.5069 | 0.073* | |
| C6 | 0.2142 (2) | 0.3747 (3) | 0.3484 (3) | 0.0472 (8) | |
| H6A | 0.1822 | 0.3257 | 0.3639 | 0.057* | |
| C7 | 0.10284 (19) | 0.3224 (2) | 0.0110 (3) | 0.0351 (7) | |
| C8 | 0.1568 (2) | 0.3472 (3) | −0.0540 (4) | 0.0529 (9) | |
| H8A | 0.1849 | 0.4048 | −0.0367 | 0.064* | |
| C9 | 0.1693 (3) | 0.2867 (3) | −0.1445 (4) | 0.0690 (12) | |
| H9A | 0.2050 | 0.3040 | −0.1888 | 0.083* | |
| C10 | 0.1292 (3) | 0.2022 (3) | −0.1684 (4) | 0.0702 (13) | |
| H10A | 0.1385 | 0.1613 | −0.2282 | 0.084* | |
| C11 | 0.0753 (3) | 0.1761 (3) | −0.1058 (4) | 0.0677 (13) | |
| H11A | 0.0477 | 0.1183 | −0.1237 | 0.081* | |
| C12 | 0.0620 (2) | 0.2364 (2) | −0.0154 (3) | 0.0490 (9) | |
| H12A | 0.0255 | 0.2189 | 0.0274 | 0.059* | |
| C13 | 0.04348 (17) | 0.5080 (2) | 0.0442 (3) | 0.0339 (6) | |
| H13A | 0.0432 | 0.5582 | 0.1039 | 0.041* | |
| H13B | 0.0787 | 0.5278 | −0.0046 | 0.041* |
| Ag1 | 0.0364 (2) | 0.0378 (2) | 0.0391 (2) | 0.000 | 0.01439 (15) | 0.000 |
| P1 | 0.0287 (4) | 0.0281 (4) | 0.0297 (4) | 0.0031 (3) | 0.0081 (3) | 0.0020 (3) |
| O1 | 0.0397 (13) | 0.0446 (14) | 0.0527 (14) | 0.0038 (10) | −0.0010 (11) | 0.0004 (11) |
| O2 | 0.077 (3) | 0.038 (2) | 0.118 (4) | 0.000 | 0.029 (3) | 0.000 |
| N1 | 0.042 (2) | 0.033 (2) | 0.049 (2) | 0.000 | 0.0154 (19) | 0.000 |
| C1 | 0.0290 (15) | 0.0384 (16) | 0.0348 (15) | 0.0051 (12) | 0.0096 (13) | −0.0052 (13) |
| C2 | 0.0403 (19) | 0.049 (2) | 0.054 (2) | −0.0047 (15) | 0.0113 (16) | −0.0005 (16) |
| C3 | 0.0357 (19) | 0.063 (3) | 0.088 (3) | −0.0127 (17) | 0.014 (2) | −0.018 (2) |
| C4 | 0.0361 (19) | 0.082 (3) | 0.059 (2) | 0.006 (2) | −0.0046 (18) | −0.028 (2) |
| C5 | 0.047 (2) | 0.083 (3) | 0.043 (2) | 0.015 (2) | −0.0008 (18) | −0.0020 (19) |
| C6 | 0.0372 (18) | 0.062 (2) | 0.0404 (18) | 0.0085 (16) | 0.0087 (15) | 0.0075 (16) |
| C7 | 0.0380 (17) | 0.0331 (16) | 0.0326 (15) | 0.0098 (12) | 0.0088 (13) | −0.0003 (12) |
| C8 | 0.054 (2) | 0.052 (2) | 0.060 (2) | −0.0011 (17) | 0.0288 (19) | −0.0087 (17) |
| C9 | 0.077 (3) | 0.081 (3) | 0.062 (3) | 0.013 (2) | 0.040 (2) | −0.015 (2) |
| C10 | 0.097 (3) | 0.063 (3) | 0.049 (2) | 0.027 (2) | 0.021 (2) | −0.014 (2) |
| C11 | 0.107 (4) | 0.040 (2) | 0.047 (2) | 0.000 (2) | 0.011 (2) | −0.0088 (17) |
| C12 | 0.071 (2) | 0.0376 (18) | 0.0369 (17) | −0.0022 (16) | 0.0145 (17) | 0.0004 (14) |
| C13 | 0.0335 (16) | 0.0294 (15) | 0.0366 (15) | 0.0031 (12) | 0.0080 (13) | 0.0042 (12) |
| Ag1—P1 | 2.4066 (9) | C5—C6 | 1.376 (5) |
| Ag1—P1i | 2.4066 (9) | C5—H5A | 0.9300 |
| Ag1—O1i | 2.508 (2) | C6—H6A | 0.9300 |
| Ag1—O1 | 2.508 (2) | C7—C12 | 1.381 (5) |
| P1—C7 | 1.815 (3) | C7—C8 | 1.386 (5) |
| P1—C1 | 1.816 (3) | C8—C9 | 1.385 (5) |
| P1—C13 | 1.834 (3) | C8—H8A | 0.9300 |
| O1—N1 | 1.250 (3) | C9—C10 | 1.357 (7) |
| O2—N1 | 1.225 (5) | C9—H9A | 0.9300 |
| N1—O1i | 1.250 (3) | C10—C11 | 1.370 (7) |
| C1—C2 | 1.382 (5) | C10—H10A | 0.9300 |
| C1—C6 | 1.393 (4) | C11—C12 | 1.387 (5) |
| C2—C3 | 1.388 (5) | C11—H11A | 0.9300 |
| C2—H2A | 0.9300 | C12—H12A | 0.9300 |
| C3—C4 | 1.381 (6) | C13—C13ii | 1.521 (6) |
| C3—H3A | 0.9300 | C13—H13A | 0.9700 |
| C4—C5 | 1.343 (6) | C13—H13B | 0.9700 |
| C4—H4A | 0.9300 | ||
| P1—Ag1—P1i | 137.49 (4) | C4—C5—H5A | 119.6 |
| P1—Ag1—O1i | 115.92 (7) | C6—C5—H5A | 119.6 |
| P1i—Ag1—O1i | 102.63 (7) | C5—C6—C1 | 120.4 (4) |
| P1—Ag1—O1 | 102.63 (6) | C5—C6—H6A | 119.8 |
| P1i—Ag1—O1 | 115.92 (7) | C1—C6—H6A | 119.8 |
| O1i—Ag1—O1 | 50.52 (11) | C12—C7—C8 | 119.1 (3) |
| C7—P1—C1 | 105.68 (14) | C12—C7—P1 | 118.6 (3) |
| C7—P1—C13 | 103.59 (14) | C8—C7—P1 | 122.4 (3) |
| C1—P1—C13 | 105.93 (14) | C9—C8—C7 | 120.3 (4) |
| C7—P1—Ag1 | 117.71 (11) | C9—C8—H8A | 119.8 |
| C1—P1—Ag1 | 109.46 (10) | C7—C8—H8A | 119.8 |
| C13—P1—Ag1 | 113.56 (10) | C10—C9—C8 | 119.8 (4) |
| N1—O1—Ag1 | 95.88 (19) | C10—C9—H9A | 120.1 |
| O2—N1—O1 | 121.14 (18) | C8—C9—H9A | 120.1 |
| O2—N1—O1i | 121.14 (18) | C9—C10—C11 | 121.0 (4) |
| O1—N1—O1i | 117.7 (4) | C9—C10—H10A | 119.5 |
| C2—C1—C6 | 118.3 (3) | C11—C10—H10A | 119.5 |
| C2—C1—P1 | 124.7 (2) | C10—C11—C12 | 119.7 (4) |
| C6—C1—P1 | 117.0 (3) | C10—C11—H11A | 120.2 |
| C1—C2—C3 | 120.5 (4) | C12—C11—H11A | 120.2 |
| C1—C2—H2A | 119.8 | C7—C12—C11 | 120.1 (4) |
| C3—C2—H2A | 119.8 | C7—C12—H12A | 119.9 |
| C4—C3—C2 | 119.6 (4) | C11—C12—H12A | 119.9 |
| C4—C3—H3A | 120.2 | C13ii—C13—P1 | 110.4 (3) |
| C2—C3—H3A | 120.2 | C13ii—C13—H13A | 109.6 |
| C5—C4—C3 | 120.4 (3) | P1—C13—H13A | 109.6 |
| C5—C4—H4A | 119.8 | C13ii—C13—H13B | 109.6 |
| C3—C4—H4A | 119.8 | P1—C13—H13B | 109.6 |
| C4—C5—C6 | 120.9 (4) | H13A—C13—H13B | 108.1 |
| Ag1—P1 | 2.4066 (9) |
| Ag1—O1 | 2.508 (2) |
| P1—Ag1—P1i | 137.49 (4) |
| P1—Ag1—O1i | 115.92 (7) |
| P1—Ag1—O1 | 102.63 (6) |
| O1i—Ag1—O1 | 50.52 (11) |
Symmetry code: (i) .