| Literature DB >> 27006796 |
Julian Noll1, Marcus Korb1, Heinrich Lang1.
Abstract
The structure of the title compound, [Ag(C18H15P)4]2[Ag(C6H6NO6)(C18H15P)], exhibits trigonal (P-3) symmetry, with a C 3 axis through all three complex ions, resulting in an asymmetric unit that contains one third of the atoms present in the formula unit. The formula unit thus contains two of the cations, one anion and disordered mol-ecules of methanol as the packing solvent. Attempts to refine the solvent model were unsuccessful, indicating uninter-pretable disorder. Thus, the SQUEEZE procedure in PLATON [Spek (2015 ▸). Acta Cryst. C71, 9-18] was applied, accounting for 670 electrons per unit cell, representing approximately 18 mol-ecules of methanol in the formula unit. The stated crystal data for M r, μ etc do not take these into account.Entities:
Keywords: SQUEEZE; crystal structure; non-coordinating anion; silver; triphenyl phosphine
Year: 2016 PMID: 27006796 PMCID: PMC4778820 DOI: 10.1107/S2056989016001262
Source DB: PubMed Journal: Acta Crystallogr E Crystallogr Commun
Figure 1The structures of the molecular components of (I), with displacement ellipsoids drawn at the 50% probability level. All H atoms have been omitted for clarity. [Symmetry codes: (a) −x + y + 1, −x + 2, z; (b) −y + 2, x − y + 1, z; (c/f) −x + y + 1, −x + 1, z; (d/e) −y + 1, x − y, z.]
Figure 2PLUTON cavity plot of the crystal packing of (I) in a view along [110] showing the cavities (pale red) occupied by the disordered methanol solvent. All H atoms have been omitted for clarity.
Figure 3Crystal packing of the molecular structure of (I) with the view along [001]. All H atoms have been omitted for clarity.
Experimental details
| Crystal data | |
| Chemical formula | [Ag(C18H15P)4]2[Ag(C6H6NO6)(C18H15P)] |
|
| 2872.15 |
| Crystal system, space group | Trigonal, |
| Temperature (K) | 110 |
|
| 19.0095 (5), 31.9862 (10) |
|
| 10010.0 (6) |
|
| 2 |
| Radiation type | Mo |
| μ (mm−1) | 0.40 |
| Crystal size (mm) | 0.2 × 0.2 × 0.2 |
| Data collection | |
| Diffractometer | Oxford Gemini S |
| Absorption correction | Multi-scan ( |
|
| 0.699, 1.000 |
| No. of measured, independent and observed [ | 32447, 12365, 8561 |
|
| 0.049 |
| (sin θ/λ)max (Å−1) | 0.606 |
| Refinement | |
|
| 0.066, 0.197, 1.05 |
| No. of reflections | 12365 |
| No. of parameters | 572 |
| H-atom treatment | H-atom parameters constrained |
| Δρmax, Δρmin (e Å−3) | 1.34, −0.64 |
Computer programs: CrysAlis CCD and CrysAlis RED (Oxford Diffraction, 2006 ▸), SHELXS97 and SHELXTL (Sheldrick, 2008 ▸), SHELXL2013 (Sheldrick, 2015 ▸), ORTEP-3 for Windows and WinGX (Farrugia, 2012 ▸) and publCIF (Westrip, 2010 ▸).
| [Ag(C18H15P)4]2[Ag(C6H6NO6)(C18H15P)] | |
| Mo | |
| Trigonal, | Cell parameters from 6868 reflections |
| θ = 3.3–27.6° | |
| µ = 0.40 mm−1 | |
| Block, colorless | |
| 0.2 × 0.2 × 0.2 mm |
| Oxford Gemini S diffractometer | |
| ω scans | θmax = 25.5°, θmin = 3.2° |
| Absorption correction: multi-scan ( | |
| 32447 measured reflections | |
| 12365 independent reflections | 2 standard reflections every 50 reflections |
| 8561 reflections with | intensity decay: none |
| Refinement on | 0 restraints |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| H-atom parameters constrained | |
| (Δ/σ)max = 0.001 | |
| 12365 reflections | Δρmax = 1.34 e Å−3 |
| 572 parameters | Δρmin = −0.64 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 |
| C1 | 0.9981 (4) | 1.0723 (4) | 0.77087 (17) | 0.0510 (15) | |
| H1A | 1.0514 | 1.1195 | 0.7667 | 0.061* | |
| H1B | 0.9864 | 1.0679 | 0.8006 | 0.061* | |
| C2 | 0.9347 (4) | 1.0855 (4) | 0.7476 (2) | 0.0520 (15) | |
| C3 | 1.0199 (3) | 0.9244 (3) | 0.58793 (14) | 0.0249 (10) | |
| C4 | 1.0648 (3) | 0.9386 (3) | 0.55126 (15) | 0.0290 (11) | |
| H4 | 1.0874 | 0.9891 | 0.5382 | 0.035* | |
| C5 | 1.0757 (3) | 0.8780 (3) | 0.53427 (16) | 0.0341 (12) | |
| H5 | 1.1063 | 0.8879 | 0.5100 | 0.041* | |
| C6 | 1.0413 (3) | 0.8024 (3) | 0.55318 (17) | 0.0378 (13) | |
| H6 | 1.0474 | 0.7611 | 0.5412 | 0.045* | |
| C7 | 0.9980 (3) | 0.7884 (3) | 0.58994 (18) | 0.0402 (13) | |
| H7 | 0.9758 | 0.7382 | 0.6031 | 0.048* | |
| C8 | 0.9878 (3) | 0.8493 (3) | 0.60683 (16) | 0.0317 (11) | |
| H8 | 0.9586 | 0.8397 | 0.6315 | 0.038* | |
| C9 | 0.7784 (2) | 0.4908 (3) | 0.48160 (13) | 0.0227 (9) | |
| C10 | 0.7818 (3) | 0.5545 (3) | 0.45909 (15) | 0.0278 (10) | |
| H10 | 0.7772 | 0.5951 | 0.4730 | 0.033* | |
| C11 | 0.7920 (3) | 0.5586 (3) | 0.41567 (15) | 0.0330 (11) | |
| H11 | 0.7935 | 0.6013 | 0.4007 | 0.040* | |
| C12 | 0.7997 (3) | 0.4996 (3) | 0.39533 (15) | 0.0362 (12) | |
| H12 | 0.8076 | 0.5027 | 0.3665 | 0.043* | |
| C13 | 0.7958 (3) | 0.4347 (3) | 0.41765 (17) | 0.0395 (13) | |
| H13 | 0.8003 | 0.3942 | 0.4037 | 0.047* | |
| C14 | 0.7853 (3) | 0.4306 (3) | 0.46039 (15) | 0.0304 (11) | |
| H14 | 0.7828 | 0.3873 | 0.4752 | 0.036* | |
| C15 | 0.7362 (3) | 0.5570 (3) | 0.55164 (13) | 0.0218 (9) | |
| C16 | 0.6549 (3) | 0.5326 (3) | 0.55782 (14) | 0.0257 (10) | |
| H16 | 0.6157 | 0.4781 | 0.5551 | 0.031* | |
| C17 | 0.6318 (3) | 0.5894 (3) | 0.56809 (14) | 0.0319 (11) | |
| H17 | 0.5772 | 0.5723 | 0.5725 | 0.038* | |
| C18 | 0.6885 (3) | 0.6700 (3) | 0.57182 (15) | 0.0345 (12) | |
| H18 | 0.6725 | 0.7076 | 0.5783 | 0.041* | |
| C19 | 0.7696 (3) | 0.6952 (3) | 0.56595 (16) | 0.0372 (12) | |
| H19 | 0.8081 | 0.7499 | 0.5688 | 0.045* | |
| C20 | 0.7945 (3) | 0.6395 (3) | 0.55582 (14) | 0.0284 (10) | |
| H20 | 0.8492 | 0.6569 | 0.5519 | 0.034* | |
| C21 | 0.8692 (3) | 0.5295 (2) | 0.55785 (14) | 0.0216 (9) | |
| C22 | 0.9362 (3) | 0.5552 (3) | 0.53165 (15) | 0.0275 (10) | |
| H22 | 0.9289 | 0.5481 | 0.5029 | 0.033* | |
| C23 | 1.0147 (3) | 0.5917 (3) | 0.54861 (16) | 0.0348 (12) | |
| H23 | 1.0594 | 0.6084 | 0.5312 | 0.042* | |
| C24 | 1.0255 (3) | 0.6028 (3) | 0.59136 (16) | 0.0350 (12) | |
| H24 | 1.0775 | 0.6275 | 0.6027 | 0.042* | |
| C25 | 0.9584 (3) | 0.5770 (3) | 0.61745 (16) | 0.0324 (11) | |
| H25 | 0.9655 | 0.5848 | 0.6462 | 0.039* | |
| C26 | 0.8818 (3) | 0.5399 (3) | 0.60066 (15) | 0.0286 (10) | |
| H26 | 0.8373 | 0.5213 | 0.6184 | 0.034* | |
| C27 | 0.7674 (3) | 0.3799 (3) | 0.67114 (13) | 0.0263 (10) | |
| C28 | 0.7918 (3) | 0.4372 (3) | 0.70267 (14) | 0.0293 (11) | |
| H28 | 0.7561 | 0.4534 | 0.7126 | 0.035* | |
| C29 | 0.8694 (3) | 0.4708 (3) | 0.71949 (14) | 0.0367 (12) | |
| H29 | 0.8862 | 0.5106 | 0.7400 | 0.044* | |
| C30 | 0.9217 (3) | 0.4449 (3) | 0.70572 (15) | 0.0388 (13) | |
| H30 | 0.9729 | 0.4661 | 0.7177 | 0.047* | |
| C31 | 0.8982 (3) | 0.3876 (3) | 0.67416 (16) | 0.0392 (13) | |
| H31 | 0.9336 | 0.3707 | 0.6647 | 0.047* | |
| C32 | 0.8219 (3) | 0.3560 (3) | 0.65699 (15) | 0.0323 (11) | |
| H32 | 0.8062 | 0.3180 | 0.6356 | 0.039* | |
| C33 | 0.7197 (3) | 0.4342 (3) | 0.83069 (14) | 0.0324 (11) | |
| C34 | 0.7969 (4) | 0.4884 (3) | 0.84516 (16) | 0.0457 (14) | |
| H34 | 0.8199 | 0.4729 | 0.8663 | 0.055* | |
| C35 | 0.8402 (4) | 0.5664 (4) | 0.82803 (17) | 0.0517 (16) | |
| H35 | 0.8922 | 0.6027 | 0.8376 | 0.062* | |
| C36 | 0.8046 (4) | 0.5899 (4) | 0.79617 (16) | 0.0465 (14) | |
| H36 | 0.8325 | 0.6419 | 0.7849 | 0.056* | |
| C37 | 0.7297 (3) | 0.5358 (3) | 0.78221 (16) | 0.0390 (13) | |
| H37 | 0.7064 | 0.5510 | 0.7611 | 0.047* | |
| C38 | 0.6863 (3) | 0.4572 (3) | 0.79896 (14) | 0.0372 (12) | |
| H38 | 0.6350 | 0.4206 | 0.7887 | 0.045* | |
| C39 | 0.8225 (4) | 0.4078 (5) | 1.0209 (2) | 0.073 (2) | |
| C40 | 0.7801 (4) | 0.3373 (4) | 1.04272 (19) | 0.067 (2) | |
| H40 | 0.7470 | 0.2900 | 1.0279 | 0.080* | |
| C41 | 0.7834 (5) | 0.3322 (7) | 1.0857 (3) | 0.126 (5) | |
| H41 | 0.7567 | 0.2825 | 1.0995 | 0.152* | |
| C42 | 0.8294 (5) | 0.4061 (6) | 1.1079 (2) | 0.088 (3) | |
| H42 | 0.8292 | 0.4063 | 1.1369 | 0.106* | |
| C43 | 0.8754 (5) | 0.4791 (6) | 1.0857 (2) | 0.080 (2) | |
| H43 | 0.9086 | 0.5266 | 1.1004 | 0.096* | |
| C44 | 0.8725 (4) | 0.4820 (5) | 1.0421 (2) | 0.077 (2) | |
| H44 | 0.9021 | 0.5306 | 1.0276 | 0.092* | |
| C45 | 0.8742 (4) | 0.3609 (4) | 0.9471 (2) | 0.0607 (18) | |
| C46 | 0.8732 (4) | 0.3449 (4) | 0.90415 (18) | 0.0551 (17) | |
| H46 | 0.8444 | 0.3588 | 0.8856 | 0.066* | |
| C47 | 0.9159 (5) | 0.3081 (6) | 0.8899 (3) | 0.090 (3) | |
| H47 | 0.9131 | 0.2939 | 0.8619 | 0.108* | |
| C48 | 0.9638 (5) | 0.2919 (5) | 0.9180 (3) | 0.084 (2) | |
| H48 | 0.9943 | 0.2693 | 0.9084 | 0.101* | |
| C49 | 0.9645 (4) | 0.3106 (4) | 0.9606 (2) | 0.071 (2) | |
| H49 | 0.9952 | 0.2992 | 0.9791 | 0.086* | |
| C50 | 0.9200 (4) | 0.3458 (4) | 0.9760 (3) | 0.069 (2) | |
| H50 | 0.9211 | 0.3585 | 1.0042 | 0.083* | |
| C51 | 0.8718 (4) | 0.5109 (4) | 0.9494 (2) | 0.0674 (19) | |
| C52 | 0.8434 (3) | 0.5648 (4) | 0.95708 (19) | 0.0499 (15) | |
| H52 | 0.7919 | 0.5433 | 0.9688 | 0.060* | |
| C53 | 0.8828 (5) | 0.6430 (5) | 0.9493 (3) | 0.104 (3) | |
| H53 | 0.8630 | 0.6765 | 0.9578 | 0.124* | |
| C54 | 0.9596 (5) | 0.6749 (5) | 0.9266 (3) | 0.082 (2) | |
| H54 | 0.9871 | 0.7285 | 0.9173 | 0.098* | |
| C55 | 0.9905 (5) | 0.6236 (5) | 0.9190 (2) | 0.074 (2) | |
| H55 | 1.0408 | 0.6451 | 0.9059 | 0.088* | |
| C56 | 0.9503 (4) | 0.5414 (5) | 0.93011 (19) | 0.067 (2) | |
| H56 | 0.9728 | 0.5085 | 0.9253 | 0.080* | |
| O1 | 0.9044 (2) | 1.0481 (2) | 0.71512 (12) | 0.0467 (10) | |
| O2 | 0.9195 (3) | 1.1367 (3) | 0.76428 (15) | 0.0755 (14) | |
| P1 | 1.0000 | 1.0000 | 0.61143 (6) | 0.0240 (4) | |
| P2 | 0.76469 (7) | 0.48109 (7) | 0.53863 (4) | 0.0214 (3) | |
| P3 | 0.6667 | 0.3333 | 0.64650 (6) | 0.0230 (4) | |
| P4 | 0.6667 | 0.3333 | 0.85547 (7) | 0.0315 (5) | |
| P5 | 0.81418 (9) | 0.40685 (9) | 0.96398 (4) | 0.0393 (3) | |
| Ag1 | 1.0000 | 1.0000 | 0.68457 (2) | 0.03511 (19) | |
| Ag2 | 0.6667 | 0.3333 | 0.56556 (2) | 0.01929 (15) | |
| Ag3 | 0.6667 | 0.3333 | 0.93618 (2) | 0.03244 (18) | |
| N1 | 1.0000 | 1.0000 | 0.7572 (2) | 0.0305 (16) |
| C1 | 0.074 (4) | 0.047 (3) | 0.034 (3) | 0.032 (3) | 0.005 (3) | −0.003 (3) |
| C2 | 0.061 (4) | 0.053 (4) | 0.055 (4) | 0.038 (3) | 0.007 (3) | −0.002 (3) |
| C3 | 0.020 (2) | 0.022 (2) | 0.034 (3) | 0.012 (2) | −0.001 (2) | −0.001 (2) |
| C4 | 0.028 (3) | 0.026 (2) | 0.037 (3) | 0.016 (2) | −0.003 (2) | 0.001 (2) |
| C5 | 0.030 (3) | 0.037 (3) | 0.040 (3) | 0.020 (2) | −0.001 (2) | −0.002 (2) |
| C6 | 0.030 (3) | 0.029 (3) | 0.058 (3) | 0.017 (2) | −0.004 (3) | −0.013 (2) |
| C7 | 0.034 (3) | 0.022 (3) | 0.062 (4) | 0.012 (2) | 0.002 (3) | −0.001 (2) |
| C8 | 0.028 (3) | 0.028 (3) | 0.040 (3) | 0.015 (2) | 0.002 (2) | −0.001 (2) |
| C9 | 0.013 (2) | 0.024 (2) | 0.029 (2) | 0.0080 (19) | −0.0010 (18) | −0.0022 (19) |
| C10 | 0.025 (2) | 0.023 (2) | 0.035 (3) | 0.012 (2) | 0.003 (2) | 0.002 (2) |
| C11 | 0.035 (3) | 0.036 (3) | 0.031 (3) | 0.019 (2) | 0.001 (2) | 0.011 (2) |
| C12 | 0.030 (3) | 0.048 (3) | 0.027 (3) | 0.016 (2) | 0.003 (2) | −0.001 (2) |
| C13 | 0.038 (3) | 0.035 (3) | 0.045 (3) | 0.018 (3) | 0.005 (2) | −0.007 (2) |
| C14 | 0.027 (3) | 0.025 (2) | 0.038 (3) | 0.012 (2) | 0.003 (2) | 0.003 (2) |
| C15 | 0.025 (2) | 0.022 (2) | 0.021 (2) | 0.013 (2) | 0.0014 (18) | 0.0025 (18) |
| C16 | 0.023 (2) | 0.023 (2) | 0.031 (2) | 0.012 (2) | 0.000 (2) | 0.0026 (19) |
| C17 | 0.024 (3) | 0.044 (3) | 0.034 (3) | 0.022 (2) | 0.001 (2) | 0.002 (2) |
| C18 | 0.042 (3) | 0.036 (3) | 0.038 (3) | 0.029 (3) | 0.000 (2) | −0.002 (2) |
| C19 | 0.039 (3) | 0.022 (3) | 0.048 (3) | 0.014 (2) | −0.002 (2) | 0.000 (2) |
| C20 | 0.024 (2) | 0.023 (2) | 0.037 (3) | 0.011 (2) | 0.003 (2) | 0.002 (2) |
| C21 | 0.020 (2) | 0.015 (2) | 0.031 (2) | 0.0096 (18) | 0.0005 (19) | 0.0052 (18) |
| C22 | 0.026 (2) | 0.025 (2) | 0.030 (2) | 0.012 (2) | 0.005 (2) | 0.005 (2) |
| C23 | 0.018 (2) | 0.033 (3) | 0.046 (3) | 0.007 (2) | 0.006 (2) | 0.007 (2) |
| C24 | 0.023 (3) | 0.030 (3) | 0.050 (3) | 0.012 (2) | −0.010 (2) | −0.002 (2) |
| C25 | 0.030 (3) | 0.025 (3) | 0.036 (3) | 0.010 (2) | −0.005 (2) | 0.002 (2) |
| C26 | 0.025 (2) | 0.025 (2) | 0.036 (3) | 0.012 (2) | 0.008 (2) | 0.010 (2) |
| C27 | 0.022 (2) | 0.033 (3) | 0.019 (2) | 0.011 (2) | −0.0023 (19) | 0.003 (2) |
| C28 | 0.034 (3) | 0.029 (3) | 0.023 (2) | 0.014 (2) | 0.000 (2) | 0.001 (2) |
| C29 | 0.036 (3) | 0.040 (3) | 0.021 (2) | 0.010 (2) | −0.007 (2) | −0.001 (2) |
| C30 | 0.027 (3) | 0.043 (3) | 0.030 (3) | 0.006 (2) | −0.006 (2) | 0.006 (2) |
| C31 | 0.033 (3) | 0.051 (3) | 0.039 (3) | 0.025 (3) | 0.000 (2) | 0.007 (3) |
| C32 | 0.035 (3) | 0.032 (3) | 0.028 (2) | 0.015 (2) | −0.003 (2) | 0.001 (2) |
| C33 | 0.039 (3) | 0.041 (3) | 0.020 (2) | 0.022 (3) | −0.003 (2) | −0.004 (2) |
| C34 | 0.053 (4) | 0.045 (3) | 0.033 (3) | 0.021 (3) | −0.008 (3) | 0.005 (3) |
| C35 | 0.055 (4) | 0.044 (3) | 0.043 (3) | 0.015 (3) | −0.014 (3) | −0.005 (3) |
| C36 | 0.061 (4) | 0.042 (3) | 0.029 (3) | 0.021 (3) | 0.004 (3) | 0.002 (2) |
| C37 | 0.054 (4) | 0.044 (3) | 0.030 (3) | 0.032 (3) | 0.000 (2) | 0.002 (2) |
| C38 | 0.047 (3) | 0.048 (3) | 0.022 (2) | 0.027 (3) | 0.000 (2) | −0.003 (2) |
| C39 | 0.044 (4) | 0.088 (6) | 0.051 (4) | 0.008 (4) | −0.017 (3) | 0.001 (4) |
| C40 | 0.052 (4) | 0.058 (4) | 0.041 (3) | −0.011 (3) | −0.017 (3) | 0.001 (3) |
| C41 | 0.056 (5) | 0.159 (9) | 0.069 (5) | −0.018 (6) | −0.032 (4) | 0.040 (6) |
| C42 | 0.065 (5) | 0.139 (8) | 0.044 (4) | 0.039 (5) | 0.004 (4) | 0.005 (5) |
| C43 | 0.069 (5) | 0.114 (7) | 0.058 (4) | 0.047 (5) | −0.016 (4) | −0.020 (5) |
| C44 | 0.054 (4) | 0.115 (7) | 0.062 (4) | 0.044 (5) | −0.022 (4) | −0.036 (4) |
| C45 | 0.039 (3) | 0.065 (4) | 0.061 (4) | 0.013 (3) | −0.012 (3) | −0.008 (3) |
| C46 | 0.055 (4) | 0.086 (5) | 0.042 (3) | 0.048 (4) | −0.019 (3) | −0.021 (3) |
| C47 | 0.070 (5) | 0.123 (7) | 0.079 (5) | 0.051 (5) | −0.026 (4) | −0.033 (5) |
| C48 | 0.070 (5) | 0.075 (5) | 0.107 (7) | 0.035 (4) | −0.019 (5) | −0.015 (5) |
| C49 | 0.066 (5) | 0.073 (5) | 0.073 (5) | 0.034 (4) | −0.024 (4) | −0.015 (4) |
| C50 | 0.047 (4) | 0.050 (4) | 0.103 (6) | 0.020 (3) | −0.035 (4) | −0.009 (4) |
| C51 | 0.053 (4) | 0.060 (4) | 0.082 (5) | 0.023 (4) | −0.023 (4) | −0.006 (4) |
| C52 | 0.032 (3) | 0.054 (4) | 0.060 (4) | 0.018 (3) | −0.005 (3) | 0.002 (3) |
| C53 | 0.063 (5) | 0.058 (5) | 0.176 (10) | 0.019 (4) | −0.042 (6) | 0.008 (5) |
| C54 | 0.065 (5) | 0.063 (5) | 0.102 (6) | 0.021 (4) | −0.020 (5) | 0.008 (4) |
| C55 | 0.055 (4) | 0.081 (6) | 0.071 (5) | 0.023 (4) | −0.004 (4) | 0.004 (4) |
| C56 | 0.042 (4) | 0.074 (5) | 0.049 (4) | 0.003 (3) | −0.009 (3) | 0.015 (3) |
| O1 | 0.057 (2) | 0.059 (3) | 0.042 (2) | 0.042 (2) | −0.0079 (19) | −0.009 (2) |
| O2 | 0.101 (4) | 0.089 (4) | 0.070 (3) | 0.073 (3) | −0.002 (3) | −0.014 (3) |
| P1 | 0.0213 (6) | 0.0213 (6) | 0.0294 (11) | 0.0106 (3) | 0.000 | 0.000 |
| P2 | 0.0181 (6) | 0.0159 (6) | 0.0278 (6) | 0.0068 (5) | 0.0022 (5) | 0.0028 (5) |
| P3 | 0.0246 (6) | 0.0246 (6) | 0.0199 (10) | 0.0123 (3) | 0.000 | 0.000 |
| P4 | 0.0368 (8) | 0.0368 (8) | 0.0208 (10) | 0.0184 (4) | 0.000 | 0.000 |
| P5 | 0.0368 (8) | 0.0461 (8) | 0.0302 (7) | 0.0171 (7) | −0.0067 (6) | −0.0058 (6) |
| Ag1 | 0.0379 (3) | 0.0379 (3) | 0.0295 (3) | 0.01896 (13) | 0.000 | 0.000 |
| Ag2 | 0.0183 (2) | 0.0183 (2) | 0.0213 (3) | 0.00914 (10) | 0.000 | 0.000 |
| Ag3 | 0.0367 (3) | 0.0367 (3) | 0.0239 (3) | 0.01836 (13) | 0.000 | 0.000 |
| N1 | 0.029 (2) | 0.029 (2) | 0.034 (4) | 0.0144 (11) | 0.000 | 0.000 |
| C1—N1 | 1.460 (6) | C33—P4 | 1.841 (5) |
| C1—C2 | 1.541 (9) | C34—C35 | 1.399 (8) |
| C1—H1A | 0.9700 | C34—H34 | 0.9300 |
| C1—H1B | 0.9700 | C35—C36 | 1.413 (8) |
| C2—O1 | 1.227 (7) | C35—H35 | 0.9300 |
| C2—O2 | 1.263 (7) | C36—C37 | 1.349 (8) |
| C3—C8 | 1.380 (6) | C36—H36 | 0.9300 |
| C3—C4 | 1.395 (6) | C37—C38 | 1.402 (7) |
| C3—P1 | 1.821 (4) | C37—H37 | 0.9300 |
| C4—C5 | 1.381 (7) | C38—H38 | 0.9300 |
| C4—H4 | 0.9300 | C39—C40 | 1.361 (9) |
| C5—C6 | 1.385 (7) | C39—C44 | 1.420 (10) |
| C5—H5 | 0.9300 | C39—P5 | 1.826 (7) |
| C6—C7 | 1.384 (7) | C40—C41 | 1.381 (9) |
| C6—H6 | 0.9300 | C40—H40 | 0.9300 |
| C7—C8 | 1.376 (7) | C41—C42 | 1.419 (13) |
| C7—H7 | 0.9300 | C41—H41 | 0.9300 |
| C8—H8 | 0.9300 | C42—C43 | 1.407 (11) |
| C9—C10 | 1.382 (6) | C42—H42 | 0.9300 |
| C9—C14 | 1.393 (6) | C43—C44 | 1.397 (10) |
| C9—P2 | 1.839 (5) | C43—H43 | 0.9300 |
| C10—C11 | 1.399 (6) | C44—H44 | 0.9300 |
| C10—H10 | 0.9300 | C45—C50 | 1.395 (9) |
| C11—C12 | 1.367 (7) | C45—C46 | 1.406 (8) |
| C11—H11 | 0.9300 | C45—P5 | 1.830 (7) |
| C12—C13 | 1.396 (7) | C46—C47 | 1.388 (10) |
| C12—H12 | 0.9300 | C46—H46 | 0.9300 |
| C13—C14 | 1.378 (7) | C47—C48 | 1.417 (11) |
| C13—H13 | 0.9300 | C47—H47 | 0.9300 |
| C14—H14 | 0.9300 | C48—C49 | 1.406 (10) |
| C15—C16 | 1.387 (6) | C48—H48 | 0.9300 |
| C15—C20 | 1.403 (6) | C49—C50 | 1.404 (10) |
| C15—P2 | 1.824 (4) | C49—H49 | 0.9300 |
| C16—C17 | 1.392 (6) | C50—H50 | 0.9300 |
| C16—H16 | 0.9300 | C51—C52 | 1.399 (9) |
| C17—C18 | 1.368 (7) | C51—C56 | 1.441 (10) |
| C17—H17 | 0.9300 | C51—P5 | 1.778 (7) |
| C18—C19 | 1.379 (7) | C52—C53 | 1.310 (10) |
| C18—H18 | 0.9300 | C52—H52 | 0.9300 |
| C19—C20 | 1.397 (7) | C53—C54 | 1.464 (12) |
| C19—H19 | 0.9300 | C53—H53 | 0.9300 |
| C20—H20 | 0.9300 | C54—C55 | 1.388 (11) |
| C21—C26 | 1.387 (6) | C54—H54 | 0.9300 |
| C21—C22 | 1.394 (6) | C55—C56 | 1.399 (10) |
| C21—P2 | 1.828 (4) | C55—H55 | 0.9300 |
| C22—C23 | 1.403 (6) | C56—H56 | 0.9300 |
| C22—H22 | 0.9300 | O1—Ag1 | 2.599 (4) |
| C23—C24 | 1.383 (7) | P1—C3i | 1.821 (4) |
| C23—H23 | 0.9300 | P1—C3ii | 1.821 (5) |
| C24—C25 | 1.392 (7) | P1—Ag1 | 2.339 (2) |
| C24—H24 | 0.9300 | P2—Ag2 | 2.6210 (11) |
| C25—C26 | 1.370 (6) | P3—C27iii | 1.838 (5) |
| C25—H25 | 0.9300 | P3—C27iv | 1.838 (4) |
| C26—H26 | 0.9300 | P3—Ag2 | 2.589 (2) |
| C27—C28 | 1.384 (6) | P4—C33iii | 1.841 (5) |
| C27—C32 | 1.397 (7) | P4—C33iv | 1.841 (5) |
| C27—P3 | 1.838 (4) | P4—Ag3 | 2.582 (2) |
| C28—C29 | 1.391 (7) | P5—Ag3 | 2.5862 (14) |
| C28—H28 | 0.9300 | Ag1—N1 | 2.324 (7) |
| C29—C30 | 1.382 (8) | Ag1—O1ii | 2.599 (4) |
| C29—H29 | 0.9300 | Ag1—O1i | 2.599 (4) |
| C30—C31 | 1.385 (7) | Ag2—P2iii | 2.6210 (11) |
| C30—H30 | 0.9300 | Ag2—P2iv | 2.6211 (11) |
| C31—C32 | 1.378 (7) | Ag3—P5iii | 2.5861 (14) |
| C31—H31 | 0.9300 | Ag3—P5iv | 2.5861 (14) |
| C32—H32 | 0.9300 | N1—C1i | 1.460 (6) |
| C33—C38 | 1.379 (7) | N1—C1ii | 1.460 (6) |
| C33—C34 | 1.384 (7) | ||
| N1—C1—C2 | 113.5 (5) | C33—C38—H38 | 120.0 |
| N1—C1—H1A | 108.9 | C37—C38—H38 | 120.0 |
| C2—C1—H1A | 108.9 | C40—C39—C44 | 120.4 (6) |
| N1—C1—H1B | 108.9 | C40—C39—P5 | 119.8 (5) |
| C2—C1—H1B | 108.9 | C44—C39—P5 | 119.9 (6) |
| H1A—C1—H1B | 107.7 | C39—C40—C41 | 123.7 (7) |
| O1—C2—O2 | 125.7 (6) | C39—C40—H40 | 118.1 |
| O1—C2—C1 | 119.6 (5) | C41—C40—H40 | 118.1 |
| O2—C2—C1 | 114.8 (6) | C40—C41—C42 | 117.0 (8) |
| C8—C3—C4 | 118.7 (4) | C40—C41—H41 | 121.5 |
| C8—C3—P1 | 118.4 (3) | C42—C41—H41 | 121.5 |
| C4—C3—P1 | 122.9 (3) | C43—C42—C41 | 119.7 (7) |
| C5—C4—C3 | 120.1 (5) | C43—C42—H42 | 120.1 |
| C5—C4—H4 | 119.9 | C41—C42—H42 | 120.1 |
| C3—C4—H4 | 119.9 | C44—C43—C42 | 121.7 (8) |
| C4—C5—C6 | 120.3 (5) | C44—C43—H43 | 119.2 |
| C4—C5—H5 | 119.9 | C42—C43—H43 | 119.2 |
| C6—C5—H5 | 119.9 | C43—C44—C39 | 117.2 (8) |
| C7—C6—C5 | 119.8 (5) | C43—C44—H44 | 121.4 |
| C7—C6—H6 | 120.1 | C39—C44—H44 | 121.4 |
| C5—C6—H6 | 120.1 | C50—C45—C46 | 123.0 (7) |
| C8—C7—C6 | 119.6 (5) | C50—C45—P5 | 120.4 (6) |
| C8—C7—H7 | 120.2 | C46—C45—P5 | 116.6 (5) |
| C6—C7—H7 | 120.2 | C47—C46—C45 | 118.8 (6) |
| C7—C8—C3 | 121.5 (5) | C47—C46—H46 | 120.6 |
| C7—C8—H8 | 119.2 | C45—C46—H46 | 120.6 |
| C3—C8—H8 | 119.2 | C46—C47—C48 | 120.3 (7) |
| C10—C9—C14 | 119.0 (4) | C46—C47—H47 | 119.9 |
| C10—C9—P2 | 123.2 (3) | C48—C47—H47 | 119.9 |
| C14—C9—P2 | 117.8 (3) | C49—C48—C47 | 119.0 (8) |
| C9—C10—C11 | 120.7 (4) | C49—C48—H48 | 120.5 |
| C9—C10—H10 | 119.7 | C47—C48—H48 | 120.5 |
| C11—C10—H10 | 119.7 | C50—C49—C48 | 121.9 (7) |
| C12—C11—C10 | 119.7 (4) | C50—C49—H49 | 119.0 |
| C12—C11—H11 | 120.1 | C48—C49—H49 | 119.0 |
| C10—C11—H11 | 120.1 | C45—C50—C49 | 116.9 (7) |
| C11—C12—C13 | 120.2 (5) | C45—C50—H50 | 121.5 |
| C11—C12—H12 | 119.9 | C49—C50—H50 | 121.5 |
| C13—C12—H12 | 119.9 | C52—C51—C56 | 118.8 (7) |
| C14—C13—C12 | 120.0 (5) | C52—C51—P5 | 121.3 (6) |
| C14—C13—H13 | 120.0 | C56—C51—P5 | 119.9 (6) |
| C12—C13—H13 | 120.0 | C53—C52—C51 | 125.9 (7) |
| C13—C14—C9 | 120.5 (4) | C53—C52—H52 | 117.1 |
| C13—C14—H14 | 119.8 | C51—C52—H52 | 117.1 |
| C9—C14—H14 | 119.8 | C52—C53—C54 | 116.9 (8) |
| C16—C15—C20 | 119.0 (4) | C52—C53—H53 | 121.6 |
| C16—C15—P2 | 119.4 (3) | C54—C53—H53 | 121.6 |
| C20—C15—P2 | 121.7 (3) | C55—C54—C53 | 118.6 (8) |
| C15—C16—C17 | 120.4 (4) | C55—C54—H54 | 120.7 |
| C15—C16—H16 | 119.8 | C53—C54—H54 | 120.7 |
| C17—C16—H16 | 119.8 | C54—C55—C56 | 123.6 (8) |
| C18—C17—C16 | 120.7 (4) | C54—C55—H55 | 118.2 |
| C18—C17—H17 | 119.7 | C56—C55—H55 | 118.2 |
| C16—C17—H17 | 119.7 | C55—C56—C51 | 115.8 (8) |
| C17—C18—C19 | 119.7 (5) | C55—C56—H56 | 122.1 |
| C17—C18—H18 | 120.1 | C51—C56—H56 | 122.1 |
| C19—C18—H18 | 120.1 | C2—O1—Ag1 | 108.3 (4) |
| C18—C19—C20 | 120.8 (5) | C3i—P1—C3ii | 104.14 (18) |
| C18—C19—H19 | 119.6 | C3i—P1—C3 | 104.14 (18) |
| C20—C19—H19 | 119.6 | C3ii—P1—C3 | 104.14 (18) |
| C19—C20—C15 | 119.5 (4) | C3i—P1—Ag1 | 114.39 (15) |
| C19—C20—H20 | 120.3 | C3ii—P1—Ag1 | 114.39 (15) |
| C15—C20—H20 | 120.3 | C3—P1—Ag1 | 114.39 (15) |
| C26—C21—C22 | 118.7 (4) | C15—P2—C21 | 101.7 (2) |
| C26—C21—P2 | 118.1 (3) | C15—P2—C9 | 103.28 (19) |
| C22—C21—P2 | 123.2 (3) | C21—P2—C9 | 102.69 (19) |
| C21—C22—C23 | 120.1 (4) | C15—P2—Ag2 | 116.05 (14) |
| C21—C22—H22 | 120.0 | C21—P2—Ag2 | 116.10 (14) |
| C23—C22—H22 | 120.0 | C9—P2—Ag2 | 115.02 (14) |
| C24—C23—C22 | 119.8 (4) | C27iii—P3—C27iv | 102.95 (17) |
| C24—C23—H23 | 120.1 | C27iii—P3—C27 | 102.95 (17) |
| C22—C23—H23 | 120.1 | C27iv—P3—C27 | 102.95 (17) |
| C23—C24—C25 | 120.0 (4) | C27iii—P3—Ag2 | 115.39 (15) |
| C23—C24—H24 | 120.0 | C27iv—P3—Ag2 | 115.39 (15) |
| C25—C24—H24 | 120.0 | C27—P3—Ag2 | 115.40 (15) |
| C26—C25—C24 | 119.8 (5) | C33—P4—C33iii | 102.83 (18) |
| C26—C25—H25 | 120.1 | C33—P4—C33iv | 102.83 (18) |
| C24—C25—H25 | 120.1 | C33iii—P4—C33iv | 102.83 (18) |
| C25—C26—C21 | 121.6 (4) | C33—P4—Ag3 | 115.49 (15) |
| C25—C26—H26 | 119.2 | C33iii—P4—Ag3 | 115.50 (15) |
| C21—C26—H26 | 119.2 | C33iv—P4—Ag3 | 115.50 (15) |
| C28—C27—C32 | 118.8 (4) | C51—P5—C39 | 104.4 (3) |
| C28—C27—P3 | 123.3 (4) | C51—P5—C45 | 105.6 (3) |
| C32—C27—P3 | 117.9 (3) | C39—P5—C45 | 103.1 (3) |
| C27—C28—C29 | 120.2 (5) | C51—P5—Ag3 | 114.1 (2) |
| C27—C28—H28 | 119.9 | C39—P5—Ag3 | 114.4 (2) |
| C29—C28—H28 | 119.9 | C45—P5—Ag3 | 114.0 (2) |
| C30—C29—C28 | 120.0 (5) | N1—Ag1—P1 | 180.0 |
| C30—C29—H29 | 120.0 | N1—Ag1—O1ii | 67.92 (8) |
| C28—C29—H29 | 120.0 | P1—Ag1—O1ii | 112.08 (8) |
| C29—C30—C31 | 120.4 (5) | N1—Ag1—O1i | 67.92 (8) |
| C29—C30—H30 | 119.8 | P1—Ag1—O1i | 112.08 (8) |
| C31—C30—H30 | 119.8 | O1ii—Ag1—O1i | 106.74 (9) |
| C32—C31—C30 | 119.2 (5) | N1—Ag1—O1 | 67.92 (8) |
| C32—C31—H31 | 120.4 | P1—Ag1—O1 | 112.08 (8) |
| C30—C31—H31 | 120.4 | O1ii—Ag1—O1 | 106.74 (9) |
| C31—C32—C27 | 121.3 (5) | O1i—Ag1—O1 | 106.74 (9) |
| C31—C32—H32 | 119.4 | P3—Ag2—P2iii | 109.19 (3) |
| C27—C32—H32 | 119.4 | P3—Ag2—P2 | 109.19 (3) |
| C38—C33—C34 | 119.7 (5) | P2iii—Ag2—P2 | 109.75 (3) |
| C38—C33—P4 | 123.2 (4) | P3—Ag2—P2iv | 109.19 (3) |
| C34—C33—P4 | 117.1 (4) | P2iii—Ag2—P2iv | 109.75 (3) |
| C33—C34—C35 | 120.1 (5) | P2—Ag2—P2iv | 109.75 (3) |
| C33—C34—H34 | 120.0 | P4—Ag3—P5iii | 110.11 (3) |
| C35—C34—H34 | 120.0 | P4—Ag3—P5iv | 110.11 (3) |
| C34—C35—C36 | 119.7 (6) | P5iii—Ag3—P5iv | 108.83 (3) |
| C34—C35—H35 | 120.1 | P4—Ag3—P5 | 110.11 (3) |
| C36—C35—H35 | 120.1 | P5iii—Ag3—P5 | 108.83 (3) |
| C37—C36—C35 | 119.2 (5) | P5iv—Ag3—P5 | 108.82 (3) |
| C37—C36—H36 | 120.4 | C1—N1—C1i | 111.5 (3) |
| C35—C36—H36 | 120.4 | C1—N1—C1ii | 111.5 (3) |
| C36—C37—C38 | 121.3 (5) | C1i—N1—C1ii | 111.5 (3) |
| C36—C37—H37 | 119.3 | C1—N1—Ag1 | 107.4 (3) |
| C38—C37—H37 | 119.3 | C1i—N1—Ag1 | 107.4 (3) |
| C33—C38—C37 | 120.0 (5) | C1ii—N1—Ag1 | 107.4 (3) |
| N1—C1—C2—O1 | −15.2 (8) | P5—C51—C52—C53 | 176.6 (7) |
| N1—C1—C2—O2 | 165.8 (5) | C51—C52—C53—C54 | 6.8 (12) |
| C8—C3—C4—C5 | 0.7 (7) | C52—C53—C54—C55 | −7.4 (12) |
| P1—C3—C4—C5 | −178.0 (4) | C53—C54—C55—C56 | 3.4 (12) |
| C3—C4—C5—C6 | 0.8 (7) | C54—C55—C56—C51 | 1.5 (10) |
| C4—C5—C6—C7 | −2.0 (8) | C52—C51—C56—C55 | −2.6 (9) |
| C5—C6—C7—C8 | 1.5 (8) | P5—C51—C56—C55 | 178.9 (5) |
| C6—C7—C8—C3 | 0.0 (8) | O2—C2—O1—Ag1 | 158.1 (6) |
| C4—C3—C8—C7 | −1.1 (7) | C1—C2—O1—Ag1 | −20.8 (7) |
| P1—C3—C8—C7 | 177.6 (4) | C8—C3—P1—C3i | −88.0 (5) |
| C14—C9—C10—C11 | 0.0 (7) | C4—C3—P1—C3i | 90.7 (3) |
| P2—C9—C10—C11 | −179.7 (3) | C8—C3—P1—C3ii | 163.2 (4) |
| C9—C10—C11—C12 | −0.8 (7) | C4—C3—P1—C3ii | −18.1 (4) |
| C10—C11—C12—C13 | 1.3 (7) | C8—C3—P1—Ag1 | 37.6 (4) |
| C11—C12—C13—C14 | −1.0 (8) | C4—C3—P1—Ag1 | −143.7 (3) |
| C12—C13—C14—C9 | 0.1 (7) | C16—C15—P2—C21 | −154.3 (4) |
| C10—C9—C14—C13 | 0.3 (7) | C20—C15—P2—C21 | 25.4 (4) |
| P2—C9—C14—C13 | −179.9 (4) | C16—C15—P2—C9 | 99.5 (4) |
| C20—C15—C16—C17 | −0.1 (7) | C20—C15—P2—C9 | −80.9 (4) |
| P2—C15—C16—C17 | 179.5 (3) | C16—C15—P2—Ag2 | −27.3 (4) |
| C15—C16—C17—C18 | 0.7 (7) | C20—C15—P2—Ag2 | 152.3 (3) |
| C16—C17—C18—C19 | −0.9 (7) | C26—C21—P2—C15 | 67.2 (4) |
| C17—C18—C19—C20 | 0.6 (8) | C22—C21—P2—C15 | −113.8 (4) |
| C18—C19—C20—C15 | −0.1 (7) | C26—C21—P2—C9 | 173.8 (3) |
| C16—C15—C20—C19 | −0.2 (7) | C22—C21—P2—C9 | −7.1 (4) |
| P2—C15—C20—C19 | −179.8 (4) | C26—C21—P2—Ag2 | −59.8 (4) |
| C26—C21—C22—C23 | −0.7 (6) | C22—C21—P2—Ag2 | 119.3 (3) |
| P2—C21—C22—C23 | −179.8 (3) | C10—C9—P2—C15 | 11.9 (4) |
| C21—C22—C23—C24 | −0.6 (7) | C14—C9—P2—C15 | −167.9 (3) |
| C22—C23—C24—C25 | 0.7 (7) | C10—C9—P2—C21 | −93.6 (4) |
| C23—C24—C25—C26 | 0.6 (7) | C14—C9—P2—C21 | 86.6 (4) |
| C24—C25—C26—C21 | −2.0 (7) | C10—C9—P2—Ag2 | 139.3 (3) |
| C22—C21—C26—C25 | 2.1 (6) | C14—C9—P2—Ag2 | −40.4 (4) |
| P2—C21—C26—C25 | −178.8 (4) | C28—C27—P3—C27iii | −102.6 (3) |
| C32—C27—C28—C29 | 0.6 (7) | C32—C27—P3—C27iii | 77.7 (5) |
| P3—C27—C28—C29 | −179.1 (4) | C28—C27—P3—C27iv | 4.2 (5) |
| C27—C28—C29—C30 | −2.2 (7) | C32—C27—P3—C27iv | −175.5 (3) |
| C28—C29—C30—C31 | 2.2 (7) | C28—C27—P3—Ag2 | 130.8 (4) |
| C29—C30—C31—C32 | −0.7 (8) | C32—C27—P3—Ag2 | −48.9 (4) |
| C30—C31—C32—C27 | −0.8 (7) | C38—C33—P4—C33iii | 101.8 (3) |
| C28—C27—C32—C31 | 0.9 (7) | C34—C33—P4—C33iii | −78.0 (5) |
| P3—C27—C32—C31 | −179.4 (4) | C38—C33—P4—C33iv | −4.8 (5) |
| C38—C33—C34—C35 | 0.9 (8) | C34—C33—P4—C33iv | 175.4 (4) |
| P4—C33—C34—C35 | −179.3 (4) | C38—C33—P4—Ag3 | −131.5 (4) |
| C33—C34—C35—C36 | 0.5 (9) | C34—C33—P4—Ag3 | 48.7 (4) |
| C34—C35—C36—C37 | −1.2 (9) | C52—C51—P5—C39 | −72.5 (6) |
| C35—C36—C37—C38 | 0.6 (8) | C56—C51—P5—C39 | 105.9 (6) |
| C34—C33—C38—C37 | −1.5 (7) | C52—C51—P5—C45 | 179.2 (5) |
| P4—C33—C38—C37 | 178.6 (4) | C56—C51—P5—C45 | −2.4 (6) |
| C36—C37—C38—C33 | 0.8 (8) | C52—C51—P5—Ag3 | 53.2 (6) |
| C44—C39—C40—C41 | −1.4 (13) | C56—C51—P5—Ag3 | −128.4 (5) |
| P5—C39—C40—C41 | 179.2 (7) | C40—C39—P5—C51 | 175.4 (7) |
| C39—C40—C41—C42 | 4.7 (14) | C44—C39—P5—C51 | −4.0 (7) |
| C40—C41—C42—C43 | −6.2 (14) | C40—C39—P5—C45 | −74.4 (7) |
| C41—C42—C43—C44 | 4.8 (13) | C44—C39—P5—C45 | 106.2 (6) |
| C42—C43—C44—C39 | −1.4 (11) | C40—C39—P5—Ag3 | 49.9 (7) |
| C40—C39—C44—C43 | −0.4 (11) | C44—C39—P5—Ag3 | −129.5 (5) |
| P5—C39—C44—C43 | 179.0 (5) | C50—C45—P5—C51 | 101.5 (6) |
| C50—C45—C46—C47 | 3.9 (11) | C46—C45—P5—C51 | −76.4 (6) |
| P5—C45—C46—C47 | −178.2 (6) | C50—C45—P5—C39 | −7.8 (6) |
| C45—C46—C47—C48 | −4.1 (12) | C46—C45—P5—C39 | 174.3 (5) |
| C46—C47—C48—C49 | 2.7 (13) | C50—C45—P5—Ag3 | −132.4 (5) |
| C47—C48—C49—C50 | −1.0 (12) | C46—C45—P5—Ag3 | 49.7 (6) |
| C46—C45—C50—C49 | −2.1 (10) | C2—C1—N1—C1i | 163.9 (5) |
| P5—C45—C50—C49 | −179.9 (5) | C2—C1—N1—C1ii | −70.9 (8) |
| C48—C49—C50—C45 | 0.6 (11) | C2—C1—N1—Ag1 | 46.5 (5) |
| C56—C51—C52—C53 | −1.8 (11) |