Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806028856/ng2055sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806028856/ng2055Isup2.hkl |
CCDC reference: 618294
Data collection: XSCANS (Fait, 1991); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: SHELXL97.
[Au(C6F5)2(C19H17PS)2]ClO4·CHCl3 | Dx = 1.693 Mg m−3 |
Mr = 1366.62 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, P212121 | Cell parameters from 75 reflections |
a = 11.290 (2) Å | θ = 4.5–12.5° |
b = 13.795 (2) Å | µ = 3.16 mm−1 |
c = 34.421 (4) Å | T = 173 K |
V = 5361.1 (14) Å3 | Prism, colourless |
Z = 4 | 0.50 × 0.35 × 0.20 mm |
F(000) = 2688 |
Siemens P4 diffractometer | 9376 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.030 |
Graphite monochromator | θmax = 27.5°, θmin = 3.2° |
ω scans | h = 0→14 |
Absorption correction: ψ scan (XEMP; Siemens, 1994) | k = −17→17 |
Tmin = 0.739, Tmax = 0.834 | l = −44→40 |
17522 measured reflections | 3 standard reflections every 297 reflections |
11909 independent reflections | intensity decay: none |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.037 | H-atom parameters constrained |
wR(F2) = 0.069 | w = 1/[σ2(Fo2) + (0.0289P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.92 | (Δ/σ)max = 0.003 |
11909 reflections | Δρmax = 1.10 e Å−3 |
662 parameters | Δρmin = −0.77 e Å−3 |
562 restraints | Absolute structure: Flack (1983), 5100 Friedel pairs |
Primary atom site location: Patterson | Absolute structure parameter: −0.019 (4) |
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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 10.3627 (0.0058) x - 0.5752 (0.0158) y + 13.5850 (0.0387) z = 11.6045 (0.0238) * -0.0039 (0.0015) Au * -0.1337 (0.0020) P1 * 0.1383 (0.0020) P2 * 0.1768 (0.0024) C71 * -0.1776 (0.0026) C81 Rms deviation of fitted atoms = 0.1413 |
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 > σ(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. |
x | y | z | Uiso*/Ueq | ||
Au | 0.355390 (18) | 0.592752 (14) | 0.607929 (6) | 0.02185 (5) | |
P1 | 0.29004 (13) | 0.45276 (10) | 0.64230 (4) | 0.0226 (3) | |
P2 | 0.31007 (13) | 0.70826 (11) | 0.65786 (4) | 0.0250 (3) | |
S1 | 0.29066 (13) | 0.29124 (11) | 0.58488 (4) | 0.0305 (3) | |
S2 | 0.55969 (14) | 0.65283 (13) | 0.67298 (4) | 0.0369 (4) | |
C1 | 0.3655 (6) | 0.3408 (4) | 0.62740 (15) | 0.0294 (13) | |
H1A | 0.4493 | 0.3548 | 0.6211 | 0.035* | |
H1B | 0.3636 | 0.2931 | 0.6489 | 0.035* | |
C2 | 0.4229 (5) | 0.6897 (4) | 0.69607 (15) | 0.0270 (13) | |
H2A | 0.4352 | 0.7506 | 0.7107 | 0.032* | |
H2B | 0.3961 | 0.6391 | 0.7145 | 0.032* | |
C11 | 0.1337 (5) | 0.4322 (3) | 0.63247 (13) | 0.0264 (12) | |
C12 | 0.0761 (5) | 0.4815 (4) | 0.60321 (16) | 0.0266 (12) | |
H12 | 0.1180 | 0.5277 | 0.5881 | 0.032* | |
C13 | −0.0431 (5) | 0.4640 (4) | 0.59573 (16) | 0.0358 (14) | |
H13 | −0.0837 | 0.4990 | 0.5761 | 0.043* | |
C14 | −0.1006 (5) | 0.3953 (5) | 0.61733 (15) | 0.0411 (15) | |
H14 | −0.1820 | 0.3831 | 0.6124 | 0.049* | |
C15 | −0.0453 (5) | 0.3441 (5) | 0.64550 (19) | 0.0464 (17) | |
H15 | −0.0872 | 0.2955 | 0.6594 | 0.056* | |
C16 | 0.0720 (5) | 0.3623 (4) | 0.65419 (16) | 0.0359 (14) | |
H16 | 0.1104 | 0.3281 | 0.6746 | 0.043* | |
C21 | 0.3081 (5) | 0.4553 (4) | 0.69435 (15) | 0.0290 (13) | |
C22 | 0.2163 (6) | 0.4857 (4) | 0.71884 (16) | 0.0341 (14) | |
H22 | 0.1406 | 0.5017 | 0.7086 | 0.041* | |
C23 | 0.2388 (6) | 0.4920 (5) | 0.75882 (18) | 0.0438 (17) | |
H23 | 0.1776 | 0.5128 | 0.7758 | 0.053* | |
C24 | 0.3477 (7) | 0.4684 (4) | 0.77369 (17) | 0.0475 (16) | |
H24 | 0.3614 | 0.4739 | 0.8008 | 0.057* | |
C25 | 0.4377 (6) | 0.4370 (4) | 0.74970 (17) | 0.0424 (16) | |
H25 | 0.5125 | 0.4197 | 0.7603 | 0.051* | |
C26 | 0.4181 (5) | 0.4307 (4) | 0.70966 (16) | 0.0330 (14) | |
H26 | 0.4799 | 0.4097 | 0.6929 | 0.040* | |
C31 | 0.4074 (5) | 0.2416 (4) | 0.55693 (15) | 0.0272 (12) | |
C32 | 0.3804 (5) | 0.2232 (4) | 0.51829 (16) | 0.0402 (15) | |
H32 | 0.3046 | 0.2393 | 0.5082 | 0.048* | |
C33 | 0.4653 (6) | 0.1809 (5) | 0.49467 (18) | 0.0493 (18) | |
H33 | 0.4472 | 0.1670 | 0.4683 | 0.059* | |
C34 | 0.5755 (6) | 0.1591 (5) | 0.5091 (2) | 0.0540 (18) | |
H34 | 0.6338 | 0.1319 | 0.4925 | 0.065* | |
C35 | 0.6019 (6) | 0.1761 (5) | 0.5469 (2) | 0.0470 (17) | |
H35 | 0.6778 | 0.1597 | 0.5569 | 0.056* | |
C36 | 0.5185 (5) | 0.2172 (4) | 0.57078 (17) | 0.0381 (14) | |
H36 | 0.5374 | 0.2291 | 0.5973 | 0.046* | |
C41 | 0.3275 (5) | 0.8334 (4) | 0.64230 (15) | 0.0300 (14) | |
C42 | 0.2269 (6) | 0.8828 (4) | 0.62898 (17) | 0.0431 (17) | |
H42 | 0.1507 | 0.8537 | 0.6300 | 0.052* | |
C43 | 0.2420 (7) | 0.9764 (4) | 0.6141 (2) | 0.063 (2) | |
H43 | 0.1756 | 1.0110 | 0.6044 | 0.075* | |
C44 | 0.3533 (7) | 1.0190 (4) | 0.6135 (2) | 0.0633 (19) | |
H44 | 0.3617 | 1.0833 | 0.6040 | 0.076* | |
C45 | 0.4520 (7) | 0.9696 (5) | 0.6264 (2) | 0.0551 (19) | |
H45 | 0.5281 | 0.9987 | 0.6247 | 0.066* | |
C46 | 0.4397 (6) | 0.8774 (4) | 0.64168 (18) | 0.0400 (16) | |
H46 | 0.5067 | 0.8441 | 0.6517 | 0.048* | |
C51 | 0.1662 (5) | 0.7028 (4) | 0.68073 (14) | 0.0272 (13) | |
C52 | 0.1542 (6) | 0.7257 (4) | 0.72017 (15) | 0.0365 (13) | |
H52 | 0.2217 | 0.7418 | 0.7353 | 0.044* | |
C53 | 0.0434 (6) | 0.7248 (5) | 0.73659 (18) | 0.0467 (18) | |
H53 | 0.0339 | 0.7406 | 0.7633 | 0.056* | |
C54 | −0.0539 (6) | 0.7009 (6) | 0.71445 (18) | 0.0548 (19) | |
H54 | −0.1303 | 0.7003 | 0.7260 | 0.066* | |
C55 | −0.0417 (5) | 0.6780 (5) | 0.67581 (18) | 0.0474 (18) | |
H55 | −0.1089 | 0.6601 | 0.6608 | 0.057* | |
C56 | 0.0677 (5) | 0.6811 (4) | 0.65923 (16) | 0.0312 (13) | |
H56 | 0.0758 | 0.6680 | 0.6323 | 0.037* | |
C61 | 0.6386 (5) | 0.6005 (4) | 0.71244 (13) | 0.0331 (11) | |
C62 | 0.7134 (5) | 0.5223 (4) | 0.70322 (19) | 0.0415 (15) | |
H62 | 0.7185 | 0.4988 | 0.6773 | 0.050* | |
C63 | 0.7791 (6) | 0.4805 (5) | 0.7325 (2) | 0.0503 (17) | |
H63 | 0.8316 | 0.4289 | 0.7264 | 0.060* | |
C64 | 0.7706 (6) | 0.5119 (5) | 0.7704 (2) | 0.058 (2) | |
H64 | 0.8154 | 0.4814 | 0.7903 | 0.070* | |
C65 | 0.6956 (5) | 0.5885 (6) | 0.77913 (18) | 0.0533 (17) | |
H65 | 0.6887 | 0.6097 | 0.8053 | 0.064* | |
C66 | 0.6307 (6) | 0.6345 (4) | 0.75051 (15) | 0.0385 (14) | |
H66 | 0.5817 | 0.6883 | 0.7567 | 0.046* | |
C71 | 0.4265 (5) | 0.5091 (4) | 0.56345 (14) | 0.0235 (12) | |
C72 | 0.5429 (5) | 0.4802 (3) | 0.56595 (15) | 0.0291 (13) | |
C73 | 0.6021 (5) | 0.4398 (4) | 0.53477 (16) | 0.0319 (14) | |
C74 | 0.5449 (5) | 0.4276 (4) | 0.49986 (15) | 0.0340 (14) | |
C75 | 0.4266 (5) | 0.4541 (4) | 0.49700 (16) | 0.0324 (13) | |
C76 | 0.3715 (5) | 0.4960 (4) | 0.52829 (15) | 0.0278 (12) | |
F1 | 0.6033 (3) | 0.4903 (2) | 0.59932 (9) | 0.0379 (9) | |
F2 | 0.7162 (3) | 0.4146 (3) | 0.53794 (10) | 0.0484 (9) | |
F3 | 0.6008 (3) | 0.3896 (3) | 0.46927 (9) | 0.0500 (10) | |
F4 | 0.3687 (4) | 0.4387 (2) | 0.46353 (9) | 0.0512 (10) | |
F5 | 0.2582 (3) | 0.5250 (3) | 0.52375 (10) | 0.0395 (9) | |
C81 | 0.3943 (5) | 0.7065 (4) | 0.57024 (15) | 0.0336 (15) | |
C82 | 0.5058 (6) | 0.7344 (4) | 0.56032 (16) | 0.0424 (16) | |
C83 | 0.5260 (7) | 0.8082 (5) | 0.53414 (19) | 0.062 (2) | |
C84 | 0.4322 (7) | 0.8539 (6) | 0.5172 (2) | 0.074 (3) | |
C85 | 0.3187 (7) | 0.8273 (5) | 0.5262 (2) | 0.067 (2) | |
C86 | 0.3015 (6) | 0.7527 (4) | 0.55292 (18) | 0.0449 (17) | |
F6 | 0.6004 (3) | 0.6906 (3) | 0.57596 (11) | 0.0519 (10) | |
F7 | 0.6385 (5) | 0.8364 (3) | 0.52578 (12) | 0.0921 (16) | |
F8 | 0.4511 (6) | 0.9271 (4) | 0.49205 (14) | 0.123 (2) | |
F9 | 0.2251 (5) | 0.8722 (3) | 0.51038 (14) | 0.0998 (19) | |
F10 | 0.1882 (3) | 0.7285 (3) | 0.56119 (11) | 0.0532 (11) | |
Cl1 | 0.35446 (16) | 0.72948 (10) | 0.81964 (4) | 0.0398 (3) | |
O1 | 0.4443 (5) | 0.6648 (4) | 0.83187 (16) | 0.0760 (19) | |
O2 | 0.3525 (4) | 0.8115 (3) | 0.84529 (10) | 0.0402 (10) | |
O3 | 0.3822 (5) | 0.7623 (4) | 0.78082 (12) | 0.0645 (16) | |
O4 | 0.2436 (5) | 0.6849 (4) | 0.81788 (19) | 0.089 (2) | |
C99 | 0.3314 (8) | 0.5847 (7) | 0.3975 (3) | 0.101 (3)* | |
H99 | 0.2767 | 0.5510 | 0.4159 | 0.121* | |
Cl2 | 0.4399 (3) | 0.6445 (2) | 0.42461 (8) | 0.1161 (10) | |
Cl3 | 0.2502 (3) | 0.6623 (2) | 0.36987 (9) | 0.1238 (11) | |
Cl4 | 0.3972 (5) | 0.4983 (3) | 0.36822 (12) | 0.230 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Au | 0.02438 (9) | 0.02016 (8) | 0.02100 (8) | −0.00173 (11) | −0.00004 (11) | 0.00316 (10) |
P1 | 0.0244 (8) | 0.0199 (7) | 0.0235 (7) | −0.0011 (6) | 0.0004 (6) | 0.0025 (6) |
P2 | 0.0287 (9) | 0.0208 (8) | 0.0255 (8) | −0.0031 (6) | −0.0005 (6) | 0.0017 (6) |
S1 | 0.0283 (8) | 0.0291 (8) | 0.0339 (8) | −0.0018 (7) | 0.0006 (7) | −0.0057 (7) |
S2 | 0.0304 (9) | 0.0522 (10) | 0.0281 (8) | 0.0035 (8) | 0.0005 (7) | 0.0017 (8) |
C1 | 0.038 (4) | 0.017 (3) | 0.033 (3) | 0.005 (3) | 0.012 (3) | 0.002 (2) |
C2 | 0.032 (3) | 0.025 (3) | 0.024 (3) | 0.000 (3) | −0.002 (3) | −0.003 (2) |
C11 | 0.028 (3) | 0.025 (3) | 0.026 (2) | −0.004 (3) | 0.005 (3) | −0.0030 (19) |
C12 | 0.027 (3) | 0.027 (3) | 0.026 (3) | −0.006 (2) | 0.002 (3) | 0.002 (2) |
C13 | 0.033 (3) | 0.045 (4) | 0.030 (3) | 0.006 (3) | −0.001 (2) | −0.004 (3) |
C14 | 0.026 (3) | 0.059 (4) | 0.039 (4) | −0.011 (3) | 0.001 (2) | −0.004 (3) |
C15 | 0.030 (4) | 0.059 (4) | 0.051 (4) | −0.016 (3) | −0.002 (3) | 0.012 (3) |
C16 | 0.039 (4) | 0.041 (3) | 0.028 (3) | −0.006 (3) | −0.005 (3) | 0.008 (3) |
C21 | 0.044 (3) | 0.019 (3) | 0.023 (3) | −0.003 (3) | −0.004 (2) | 0.005 (2) |
C22 | 0.044 (4) | 0.028 (3) | 0.031 (3) | −0.001 (3) | 0.002 (3) | 0.001 (3) |
C23 | 0.057 (4) | 0.044 (4) | 0.031 (3) | −0.010 (3) | 0.012 (3) | 0.000 (3) |
C24 | 0.078 (5) | 0.041 (4) | 0.024 (3) | −0.005 (4) | −0.007 (3) | 0.003 (3) |
C25 | 0.051 (4) | 0.040 (4) | 0.036 (3) | −0.004 (3) | −0.013 (3) | 0.009 (3) |
C26 | 0.039 (3) | 0.030 (4) | 0.030 (3) | −0.005 (3) | −0.001 (3) | 0.004 (3) |
C31 | 0.029 (3) | 0.019 (3) | 0.034 (3) | −0.004 (2) | 0.006 (3) | 0.000 (2) |
C32 | 0.043 (4) | 0.035 (3) | 0.042 (3) | −0.003 (3) | −0.003 (3) | −0.016 (3) |
C33 | 0.060 (4) | 0.054 (4) | 0.035 (3) | −0.012 (4) | 0.007 (3) | −0.021 (3) |
C34 | 0.045 (4) | 0.045 (4) | 0.072 (5) | −0.002 (3) | 0.021 (4) | −0.018 (4) |
C35 | 0.033 (4) | 0.050 (4) | 0.059 (4) | 0.010 (3) | 0.012 (3) | −0.004 (4) |
C36 | 0.044 (4) | 0.035 (3) | 0.035 (3) | 0.005 (3) | 0.004 (3) | 0.001 (3) |
C41 | 0.040 (4) | 0.021 (3) | 0.029 (3) | −0.004 (2) | 0.002 (3) | 0.002 (2) |
C42 | 0.053 (4) | 0.029 (4) | 0.047 (4) | −0.002 (3) | −0.013 (3) | 0.009 (3) |
C43 | 0.090 (5) | 0.035 (4) | 0.063 (5) | 0.007 (4) | −0.016 (5) | 0.019 (4) |
C44 | 0.100 (5) | 0.026 (3) | 0.064 (5) | −0.012 (4) | −0.003 (6) | 0.011 (3) |
C45 | 0.074 (5) | 0.036 (4) | 0.056 (5) | −0.017 (4) | 0.009 (4) | 0.001 (3) |
C46 | 0.042 (4) | 0.033 (4) | 0.044 (4) | −0.007 (3) | 0.007 (3) | 0.002 (3) |
C51 | 0.031 (3) | 0.024 (3) | 0.026 (3) | −0.001 (3) | 0.003 (2) | 0.001 (2) |
C52 | 0.038 (3) | 0.037 (3) | 0.034 (3) | −0.003 (3) | 0.005 (3) | −0.009 (3) |
C53 | 0.042 (4) | 0.067 (5) | 0.031 (3) | −0.009 (4) | 0.011 (3) | −0.013 (3) |
C54 | 0.027 (3) | 0.085 (6) | 0.052 (4) | −0.005 (4) | 0.016 (3) | −0.001 (4) |
C55 | 0.032 (3) | 0.069 (5) | 0.041 (4) | −0.009 (4) | −0.007 (3) | −0.009 (4) |
C56 | 0.039 (3) | 0.026 (3) | 0.029 (3) | 0.001 (3) | −0.005 (3) | −0.006 (2) |
C61 | 0.029 (3) | 0.041 (3) | 0.030 (2) | −0.004 (3) | 0.004 (3) | 0.004 (3) |
C62 | 0.034 (4) | 0.045 (4) | 0.045 (4) | −0.003 (3) | 0.000 (3) | −0.002 (3) |
C63 | 0.039 (4) | 0.046 (4) | 0.065 (4) | 0.008 (3) | −0.001 (4) | 0.011 (3) |
C64 | 0.049 (5) | 0.072 (5) | 0.053 (4) | 0.015 (4) | −0.004 (4) | 0.027 (4) |
C65 | 0.043 (4) | 0.080 (5) | 0.036 (3) | 0.003 (4) | −0.004 (3) | 0.007 (4) |
C66 | 0.031 (4) | 0.054 (4) | 0.031 (3) | 0.004 (3) | 0.000 (3) | 0.000 (3) |
C71 | 0.026 (3) | 0.026 (3) | 0.018 (3) | 0.004 (2) | 0.003 (2) | 0.003 (2) |
C72 | 0.030 (3) | 0.026 (3) | 0.031 (3) | −0.006 (3) | −0.006 (3) | 0.005 (2) |
C73 | 0.032 (3) | 0.031 (3) | 0.033 (3) | −0.001 (2) | 0.004 (2) | 0.000 (3) |
C74 | 0.044 (3) | 0.029 (4) | 0.030 (3) | −0.006 (3) | 0.008 (3) | −0.002 (2) |
C75 | 0.041 (3) | 0.029 (3) | 0.028 (3) | −0.009 (3) | 0.001 (3) | 0.005 (2) |
C76 | 0.026 (3) | 0.028 (3) | 0.029 (3) | −0.007 (3) | −0.003 (2) | 0.006 (2) |
F1 | 0.032 (2) | 0.050 (2) | 0.031 (2) | 0.0029 (15) | −0.0055 (14) | −0.0025 (16) |
F2 | 0.031 (2) | 0.056 (2) | 0.058 (2) | 0.005 (2) | 0.0062 (17) | −0.015 (2) |
F3 | 0.059 (2) | 0.055 (3) | 0.0363 (18) | 0.002 (2) | 0.0182 (17) | −0.0157 (18) |
F4 | 0.067 (3) | 0.057 (2) | 0.0295 (17) | −0.004 (2) | −0.015 (2) | −0.0070 (15) |
F5 | 0.036 (2) | 0.043 (2) | 0.040 (2) | 0.0043 (18) | −0.0100 (17) | 0.0013 (17) |
C81 | 0.056 (4) | 0.022 (3) | 0.022 (3) | −0.007 (3) | 0.007 (3) | 0.003 (2) |
C82 | 0.059 (4) | 0.036 (4) | 0.032 (3) | −0.010 (3) | 0.015 (3) | 0.005 (3) |
C83 | 0.101 (6) | 0.044 (4) | 0.042 (4) | −0.024 (4) | 0.025 (4) | 0.005 (3) |
C84 | 0.137 (7) | 0.041 (4) | 0.044 (4) | −0.014 (5) | 0.014 (5) | 0.029 (4) |
C85 | 0.112 (6) | 0.041 (4) | 0.047 (4) | 0.011 (4) | −0.011 (4) | 0.024 (3) |
C86 | 0.071 (5) | 0.027 (3) | 0.036 (4) | 0.008 (3) | 0.001 (3) | 0.008 (3) |
F6 | 0.047 (3) | 0.059 (3) | 0.049 (2) | −0.020 (2) | 0.0121 (19) | 0.004 (2) |
F7 | 0.119 (4) | 0.081 (3) | 0.077 (3) | −0.056 (3) | 0.042 (3) | 0.013 (3) |
F8 | 0.221 (7) | 0.068 (4) | 0.082 (3) | −0.022 (4) | 0.015 (4) | 0.050 (3) |
F9 | 0.144 (5) | 0.072 (4) | 0.084 (4) | 0.026 (3) | −0.026 (3) | 0.043 (3) |
F10 | 0.053 (3) | 0.051 (2) | 0.055 (2) | 0.015 (2) | −0.0105 (19) | 0.010 (2) |
Cl1 | 0.0363 (8) | 0.0387 (8) | 0.0444 (8) | 0.0044 (9) | −0.0022 (9) | −0.0167 (7) |
O1 | 0.098 (5) | 0.065 (4) | 0.065 (4) | 0.050 (3) | −0.030 (3) | −0.023 (3) |
O2 | 0.043 (2) | 0.036 (2) | 0.042 (2) | 0.009 (2) | −0.002 (2) | −0.0162 (18) |
O3 | 0.077 (4) | 0.084 (4) | 0.033 (2) | 0.003 (3) | −0.004 (3) | −0.010 (3) |
O4 | 0.064 (4) | 0.074 (4) | 0.129 (5) | −0.029 (3) | 0.033 (4) | −0.052 (4) |
Cl2 | 0.0904 (19) | 0.146 (3) | 0.112 (2) | −0.0376 (19) | −0.0142 (17) | 0.0093 (19) |
Cl3 | 0.097 (2) | 0.138 (3) | 0.137 (3) | 0.007 (2) | −0.0248 (19) | 0.024 (2) |
Cl4 | 0.324 (6) | 0.173 (4) | 0.191 (4) | 0.113 (4) | −0.157 (4) | −0.086 (3) |
Au—C71 | 2.079 (5) | C44—C45 | 1.379 (8) |
Au—C81 | 2.083 (5) | C44—H44 | 0.9500 |
Au—P1 | 2.3818 (14) | C45—C46 | 1.383 (8) |
Au—P2 | 2.3990 (15) | C45—H45 | 0.9500 |
P1—C21 | 1.804 (5) | C46—H46 | 0.9500 |
P1—C11 | 1.820 (6) | C51—C56 | 1.369 (7) |
P1—C1 | 1.837 (5) | C51—C52 | 1.401 (7) |
P2—C51 | 1.806 (6) | C52—C53 | 1.372 (8) |
P2—C41 | 1.818 (5) | C52—H52 | 0.9500 |
P2—C2 | 1.849 (5) | C53—C54 | 1.378 (8) |
S1—C31 | 1.769 (6) | C53—H53 | 0.9500 |
S1—C1 | 1.823 (6) | C54—C55 | 1.374 (8) |
S2—C61 | 1.778 (6) | C54—H54 | 0.9500 |
S2—C2 | 1.810 (6) | C55—C56 | 1.361 (8) |
C1—H1A | 0.9900 | C55—H55 | 0.9500 |
C1—H1B | 0.9900 | C56—H56 | 0.9500 |
C2—H2A | 0.9900 | C61—C66 | 1.394 (7) |
C2—H2B | 0.9900 | C61—C62 | 1.406 (8) |
C11—C12 | 1.378 (7) | C62—C63 | 1.378 (8) |
C11—C16 | 1.405 (7) | C62—H62 | 0.9500 |
C12—C13 | 1.391 (7) | C63—C64 | 1.378 (8) |
C12—H12 | 0.9500 | C63—H63 | 0.9500 |
C13—C14 | 1.368 (7) | C64—C65 | 1.386 (9) |
C13—H13 | 0.9500 | C64—H64 | 0.9500 |
C14—C15 | 1.352 (7) | C65—C66 | 1.382 (8) |
C14—H14 | 0.9500 | C65—H65 | 0.9500 |
C15—C16 | 1.381 (8) | C66—H66 | 0.9500 |
C15—H15 | 0.9500 | C71—C76 | 1.372 (6) |
C16—H16 | 0.9500 | C71—C72 | 1.376 (7) |
C21—C26 | 1.391 (7) | C72—F1 | 1.343 (6) |
C21—C22 | 1.400 (7) | C72—C73 | 1.381 (7) |
C22—C23 | 1.402 (8) | C73—F2 | 1.340 (6) |
C22—H22 | 0.9500 | C73—C74 | 1.375 (7) |
C23—C24 | 1.371 (8) | C74—F3 | 1.335 (6) |
C23—H23 | 0.9500 | C74—C75 | 1.388 (7) |
C24—C25 | 1.379 (8) | C75—F4 | 1.341 (6) |
C24—H24 | 0.9500 | C75—C76 | 1.372 (7) |
C25—C26 | 1.399 (7) | C76—F5 | 1.349 (6) |
C25—H25 | 0.9500 | C81—C82 | 1.359 (8) |
C26—H26 | 0.9500 | C81—C86 | 1.364 (7) |
C31—C36 | 1.385 (7) | C82—F6 | 1.340 (7) |
C31—C32 | 1.388 (7) | C82—C83 | 1.379 (8) |
C32—C33 | 1.386 (8) | C83—F7 | 1.359 (8) |
C32—H32 | 0.9500 | C83—C84 | 1.364 (9) |
C33—C34 | 1.373 (8) | C84—F8 | 1.348 (8) |
C33—H33 | 0.9500 | C84—C85 | 1.368 (9) |
C34—C35 | 1.355 (8) | C85—F9 | 1.340 (8) |
C34—H34 | 0.9500 | C85—C86 | 1.394 (8) |
C35—C36 | 1.371 (7) | C86—F10 | 1.352 (7) |
C35—H35 | 0.9500 | Cl1—O4 | 1.395 (5) |
C36—H36 | 0.9500 | Cl1—O1 | 1.415 (5) |
C41—C42 | 1.402 (7) | Cl1—O2 | 1.436 (4) |
C41—C46 | 1.406 (7) | Cl1—O3 | 1.445 (4) |
C42—C43 | 1.398 (8) | C99—Cl3 | 1.700 (9) |
C42—H42 | 0.9500 | C99—Cl4 | 1.729 (9) |
C43—C44 | 1.388 (8) | C99—Cl2 | 1.748 (9) |
C43—H43 | 0.9500 | C99—H99 | 1.0000 |
C71—Au—C81 | 83.0 (2) | C42—C43—H43 | 119.8 |
C71—Au—P1 | 92.02 (14) | C45—C44—C43 | 121.2 (6) |
C81—Au—P1 | 170.25 (15) | C45—C44—H44 | 119.4 |
C71—Au—P2 | 168.21 (15) | C43—C44—H44 | 119.4 |
C81—Au—P2 | 89.47 (15) | C44—C45—C46 | 119.7 (7) |
P1—Au—P2 | 96.70 (5) | C44—C45—H45 | 120.2 |
C21—P1—C11 | 107.3 (2) | C46—C45—H45 | 120.2 |
C21—P1—C1 | 104.0 (2) | C45—C46—C41 | 119.6 (7) |
C11—P1—C1 | 105.5 (3) | C45—C46—H46 | 120.2 |
C21—P1—Au | 116.27 (18) | C41—C46—H46 | 120.2 |
C11—P1—Au | 109.54 (16) | C56—C51—C52 | 119.6 (6) |
C1—P1—Au | 113.56 (19) | C56—C51—P2 | 120.3 (4) |
C51—P2—C41 | 105.4 (2) | C52—C51—P2 | 120.0 (4) |
C51—P2—C2 | 107.7 (2) | C53—C52—C51 | 119.1 (6) |
C41—P2—C2 | 105.5 (3) | C53—C52—H52 | 120.5 |
C51—P2—Au | 118.44 (18) | C51—C52—H52 | 120.5 |
C41—P2—Au | 113.36 (18) | C52—C53—C54 | 120.1 (6) |
C2—P2—Au | 105.71 (18) | C52—C53—H53 | 120.0 |
C31—S1—C1 | 103.7 (3) | C54—C53—H53 | 120.0 |
C61—S2—C2 | 101.9 (2) | C55—C54—C53 | 120.7 (6) |
S1—C1—P1 | 108.9 (3) | C55—C54—H54 | 119.7 |
S1—C1—H1A | 109.9 | C53—C54—H54 | 119.7 |
P1—C1—H1A | 109.9 | C56—C55—C54 | 119.3 (6) |
S1—C1—H1B | 109.9 | C56—C55—H55 | 120.3 |
P1—C1—H1B | 109.9 | C54—C55—H55 | 120.3 |
H1A—C1—H1B | 108.3 | C55—C56—C51 | 121.2 (5) |
S2—C2—P2 | 108.3 (3) | C55—C56—H56 | 119.4 |
S2—C2—H2A | 110.0 | C51—C56—H56 | 119.4 |
P2—C2—H2A | 110.0 | C66—C61—C62 | 120.6 (6) |
S2—C2—H2B | 110.0 | C66—C61—S2 | 123.3 (5) |
P2—C2—H2B | 110.0 | C62—C61—S2 | 116.1 (4) |
H2A—C2—H2B | 108.4 | C63—C62—C61 | 118.6 (6) |
C12—C11—C16 | 119.6 (5) | C63—C62—H62 | 120.7 |
C12—C11—P1 | 121.1 (4) | C61—C62—H62 | 120.7 |
C16—C11—P1 | 119.3 (4) | C64—C63—C62 | 121.6 (7) |
C11—C12—C13 | 120.4 (5) | C64—C63—H63 | 119.2 |
C11—C12—H12 | 119.8 | C62—C63—H63 | 119.2 |
C13—C12—H12 | 119.8 | C63—C64—C65 | 119.1 (6) |
C14—C13—C12 | 118.6 (5) | C63—C64—H64 | 120.4 |
C14—C13—H13 | 120.7 | C65—C64—H64 | 120.4 |
C12—C13—H13 | 120.7 | C66—C65—C64 | 121.3 (6) |
C15—C14—C13 | 122.1 (6) | C66—C65—H65 | 119.4 |
C15—C14—H14 | 118.9 | C64—C65—H65 | 119.4 |
C13—C14—H14 | 118.9 | C65—C66—C61 | 118.8 (6) |
C14—C15—C16 | 120.2 (6) | C65—C66—H66 | 120.6 |
C14—C15—H15 | 119.9 | C61—C66—H66 | 120.6 |
C16—C15—H15 | 119.9 | C76—C71—C72 | 116.7 (5) |
C15—C16—C11 | 119.0 (6) | C76—C71—Au | 123.2 (4) |
C15—C16—H16 | 120.5 | C72—C71—Au | 118.9 (4) |
C11—C16—H16 | 120.5 | F1—C72—C71 | 120.5 (5) |
C26—C21—C22 | 120.4 (5) | F1—C72—C73 | 117.5 (5) |
C26—C21—P1 | 118.2 (4) | C71—C72—C73 | 122.0 (5) |
C22—C21—P1 | 121.3 (4) | F2—C73—C74 | 119.4 (5) |
C21—C22—C23 | 118.4 (6) | F2—C73—C72 | 120.4 (5) |
C21—C22—H22 | 120.8 | C74—C73—C72 | 120.1 (5) |
C23—C22—H22 | 120.8 | F3—C74—C73 | 121.0 (5) |
C24—C23—C22 | 120.9 (6) | F3—C74—C75 | 120.2 (5) |
C24—C23—H23 | 119.5 | C73—C74—C75 | 118.8 (5) |
C22—C23—H23 | 119.5 | F4—C75—C76 | 121.4 (5) |
C23—C24—C25 | 120.8 (6) | F4—C75—C74 | 119.2 (5) |
C23—C24—H24 | 119.6 | C76—C75—C74 | 119.5 (5) |
C25—C24—H24 | 119.6 | F5—C76—C75 | 117.6 (5) |
C24—C25—C26 | 119.5 (6) | F5—C76—C71 | 119.5 (5) |
C24—C25—H25 | 120.2 | C75—C76—C71 | 122.8 (5) |
C26—C25—H25 | 120.2 | C82—C81—C86 | 118.0 (6) |
C21—C26—C25 | 120.0 (6) | C82—C81—Au | 124.4 (5) |
C21—C26—H26 | 120.0 | C86—C81—Au | 117.5 (4) |
C25—C26—H26 | 120.0 | F6—C82—C81 | 120.7 (5) |
C36—C31—C32 | 119.0 (5) | F6—C82—C83 | 117.6 (6) |
C36—C31—S1 | 125.6 (4) | C81—C82—C83 | 121.8 (7) |
C32—C31—S1 | 115.4 (4) | F7—C83—C84 | 120.2 (6) |
C33—C32—C31 | 119.2 (6) | F7—C83—C82 | 120.3 (7) |
C33—C32—H32 | 120.4 | C84—C83—C82 | 119.4 (7) |
C31—C32—H32 | 120.4 | F8—C84—C83 | 119.9 (7) |
C34—C33—C32 | 120.4 (6) | F8—C84—C85 | 119.6 (7) |
C34—C33—H33 | 119.8 | C83—C84—C85 | 120.5 (6) |
C32—C33—H33 | 119.8 | F9—C85—C84 | 121.5 (6) |
C35—C34—C33 | 120.6 (6) | F9—C85—C86 | 120.0 (7) |
C35—C34—H34 | 119.7 | C84—C85—C86 | 118.5 (7) |
C33—C34—H34 | 119.7 | F10—C86—C81 | 121.3 (5) |
C34—C35—C36 | 119.7 (6) | F10—C86—C85 | 116.9 (6) |
C34—C35—H35 | 120.1 | C81—C86—C85 | 121.7 (7) |
C36—C35—H35 | 120.1 | O4—Cl1—O1 | 112.2 (4) |
C35—C36—C31 | 121.1 (6) | O4—Cl1—O2 | 111.1 (3) |
C35—C36—H36 | 119.5 | O1—Cl1—O2 | 109.0 (3) |
C31—C36—H36 | 119.5 | O4—Cl1—O3 | 107.0 (4) |
C42—C41—C46 | 121.0 (5) | O1—Cl1—O3 | 108.5 (3) |
C42—C41—P2 | 118.1 (4) | O2—Cl1—O3 | 109.0 (3) |
C46—C41—P2 | 120.8 (4) | Cl3—C99—Cl4 | 110.0 (5) |
C43—C42—C41 | 118.0 (6) | Cl3—C99—Cl2 | 112.3 (6) |
C43—C42—H42 | 121.0 | Cl4—C99—Cl2 | 109.6 (5) |
C41—C42—H42 | 121.0 | Cl3—C99—H99 | 108.3 |
C44—C43—C42 | 120.5 (7) | Cl4—C99—H99 | 108.3 |
C44—C43—H43 | 119.8 | Cl2—C99—H99 | 108.3 |
C71—Au—P1—C21 | 139.7 (3) | Au—P2—C51—C52 | 145.4 (4) |
P2—Au—P1—C21 | −32.4 (2) | C56—C51—C52—C53 | 0.8 (8) |
C71—Au—P1—C11 | −98.5 (2) | P2—C51—C52—C53 | 177.5 (5) |
P2—Au—P1—C11 | 89.43 (17) | C51—C52—C53—C54 | 0.4 (9) |
C71—Au—P1—C1 | 19.1 (3) | C52—C53—C54—C55 | −0.1 (11) |
P2—Au—P1—C1 | −152.9 (2) | C53—C54—C55—C56 | −1.4 (12) |
C81—Au—P2—C51 | 124.4 (2) | C54—C55—C56—C51 | 2.7 (10) |
P1—Au—P2—C51 | −48.0 (2) | C52—C51—C56—C55 | −2.4 (9) |
C81—Au—P2—C41 | 0.2 (2) | P2—C51—C56—C55 | −179.0 (5) |
P1—Au—P2—C41 | −172.2 (2) | C2—S2—C61—C66 | −34.3 (6) |
C81—Au—P2—C2 | −114.8 (2) | C2—S2—C61—C62 | 146.9 (4) |
P1—Au—P2—C2 | 72.73 (19) | C66—C61—C62—C63 | −0.4 (8) |
C31—S1—C1—P1 | 144.2 (3) | S2—C61—C62—C63 | 178.4 (5) |
C21—P1—C1—S1 | 148.1 (3) | C61—C62—C63—C64 | 1.8 (9) |
C11—P1—C1—S1 | 35.3 (3) | C62—C63—C64—C65 | −1.2 (11) |
Au—P1—C1—S1 | −84.6 (3) | C63—C64—C65—C66 | −0.8 (11) |
C61—S2—C2—P2 | −161.4 (3) | C64—C65—C66—C61 | 2.2 (10) |
C51—P2—C2—S2 | 160.3 (3) | C62—C61—C66—C65 | −1.5 (9) |
C41—P2—C2—S2 | −87.6 (3) | S2—C61—C66—C65 | 179.8 (5) |
Au—P2—C2—S2 | 32.8 (3) | C81—Au—C71—C76 | −69.7 (5) |
C21—P1—C11—C12 | 138.9 (4) | P1—Au—C71—C76 | 101.8 (4) |
C1—P1—C11—C12 | −110.7 (4) | P2—Au—C71—C76 | −120.4 (6) |
Au—P1—C11—C12 | 11.9 (4) | C81—Au—C71—C72 | 97.5 (4) |
C21—P1—C11—C16 | −43.4 (5) | P1—Au—C71—C72 | −90.9 (3) |
C1—P1—C11—C16 | 66.9 (4) | P2—Au—C71—C72 | 46.9 (9) |
Au—P1—C11—C16 | −170.5 (4) | C76—C71—C72—F1 | −179.9 (5) |
C16—C11—C12—C13 | 1.5 (7) | Au—C71—C72—F1 | 12.0 (6) |
P1—C11—C12—C13 | 179.1 (4) | C76—C71—C72—C73 | −0.1 (6) |
C11—C12—C13—C14 | −1.7 (7) | Au—C71—C72—C73 | −168.2 (4) |
C12—C13—C14—C15 | −0.1 (9) | F1—C72—C73—F2 | −1.8 (7) |
C13—C14—C15—C16 | 2.0 (10) | C71—C72—C73—F2 | 178.5 (5) |
C14—C15—C16—C11 | −2.2 (10) | F1—C72—C73—C74 | 179.9 (5) |
C12—C11—C16—C15 | 0.4 (8) | C71—C72—C73—C74 | 0.2 (7) |
P1—C11—C16—C15 | −177.3 (5) | F2—C73—C74—F3 | 1.0 (8) |
C11—P1—C21—C26 | 154.3 (4) | C72—C73—C74—F3 | 179.3 (4) |
C1—P1—C21—C26 | 42.9 (5) | F2—C73—C74—C75 | −180.0 (5) |
Au—P1—C21—C26 | −82.7 (4) | C72—C73—C74—C75 | −1.7 (8) |
C11—P1—C21—C22 | −28.8 (5) | F3—C74—C75—F4 | 1.8 (8) |
C1—P1—C21—C22 | −140.3 (5) | C73—C74—C75—F4 | −177.3 (5) |
Au—P1—C21—C22 | 94.1 (4) | F3—C74—C75—C76 | −177.8 (5) |
C26—C21—C22—C23 | 0.9 (8) | C73—C74—C75—C76 | 3.1 (8) |
P1—C21—C22—C23 | −175.9 (4) | F4—C75—C76—F5 | −2.7 (8) |
C21—C22—C23—C24 | −0.4 (8) | C74—C75—C76—F5 | 176.9 (5) |
C22—C23—C24—C25 | −0.7 (10) | F4—C75—C76—C71 | 177.2 (5) |
C23—C24—C25—C26 | 1.2 (10) | C74—C75—C76—C71 | −3.2 (8) |
C22—C21—C26—C25 | −0.5 (8) | C72—C71—C76—F5 | −178.4 (4) |
P1—C21—C26—C25 | 176.4 (4) | Au—C71—C76—F5 | −10.9 (7) |
C24—C25—C26—C21 | −0.6 (9) | C72—C71—C76—C75 | 1.7 (8) |
C1—S1—C31—C36 | 19.8 (6) | Au—C71—C76—C75 | 169.2 (4) |
C1—S1—C31—C32 | −162.8 (4) | C71—Au—C81—C82 | −67.2 (4) |
C36—C31—C32—C33 | −0.1 (8) | P2—Au—C81—C82 | 103.7 (4) |
S1—C31—C32—C33 | −177.6 (4) | C71—Au—C81—C86 | 109.3 (5) |
C31—C32—C33—C34 | −1.1 (9) | P2—Au—C81—C86 | −79.8 (4) |
C32—C33—C34—C35 | 1.8 (10) | C86—C81—C82—F6 | −179.0 (6) |
C33—C34—C35—C36 | −1.3 (11) | Au—C81—C82—F6 | −2.5 (7) |
C34—C35—C36—C31 | 0.1 (10) | C86—C81—C82—C83 | 1.2 (7) |
C32—C31—C36—C35 | 0.6 (9) | Au—C81—C82—C83 | 177.7 (4) |
S1—C31—C36—C35 | 177.9 (5) | F6—C82—C83—F7 | −1.9 (7) |
C51—P2—C41—C42 | −35.7 (5) | C81—C82—C83—F7 | 177.8 (6) |
C2—P2—C41—C42 | −149.5 (4) | F6—C82—C83—C84 | 179.3 (7) |
Au—P2—C41—C42 | 95.3 (4) | C81—C82—C83—C84 | −0.9 (8) |
C51—P2—C41—C46 | 147.6 (5) | F7—C83—C84—F8 | 0.3 (11) |
C2—P2—C41—C46 | 33.9 (5) | C82—C83—C84—F8 | 179.0 (6) |
Au—P2—C41—C46 | −81.3 (5) | F7—C83—C84—C85 | −178.5 (7) |
C46—C41—C42—C43 | 1.6 (8) | C82—C83—C84—C85 | 0.3 (11) |
P2—C41—C42—C43 | −175.0 (5) | F8—C84—C85—F9 | 0.3 (13) |
C41—C42—C43—C44 | −1.3 (9) | C83—C84—C85—F9 | 179.0 (7) |
C42—C43—C44—C45 | 1.8 (11) | F8—C84—C85—C86 | −178.8 (6) |
C43—C44—C45—C46 | −2.6 (11) | C83—C84—C85—C86 | 0.0 (13) |
C44—C45—C46—C41 | 2.9 (10) | C82—C81—C86—F10 | 179.6 (5) |
C42—C41—C46—C45 | −2.4 (9) | Au—C81—C86—F10 | 2.9 (8) |
P2—C41—C46—C45 | 174.1 (5) | C82—C81—C86—C85 | −0.9 (9) |
C41—P2—C51—C56 | 90.2 (5) | Au—C81—C86—C85 | −177.7 (5) |
C2—P2—C51—C56 | −157.6 (4) | F9—C85—C86—F10 | 0.7 (10) |
Au—P2—C51—C56 | −37.9 (5) | C84—C85—C86—F10 | 179.8 (7) |
C41—P2—C51—C52 | −86.5 (5) | F9—C85—C86—C81 | −178.7 (6) |
C2—P2—C51—C52 | 25.7 (5) | C84—C85—C86—C81 | 0.4 (11) |
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2A···O3 | 0.99 | 2.49 | 3.118 (7) | 121 |
C52—H52···O3 | 0.95 | 2.41 | 3.353 (8) | 171 |
C66—H66···O3 | 0.95 | 2.61 | 3.473 (8) | 152 |
C36—H36···O1i | 0.95 | 2.60 | 3.454 (8) | 149 |
C1—H1A···O2i | 0.99 | 2.59 | 3.345 (8) | 133 |
C26—H26···O2i | 0.95 | 2.67 | 3.605 (8) | 167 |
C36—H36···O2i | 0.95 | 2.60 | 3.487 (7) | 156 |
C14—H14···O2ii | 0.95 | 2.61 | 3.328 (7) | 133 |
C15—H15···O4ii | 0.95 | 2.46 | 3.380 (8) | 163 |
Symmetry codes: (i) −x+1, y−1/2, −z+3/2; (ii) −x, y−1/2, −z+3/2. |