metal-organic compounds
Tetrakis(triphenylarsane-κAs)silver(I) trifluoroacetate hemihydrate methanol hemisolvate
aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia, and bChemistry Department, King Abdulaziz University, PO Box 80203 Jeddah, Saudi Arabia
*Correspondence e-mail: seikweng@um.edu.my
The AgI atom in the title hydrated solvated salt, [Ag(C18H15As)4](CF3CO2)·0.5CH3OH·0.5H2O, is coordinated by four As atoms from triphenylarsane ligands in a distorted tetrahedral geometry. In the crystal, O—H⋯O hydrogen bonding occurs between carboxylate groups of anions and lattice solvent molecules. Of the four triphenylarsane ligands in the Ag complex cation, two each have an equally disordered phenyl ring while the trifluoroacetate anion is disordered over two positions with respect to the lattice methanol and water molecules which both show half-occupyncy. The crystal studied was a non-merohedral twin with a 13.6 (1)% contribution of the minor twin component.
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2009); cell SAINT (Bruker, 2009); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).
Supporting information
10.1107/S1600536812045072/xu5641sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812045072/xu5641Isup2.hkl
Silver trifluoroacetate (1 mmol) and triphenylarsane (4 mmol) were heated in methanol (25 ml) until the reactants dissolved completely. Colorless crystals were isolated from the filtered solution after several days.
Carbon-bound H-atoms were placed in calculated positions (C—H 0.95 to 0.98 Å) and were included in the
in the riding model approximation, with U(H) set to 1.2 to 1.5U(C).The trifluoroacetate ion is disordered over two positions; as the occupancy refined to nearly 50%, the disorder was then fixed as a 1:1 type of disorder. The C–O distances were restrained to 1.25±0.01 Å, the C–C distances to 1.50±0.01 Å and the C–F distances to 1.35±0.01 Å. Additionally, the O···O distances were restrained to 2.17±0.01 Å and the F···F distances to 2.21±0.01 Å.
One half-occupancy trifluoroacetate portion is hydrogen bonded to a half-occupancy water molecule whereas the other half-occupancy portion is hydrogen bonded to a half-occupancy methanol molecule. For the methanol molecule, the C–O distance was restrained to 1.45±0.01 Å. The H atoms were placed in calculated positions (O–H 0.84 Å) and their temperature factors tied by a factor of 1.5 times.
The anisotropic temperature factors of the disordered atoms were restrained to be nearly isotropic.
Of the four triphenylarsane groups, two have each a disordered phenyl ring. The disorder was also treated as a 1:1 type of disorder. Pairs of As—C distances were restrained to within 0.01 Å of each other. The aromatic rings were refined as a rigid hexagon of 1.39 Å sides, and the temperature factors of the primed atoms were set to those of the unprimed ones. The anisotropic temperature factors were also restrained to be nearly isotropic.
The (1 0 0), (0 1 0) and (0 - 1 1) reflections that were affected by the beamstop as well as (-1 4 12) and (-3 8 1) were omitted.
The final difference Fourier map was featureless except for a peak at 0.88 Å from C74.
Data collection: APEX2 (Bruker, 2009); cell
SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).[Ag(C18H15As)4](C2F3O2)·0.5CH4O·0.5H2O | Z = 2 |
Mr = 1470.80 | F(000) = 1480 |
Triclinic, P1 | Dx = 1.526 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.9069 (2) Å | Cell parameters from 4258 reflections |
b = 14.5530 (3) Å | θ = 2.2–25.5° |
c = 18.5573 (4) Å | µ = 2.42 mm−1 |
α = 88.893 (2)° | T = 100 K |
β = 85.782 (1)° | Prism, colorless |
γ = 86.808 (1)° | 0.22 × 0.17 × 0.11 mm |
V = 3201.57 (11) Å3 |
Bruker SMART APEX diffractometer | 14449 independent reflections |
Radiation source: fine-focus sealed tube | 10289 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
ω scans | θmax = 27.5°, θmin = 1.1° |
Absorption correction: multi-scan (TWINABS; Bruker, 2009) | h = −15→15 |
Tmin = 0.618, Tmax = 0.776 | k = −18→18 |
48380 measured reflections | l = 0→24 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.111 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0263P)2 + 7.5548P] where P = (Fo2 + 2Fc2)/3 |
14449 reflections | (Δ/σ)max = 0.001 |
838 parameters | Δρmax = 1.08 e Å−3 |
197 restraints | Δρmin = −0.56 e Å−3 |
[Ag(C18H15As)4](C2F3O2)·0.5CH4O·0.5H2O | γ = 86.808 (1)° |
Mr = 1470.80 | V = 3201.57 (11) Å3 |
Triclinic, P1 | Z = 2 |
a = 11.9069 (2) Å | Mo Kα radiation |
b = 14.5530 (3) Å | µ = 2.42 mm−1 |
c = 18.5573 (4) Å | T = 100 K |
α = 88.893 (2)° | 0.22 × 0.17 × 0.11 mm |
β = 85.782 (1)° |
Bruker SMART APEX diffractometer | 14449 independent reflections |
Absorption correction: multi-scan (TWINABS; Bruker, 2009) | 10289 reflections with I > 2σ(I) |
Tmin = 0.618, Tmax = 0.776 | Rint = 0.058 |
48380 measured reflections |
R[F2 > 2σ(F2)] = 0.048 | 197 restraints |
wR(F2) = 0.111 | H-atom parameters constrained |
S = 1.03 | Δρmax = 1.08 e Å−3 |
14449 reflections | Δρmin = −0.56 e Å−3 |
838 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ag1 | 0.49421 (3) | 0.25589 (3) | 0.24626 (2) | 0.01910 (9) | |
As1 | 0.56948 (4) | 0.42096 (3) | 0.21599 (3) | 0.02081 (12) | |
As2 | 0.33767 (4) | 0.21756 (3) | 0.15901 (3) | 0.01929 (12) | |
As3 | 0.40995 (5) | 0.25168 (4) | 0.38150 (3) | 0.02716 (13) | |
As4 | 0.66244 (4) | 0.12921 (4) | 0.23054 (3) | 0.02178 (12) | |
C1 | 0.6503 (8) | 0.4230 (7) | 0.1228 (3) | 0.0268 (14) | 0.50 |
C2 | 0.7331 (8) | 0.3536 (7) | 0.1076 (5) | 0.024 (2) | 0.50 |
H2 | 0.7507 | 0.3091 | 0.1438 | 0.029* | 0.50 |
C3 | 0.7901 (7) | 0.3493 (6) | 0.0396 (6) | 0.049 (3) | 0.50 |
H3A | 0.8468 | 0.3018 | 0.0292 | 0.059* | 0.50 |
C4 | 0.7643 (8) | 0.4144 (7) | −0.0133 (4) | 0.051 (3) | 0.50 |
H4 | 0.8033 | 0.4114 | −0.0599 | 0.061* | 0.50 |
C5 | 0.6815 (9) | 0.4838 (6) | 0.0018 (4) | 0.062 (3) | 0.50 |
H5 | 0.6639 | 0.5283 | −0.0344 | 0.075* | 0.50 |
C6 | 0.6245 (7) | 0.4881 (6) | 0.0698 (5) | 0.036 (2) | 0.50 |
H6 | 0.5678 | 0.5356 | 0.0802 | 0.043* | 0.50 |
C1' | 0.6480 (8) | 0.4370 (7) | 0.1207 (3) | 0.0268 (14) | 0.50 |
C2' | 0.7066 (9) | 0.3600 (6) | 0.0906 (5) | 0.024 (2) | 0.50 |
H2' | 0.6996 | 0.3014 | 0.1134 | 0.029* | 0.50 |
C3' | 0.7754 (8) | 0.3689 (6) | 0.0273 (6) | 0.049 (3) | 0.50 |
H3' | 0.8154 | 0.3162 | 0.0068 | 0.059* | 0.50 |
C4' | 0.7856 (8) | 0.4547 (7) | −0.0060 (4) | 0.051 (3) | 0.50 |
H4' | 0.8326 | 0.4607 | −0.0492 | 0.061* | 0.50 |
C5' | 0.7270 (8) | 0.5317 (6) | 0.0241 (4) | 0.062 (3) | 0.50 |
H5' | 0.7340 | 0.5903 | 0.0013 | 0.075* | 0.50 |
C6' | 0.6582 (7) | 0.5228 (6) | 0.0874 (4) | 0.036 (2) | 0.50 |
H6' | 0.6182 | 0.5754 | 0.1079 | 0.043* | 0.50 |
C7 | 0.6762 (4) | 0.4713 (3) | 0.2772 (3) | 0.0218 (11) | |
C8 | 0.6637 (5) | 0.4545 (4) | 0.3509 (3) | 0.0281 (12) | |
H8 | 0.6078 | 0.4150 | 0.3703 | 0.034* | |
C9 | 0.7330 (5) | 0.4955 (4) | 0.3966 (3) | 0.0407 (15) | |
H9 | 0.7244 | 0.4839 | 0.4472 | 0.049* | |
C10 | 0.8142 (5) | 0.5529 (4) | 0.3686 (3) | 0.0391 (15) | |
H10 | 0.8601 | 0.5822 | 0.4001 | 0.047* | |
C11 | 0.8287 (5) | 0.5677 (4) | 0.2952 (4) | 0.0385 (15) | |
H11 | 0.8864 | 0.6056 | 0.2758 | 0.046* | |
C12 | 0.7594 (4) | 0.5276 (4) | 0.2496 (3) | 0.0292 (12) | |
H12 | 0.7691 | 0.5388 | 0.1990 | 0.035* | |
C13 | 0.4587 (4) | 0.5245 (3) | 0.2146 (3) | 0.0232 (11) | |
C14 | 0.4769 (5) | 0.6085 (4) | 0.2426 (3) | 0.0294 (12) | |
H14 | 0.5480 | 0.6191 | 0.2601 | 0.035* | |
C15 | 0.3922 (5) | 0.6783 (4) | 0.2456 (3) | 0.0339 (13) | |
H15 | 0.4055 | 0.7359 | 0.2655 | 0.041* | |
C16 | 0.2898 (5) | 0.6643 (4) | 0.2199 (3) | 0.0339 (14) | |
H16 | 0.2324 | 0.7123 | 0.2213 | 0.041* | |
C17 | 0.2709 (6) | 0.5806 (5) | 0.1920 (4) | 0.055 (2) | |
H17 | 0.1992 | 0.5700 | 0.1753 | 0.066* | |
C18 | 0.3557 (5) | 0.5109 (4) | 0.1881 (4) | 0.0480 (18) | |
H18 | 0.3428 | 0.4539 | 0.1670 | 0.058* | |
C19 | 0.2016 (6) | 0.2973 (6) | 0.1538 (7) | 0.0200 (11) | 0.50 |
C20 | 0.1681 (9) | 0.3572 (7) | 0.2097 (6) | 0.032 (3) | 0.50 |
H20 | 0.2105 | 0.3582 | 0.2511 | 0.039* | 0.50 |
C21 | 0.0725 (10) | 0.4158 (7) | 0.2051 (6) | 0.037 (3) | 0.50 |
H21 | 0.0496 | 0.4568 | 0.2433 | 0.044* | 0.50 |
C22 | 0.0105 (7) | 0.4144 (7) | 0.1446 (7) | 0.0364 (17) | 0.50 |
H22 | −0.0549 | 0.4544 | 0.1415 | 0.044* | 0.50 |
C23 | 0.0439 (7) | 0.3544 (6) | 0.0887 (6) | 0.035 (3) | 0.50 |
H23 | 0.0015 | 0.3535 | 0.0474 | 0.042* | 0.50 |
C24 | 0.1395 (7) | 0.2959 (5) | 0.0933 (6) | 0.029 (2) | 0.50 |
H24 | 0.1624 | 0.2549 | 0.0551 | 0.034* | 0.50 |
C19' | 0.2035 (6) | 0.2995 (6) | 0.1534 (7) | 0.0200 (11) | 0.50 |
C20' | 0.1488 (10) | 0.3303 (7) | 0.2179 (6) | 0.032 (3) | 0.50 |
H20B | 0.1749 | 0.3089 | 0.2627 | 0.039* | 0.50 |
C21' | 0.0558 (10) | 0.3923 (8) | 0.2168 (6) | 0.037 (3) | 0.50 |
H21B | 0.0184 | 0.4134 | 0.2609 | 0.044* | 0.50 |
C22' | 0.0176 (7) | 0.4236 (7) | 0.1512 (7) | 0.0364 (17) | 0.50 |
H22B | −0.0459 | 0.4660 | 0.1505 | 0.044* | 0.50 |
C23' | 0.0724 (8) | 0.3928 (6) | 0.0867 (6) | 0.035 (3) | 0.50 |
H23B | 0.0463 | 0.4141 | 0.0419 | 0.042* | 0.50 |
C24' | 0.1653 (7) | 0.3307 (6) | 0.0878 (6) | 0.029 (2) | 0.50 |
H24B | 0.2028 | 0.3097 | 0.0437 | 0.034* | 0.50 |
C25 | 0.2712 (4) | 0.0995 (3) | 0.1782 (3) | 0.0224 (11) | |
C26 | 0.3435 (4) | 0.0212 (4) | 0.1775 (3) | 0.0286 (12) | |
H26 | 0.4221 | 0.0263 | 0.1667 | 0.034* | |
C27 | 0.3007 (5) | −0.0643 (4) | 0.1927 (3) | 0.0363 (14) | |
H27 | 0.3502 | −0.1179 | 0.1918 | 0.044* | |
C28 | 0.1862 (5) | −0.0720 (4) | 0.2091 (3) | 0.0326 (13) | |
H28 | 0.1569 | −0.1304 | 0.2200 | 0.039* | |
C29 | 0.1156 (5) | 0.0059 (4) | 0.2094 (3) | 0.0369 (14) | |
H29 | 0.0369 | 0.0006 | 0.2198 | 0.044* | |
C30 | 0.1568 (4) | 0.0921 (4) | 0.1948 (3) | 0.0283 (12) | |
H30 | 0.1071 | 0.1455 | 0.1961 | 0.034* | |
C31 | 0.3875 (4) | 0.2082 (3) | 0.0575 (3) | 0.0208 (11) | |
C32 | 0.3434 (5) | 0.1457 (4) | 0.0127 (3) | 0.0311 (13) | |
H32 | 0.2907 | 0.1036 | 0.0324 | 0.037* | |
C33 | 0.3763 (6) | 0.1448 (4) | −0.0608 (3) | 0.0424 (16) | |
H33 | 0.3463 | 0.1020 | −0.0912 | 0.051* | |
C34 | 0.4523 (6) | 0.2060 (4) | −0.0894 (3) | 0.0411 (16) | |
H34 | 0.4739 | 0.2058 | −0.1398 | 0.049* | |
C35 | 0.4975 (5) | 0.2677 (4) | −0.0452 (3) | 0.0387 (15) | |
H35 | 0.5504 | 0.3094 | −0.0652 | 0.046* | |
C36 | 0.4658 (4) | 0.2687 (4) | 0.0281 (3) | 0.0312 (13) | |
H36 | 0.4975 | 0.3107 | 0.0583 | 0.037* | |
C37 | 0.3449 (5) | 0.1394 (4) | 0.4188 (3) | 0.0340 (13) | |
C38 | 0.2712 (5) | 0.0977 (4) | 0.3775 (3) | 0.0366 (14) | |
H38 | 0.2553 | 0.1232 | 0.3316 | 0.044* | |
C39 | 0.2206 (6) | 0.0196 (5) | 0.4024 (4) | 0.0476 (17) | |
H39 | 0.1690 | −0.0083 | 0.3741 | 0.057* | |
C40 | 0.2444 (7) | −0.0185 (6) | 0.4683 (4) | 0.072 (3) | |
H40 | 0.2106 | −0.0730 | 0.4856 | 0.086* | |
C41 | 0.3192 (8) | 0.0245 (6) | 0.5094 (5) | 0.081 (3) | |
H41 | 0.3347 | −0.0007 | 0.5555 | 0.098* | |
C42 | 0.3707 (6) | 0.1018 (5) | 0.4851 (4) | 0.056 (2) | |
H42 | 0.4231 | 0.1292 | 0.5131 | 0.067* | |
C43 | 0.5097 (5) | 0.2796 (4) | 0.4557 (3) | 0.0286 (12) | |
C44 | 0.6176 (5) | 0.2395 (5) | 0.4512 (3) | 0.0444 (16) | |
H44 | 0.6410 | 0.1976 | 0.4138 | 0.053* | |
C45 | 0.6922 (6) | 0.2611 (5) | 0.5024 (3) | 0.0473 (17) | |
H45 | 0.7666 | 0.2337 | 0.4995 | 0.057* | |
C46 | 0.6592 (5) | 0.3214 (5) | 0.5567 (4) | 0.0441 (16) | |
H46 | 0.7100 | 0.3347 | 0.5918 | 0.053* | |
C47 | 0.5533 (6) | 0.3620 (5) | 0.5601 (4) | 0.0517 (18) | |
H47 | 0.5307 | 0.4047 | 0.5972 | 0.062* | |
C48 | 0.4776 (5) | 0.3412 (4) | 0.5096 (3) | 0.0406 (15) | |
H48 | 0.4036 | 0.3697 | 0.5125 | 0.049* | |
C49 | 0.2838 (5) | 0.3400 (4) | 0.4013 (3) | 0.0303 (13) | |
C50 | 0.1901 (5) | 0.3177 (4) | 0.4462 (3) | 0.0372 (14) | |
H50 | 0.1888 | 0.2595 | 0.4703 | 0.045* | |
C51 | 0.0992 (5) | 0.3804 (5) | 0.4558 (4) | 0.0477 (17) | |
H51 | 0.0352 | 0.3654 | 0.4865 | 0.057* | |
C52 | 0.1010 (6) | 0.4646 (5) | 0.4210 (3) | 0.051 (2) | |
H52 | 0.0380 | 0.5074 | 0.4275 | 0.061* | |
C53 | 0.1939 (6) | 0.4875 (5) | 0.3765 (3) | 0.0486 (18) | |
H53 | 0.1947 | 0.5458 | 0.3526 | 0.058* | |
C54 | 0.2865 (6) | 0.4246 (4) | 0.3669 (3) | 0.0403 (15) | |
H54 | 0.3509 | 0.4402 | 0.3368 | 0.048* | |
C55 | 0.7410 (4) | 0.1122 (4) | 0.1358 (3) | 0.0250 (11) | |
C56 | 0.6771 (5) | 0.1027 (4) | 0.0766 (3) | 0.0302 (13) | |
H56 | 0.5972 | 0.1033 | 0.0834 | 0.036* | |
C57 | 0.7298 (5) | 0.0923 (4) | 0.0079 (3) | 0.0389 (15) | |
H57 | 0.6855 | 0.0872 | −0.0323 | 0.047* | |
C58 | 0.8449 (6) | 0.0894 (4) | −0.0029 (3) | 0.0444 (16) | |
H58 | 0.8804 | 0.0809 | −0.0500 | 0.053* | |
C59 | 0.9097 (5) | 0.0989 (5) | 0.0559 (3) | 0.0486 (18) | |
H59 | 0.9896 | 0.0973 | 0.0488 | 0.058* | |
C60 | 0.8584 (5) | 0.1105 (5) | 0.1241 (3) | 0.0403 (15) | |
H60 | 0.9032 | 0.1176 | 0.1637 | 0.048* | |
C61 | 0.7870 (4) | 0.1530 (4) | 0.2891 (3) | 0.0253 (11) | |
C62 | 0.8187 (5) | 0.2417 (4) | 0.2932 (4) | 0.054 (2) | |
H62 | 0.7826 | 0.2894 | 0.2662 | 0.065* | |
C63 | 0.9038 (6) | 0.2618 (5) | 0.3370 (5) | 0.064 (2) | |
H63 | 0.9235 | 0.3238 | 0.3411 | 0.077* | |
C64 | 0.9581 (5) | 0.1952 (5) | 0.3733 (3) | 0.0463 (17) | |
H64 | 1.0181 | 0.2095 | 0.4015 | 0.056* | |
C65 | 0.9280 (5) | 0.1078 (6) | 0.3700 (4) | 0.058 (2) | |
H65 | 0.9659 | 0.0608 | 0.3967 | 0.070* | |
C66 | 0.8416 (5) | 0.0853 (5) | 0.3276 (3) | 0.0426 (17) | |
H66 | 0.8207 | 0.0234 | 0.3256 | 0.051* | |
C67 | 0.6337 (5) | 0.0041 (4) | 0.2601 (3) | 0.0305 (13) | |
C68 | 0.7066 (6) | −0.0709 (4) | 0.2393 (3) | 0.0425 (16) | |
H68 | 0.7694 | −0.0627 | 0.2056 | 0.051* | |
C69 | 0.6860 (8) | −0.1578 (4) | 0.2685 (4) | 0.060 (2) | |
H69 | 0.7362 | −0.2087 | 0.2553 | 0.072* | |
C70 | 0.5940 (7) | −0.1710 (5) | 0.3161 (4) | 0.057 (2) | |
H70 | 0.5815 | −0.2305 | 0.3359 | 0.068* | |
C71 | 0.5210 (6) | −0.0990 (5) | 0.3348 (4) | 0.0523 (19) | |
H71 | 0.4565 | −0.1087 | 0.3668 | 0.063* | |
C72 | 0.5402 (5) | −0.0107 (4) | 0.3072 (3) | 0.0393 (15) | |
H72 | 0.4889 | 0.0394 | 0.3208 | 0.047* | |
F1 | 1.0254 (7) | 0.8237 (6) | 0.4465 (4) | 0.080 (3) | 0.50 |
F2 | 0.8632 (5) | 0.8126 (5) | 0.4040 (4) | 0.056 (2) | 0.50 |
F3 | 0.9807 (6) | 0.9013 (5) | 0.3532 (4) | 0.053 (2) | 0.50 |
O1 | 1.0064 (8) | 0.7603 (7) | 0.2714 (5) | 0.054 (3) | 0.50 |
O2 | 1.0643 (10) | 0.6786 (7) | 0.3636 (6) | 0.048 (3) | 0.50 |
O3 | 1.0074 (10) | 0.6640 (8) | 0.1419 (7) | 0.084 (4) | 0.50 |
H3 | 1.0100 | 0.6902 | 0.1816 | 0.127* | 0.50 |
C73 | 1.0177 (9) | 0.7479 (7) | 0.3359 (5) | 0.045 (3) | 0.50 |
C74 | 0.9723 (7) | 0.8223 (6) | 0.3867 (4) | 0.030 (3) | 0.50 |
C75 | 0.934 (2) | 0.7209 (18) | 0.1002 (14) | 0.114 (9) | 0.50 |
H75A | 0.8819 | 0.7583 | 0.1327 | 0.171* | 0.50 |
H75B | 0.8904 | 0.6820 | 0.0713 | 0.171* | 0.50 |
H75C | 0.9784 | 0.7614 | 0.0681 | 0.171* | 0.50 |
F1' | 1.0116 (10) | 0.7034 (9) | 0.0846 (9) | 0.152 (6) | 0.50 |
F2' | 0.9035 (8) | 0.8315 (6) | 0.0905 (5) | 0.090 (3) | 0.50 |
F3' | 0.8372 (8) | 0.7000 (7) | 0.1304 (5) | 0.090 (3) | 0.50 |
O1' | 1.0273 (8) | 0.7022 (7) | 0.2278 (7) | 0.068 (3) | 0.50 |
O2' | 0.9423 (8) | 0.8392 (6) | 0.2283 (6) | 0.071 (3) | 0.50 |
O1W' | 1.056 (2) | 0.7100 (17) | 0.3790 (13) | 0.167 (11) | 0.50 |
H1W1 | 1.0467 | 0.7070 | 0.3346 | 0.250* | 0.50 |
H2W2 | 1.0892 | 0.7577 | 0.3869 | 0.250* | 0.50 |
C73' | 0.9718 (9) | 0.7654 (7) | 0.1983 (6) | 0.046 (3) | 0.50 |
C74' | 0.9304 (9) | 0.7507 (7) | 0.1247 (6) | 0.058 (5) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.02018 (18) | 0.0189 (2) | 0.01837 (19) | −0.00101 (15) | −0.00220 (14) | −0.00194 (14) |
As1 | 0.0250 (3) | 0.0170 (3) | 0.0210 (3) | −0.0026 (2) | −0.0035 (2) | −0.0024 (2) |
As2 | 0.0182 (2) | 0.0200 (3) | 0.0202 (3) | −0.0031 (2) | −0.0033 (2) | −0.0019 (2) |
As3 | 0.0369 (3) | 0.0274 (3) | 0.0162 (3) | 0.0014 (2) | 0.0018 (2) | 0.0005 (2) |
As4 | 0.0208 (3) | 0.0198 (3) | 0.0250 (3) | 0.0025 (2) | −0.0044 (2) | −0.0053 (2) |
C1 | 0.027 (3) | 0.025 (4) | 0.028 (3) | 0.002 (3) | −0.002 (2) | −0.005 (2) |
C2 | 0.014 (5) | 0.033 (4) | 0.028 (5) | −0.001 (3) | −0.011 (4) | −0.012 (3) |
C3 | 0.037 (4) | 0.060 (6) | 0.050 (5) | −0.003 (4) | 0.005 (4) | −0.023 (5) |
C4 | 0.061 (6) | 0.061 (8) | 0.030 (4) | −0.005 (6) | 0.005 (4) | −0.018 (5) |
C5 | 0.072 (7) | 0.076 (7) | 0.036 (5) | 0.003 (5) | 0.008 (5) | 0.018 (5) |
C6 | 0.049 (5) | 0.033 (6) | 0.025 (4) | 0.000 (4) | 0.002 (4) | 0.000 (4) |
C1' | 0.027 (3) | 0.025 (4) | 0.028 (3) | 0.002 (3) | −0.002 (2) | −0.005 (2) |
C2' | 0.014 (5) | 0.033 (4) | 0.028 (5) | −0.001 (3) | −0.011 (4) | −0.012 (3) |
C3' | 0.037 (4) | 0.060 (6) | 0.050 (5) | −0.003 (4) | 0.005 (4) | −0.023 (5) |
C4' | 0.061 (6) | 0.061 (8) | 0.030 (4) | −0.005 (6) | 0.005 (4) | −0.018 (5) |
C5' | 0.072 (7) | 0.076 (7) | 0.036 (5) | 0.003 (5) | 0.008 (5) | 0.018 (5) |
C6' | 0.049 (5) | 0.033 (6) | 0.025 (4) | 0.000 (4) | 0.002 (4) | 0.000 (4) |
C7 | 0.027 (3) | 0.018 (3) | 0.020 (3) | 0.002 (2) | −0.003 (2) | −0.003 (2) |
C8 | 0.039 (3) | 0.023 (3) | 0.022 (3) | 0.001 (2) | −0.004 (2) | −0.001 (2) |
C9 | 0.059 (4) | 0.034 (3) | 0.030 (3) | 0.012 (3) | −0.014 (3) | −0.007 (3) |
C10 | 0.038 (3) | 0.032 (3) | 0.050 (4) | 0.007 (3) | −0.022 (3) | −0.023 (3) |
C11 | 0.026 (3) | 0.036 (4) | 0.055 (4) | −0.003 (3) | −0.005 (3) | −0.020 (3) |
C12 | 0.026 (3) | 0.024 (3) | 0.038 (3) | −0.006 (2) | 0.002 (2) | −0.006 (2) |
C13 | 0.028 (3) | 0.020 (3) | 0.022 (3) | −0.003 (2) | −0.003 (2) | 0.003 (2) |
C14 | 0.028 (3) | 0.023 (3) | 0.038 (3) | −0.005 (2) | −0.005 (2) | 0.001 (2) |
C15 | 0.040 (3) | 0.022 (3) | 0.040 (3) | 0.000 (3) | −0.006 (3) | −0.007 (3) |
C16 | 0.039 (3) | 0.030 (3) | 0.031 (3) | 0.011 (3) | −0.005 (3) | −0.001 (3) |
C17 | 0.047 (4) | 0.042 (4) | 0.081 (5) | 0.009 (3) | −0.036 (4) | −0.014 (4) |
C18 | 0.043 (4) | 0.028 (3) | 0.077 (5) | 0.008 (3) | −0.031 (4) | −0.021 (3) |
C19 | 0.019 (2) | 0.020 (2) | 0.022 (3) | −0.008 (2) | 0.000 (2) | 0.000 (2) |
C20 | 0.029 (5) | 0.030 (7) | 0.038 (4) | 0.001 (4) | −0.003 (4) | −0.004 (4) |
C21 | 0.037 (5) | 0.034 (6) | 0.036 (5) | 0.003 (4) | 0.007 (4) | −0.005 (4) |
C22 | 0.025 (3) | 0.036 (4) | 0.047 (4) | 0.007 (3) | 0.001 (3) | −0.004 (3) |
C23 | 0.028 (5) | 0.038 (6) | 0.040 (4) | 0.006 (4) | −0.008 (4) | −0.006 (5) |
C24 | 0.026 (5) | 0.026 (6) | 0.034 (4) | 0.002 (4) | −0.006 (3) | −0.005 (5) |
C19' | 0.019 (2) | 0.020 (2) | 0.022 (3) | −0.008 (2) | 0.000 (2) | 0.000 (2) |
C20' | 0.029 (5) | 0.030 (7) | 0.038 (4) | 0.001 (4) | −0.003 (4) | −0.004 (4) |
C21' | 0.037 (5) | 0.034 (6) | 0.036 (5) | 0.003 (4) | 0.007 (4) | −0.005 (4) |
C22' | 0.025 (3) | 0.036 (4) | 0.047 (4) | 0.007 (3) | 0.001 (3) | −0.004 (3) |
C23' | 0.028 (5) | 0.038 (6) | 0.040 (4) | 0.006 (4) | −0.008 (4) | −0.006 (5) |
C24' | 0.026 (5) | 0.026 (6) | 0.034 (4) | 0.002 (4) | −0.006 (3) | −0.005 (5) |
C25 | 0.024 (3) | 0.025 (3) | 0.018 (3) | 0.001 (2) | −0.005 (2) | −0.001 (2) |
C26 | 0.021 (3) | 0.030 (3) | 0.033 (3) | 0.001 (2) | 0.003 (2) | 0.007 (2) |
C27 | 0.037 (3) | 0.022 (3) | 0.048 (4) | 0.005 (3) | 0.005 (3) | 0.006 (3) |
C28 | 0.042 (3) | 0.021 (3) | 0.036 (3) | −0.005 (3) | −0.001 (3) | 0.003 (2) |
C29 | 0.030 (3) | 0.032 (3) | 0.051 (4) | −0.009 (3) | −0.010 (3) | 0.008 (3) |
C30 | 0.021 (3) | 0.025 (3) | 0.040 (3) | −0.005 (2) | −0.004 (2) | 0.008 (2) |
C31 | 0.019 (2) | 0.019 (3) | 0.024 (3) | 0.002 (2) | −0.004 (2) | 0.001 (2) |
C32 | 0.042 (3) | 0.028 (3) | 0.022 (3) | 0.001 (3) | 0.000 (2) | 0.001 (2) |
C33 | 0.071 (5) | 0.033 (3) | 0.022 (3) | 0.005 (3) | −0.001 (3) | −0.012 (3) |
C34 | 0.062 (4) | 0.038 (4) | 0.018 (3) | 0.014 (3) | 0.013 (3) | 0.003 (3) |
C35 | 0.034 (3) | 0.042 (4) | 0.036 (3) | 0.004 (3) | 0.010 (3) | 0.014 (3) |
C36 | 0.029 (3) | 0.030 (3) | 0.034 (3) | −0.004 (2) | −0.001 (2) | 0.005 (3) |
C37 | 0.039 (3) | 0.038 (3) | 0.025 (3) | −0.001 (3) | −0.001 (2) | 0.002 (3) |
C38 | 0.034 (3) | 0.043 (4) | 0.033 (3) | −0.003 (3) | −0.003 (3) | 0.001 (3) |
C39 | 0.052 (4) | 0.046 (4) | 0.048 (4) | −0.016 (3) | −0.012 (3) | −0.003 (3) |
C40 | 0.087 (6) | 0.061 (5) | 0.074 (6) | −0.036 (5) | −0.029 (5) | 0.037 (4) |
C41 | 0.119 (7) | 0.067 (6) | 0.068 (6) | −0.044 (5) | −0.050 (5) | 0.039 (5) |
C42 | 0.075 (5) | 0.056 (5) | 0.040 (4) | −0.034 (4) | −0.024 (4) | 0.025 (3) |
C43 | 0.036 (3) | 0.030 (3) | 0.018 (3) | −0.001 (2) | 0.006 (2) | 0.004 (2) |
C44 | 0.049 (4) | 0.046 (4) | 0.037 (4) | 0.012 (3) | −0.005 (3) | −0.009 (3) |
C45 | 0.048 (4) | 0.054 (4) | 0.039 (4) | 0.009 (3) | −0.006 (3) | 0.000 (3) |
C46 | 0.040 (4) | 0.046 (4) | 0.049 (4) | −0.010 (3) | −0.011 (3) | 0.004 (3) |
C47 | 0.049 (4) | 0.060 (5) | 0.048 (4) | 0.004 (4) | −0.010 (3) | −0.028 (4) |
C48 | 0.039 (3) | 0.050 (4) | 0.032 (3) | 0.005 (3) | −0.003 (3) | −0.009 (3) |
C49 | 0.038 (3) | 0.038 (3) | 0.015 (3) | 0.001 (3) | −0.003 (2) | −0.005 (2) |
C50 | 0.041 (3) | 0.048 (4) | 0.023 (3) | 0.003 (3) | −0.006 (3) | −0.013 (3) |
C51 | 0.033 (3) | 0.071 (5) | 0.039 (4) | 0.002 (3) | −0.002 (3) | −0.024 (4) |
C52 | 0.047 (4) | 0.072 (5) | 0.034 (4) | 0.026 (4) | −0.018 (3) | −0.036 (4) |
C53 | 0.072 (5) | 0.043 (4) | 0.032 (3) | 0.018 (4) | −0.018 (3) | −0.012 (3) |
C54 | 0.059 (4) | 0.040 (4) | 0.020 (3) | 0.014 (3) | −0.001 (3) | −0.006 (3) |
C55 | 0.023 (3) | 0.023 (3) | 0.029 (3) | 0.008 (2) | −0.004 (2) | −0.006 (2) |
C56 | 0.031 (3) | 0.026 (3) | 0.035 (3) | 0.001 (2) | −0.009 (2) | −0.006 (2) |
C57 | 0.051 (4) | 0.034 (3) | 0.033 (3) | 0.005 (3) | −0.011 (3) | −0.012 (3) |
C58 | 0.053 (4) | 0.048 (4) | 0.030 (3) | 0.016 (3) | 0.003 (3) | −0.012 (3) |
C59 | 0.030 (3) | 0.072 (5) | 0.041 (4) | 0.016 (3) | 0.004 (3) | −0.015 (4) |
C60 | 0.028 (3) | 0.057 (4) | 0.035 (3) | 0.008 (3) | −0.005 (3) | −0.010 (3) |
C61 | 0.020 (3) | 0.030 (3) | 0.025 (3) | 0.001 (2) | 0.001 (2) | −0.006 (2) |
C62 | 0.043 (4) | 0.034 (4) | 0.089 (6) | 0.007 (3) | −0.034 (4) | −0.018 (4) |
C63 | 0.047 (4) | 0.050 (5) | 0.100 (6) | 0.000 (4) | −0.033 (4) | −0.038 (4) |
C64 | 0.025 (3) | 0.075 (5) | 0.042 (4) | −0.012 (3) | −0.008 (3) | −0.018 (4) |
C65 | 0.044 (4) | 0.073 (5) | 0.061 (5) | −0.016 (4) | −0.030 (4) | 0.021 (4) |
C66 | 0.033 (3) | 0.048 (4) | 0.051 (4) | −0.016 (3) | −0.021 (3) | 0.018 (3) |
C67 | 0.037 (3) | 0.033 (3) | 0.024 (3) | −0.006 (3) | −0.011 (2) | −0.005 (2) |
C68 | 0.072 (5) | 0.026 (3) | 0.029 (3) | 0.010 (3) | −0.008 (3) | −0.004 (3) |
C69 | 0.119 (7) | 0.025 (3) | 0.036 (4) | 0.013 (4) | −0.024 (4) | −0.007 (3) |
C70 | 0.107 (7) | 0.029 (4) | 0.040 (4) | −0.024 (4) | −0.029 (4) | 0.006 (3) |
C71 | 0.065 (5) | 0.046 (4) | 0.050 (4) | −0.026 (4) | −0.019 (4) | 0.009 (3) |
C72 | 0.037 (3) | 0.031 (3) | 0.052 (4) | −0.007 (3) | −0.014 (3) | 0.001 (3) |
F1 | 0.090 (6) | 0.083 (6) | 0.069 (5) | 0.002 (5) | −0.024 (5) | −0.031 (5) |
F2 | 0.046 (4) | 0.081 (5) | 0.037 (4) | 0.019 (4) | 0.014 (3) | 0.000 (4) |
F3 | 0.047 (4) | 0.049 (4) | 0.062 (5) | −0.003 (3) | 0.014 (4) | −0.011 (4) |
O1 | 0.047 (5) | 0.069 (6) | 0.049 (5) | −0.033 (5) | 0.001 (4) | −0.011 (5) |
O2 | 0.050 (5) | 0.034 (5) | 0.057 (6) | 0.025 (4) | −0.002 (4) | 0.005 (4) |
O3 | 0.088 (7) | 0.078 (7) | 0.082 (7) | 0.027 (6) | 0.011 (6) | 0.002 (6) |
C73 | 0.030 (6) | 0.052 (7) | 0.056 (7) | −0.020 (5) | −0.008 (5) | 0.009 (6) |
C74 | 0.031 (5) | 0.042 (6) | 0.021 (5) | −0.012 (5) | −0.006 (4) | −0.007 (4) |
C75 | 0.092 (12) | 0.145 (13) | 0.109 (12) | 0.004 (9) | −0.026 (9) | −0.016 (9) |
F1' | 0.141 (9) | 0.176 (10) | 0.133 (9) | 0.025 (8) | 0.011 (8) | −0.023 (8) |
F2' | 0.077 (6) | 0.116 (7) | 0.075 (6) | −0.001 (5) | −0.005 (5) | 0.038 (5) |
F3' | 0.101 (6) | 0.102 (7) | 0.075 (6) | −0.043 (6) | −0.021 (5) | 0.000 (5) |
O1' | 0.050 (5) | 0.066 (6) | 0.089 (7) | 0.000 (5) | −0.009 (5) | 0.008 (6) |
O2' | 0.043 (5) | 0.057 (6) | 0.112 (7) | 0.003 (5) | 0.002 (5) | −0.002 (6) |
O1W' | 0.166 (13) | 0.177 (14) | 0.163 (14) | −0.025 (9) | −0.033 (9) | 0.001 (9) |
C73' | 0.026 (5) | 0.045 (6) | 0.066 (7) | −0.010 (5) | 0.002 (5) | 0.005 (6) |
C74' | 0.050 (8) | 0.078 (9) | 0.044 (7) | 0.009 (7) | 0.002 (6) | 0.008 (7) |
Ag1—As1 | 2.6464 (6) | C31—C36 | 1.393 (7) |
Ag1—As2 | 2.6460 (6) | C32—C33 | 1.391 (8) |
Ag1—As3 | 2.6342 (7) | C32—H32 | 0.9500 |
Ag1—As4 | 2.6494 (6) | C33—C34 | 1.377 (9) |
As1—C1 | 1.917 (5) | C33—H33 | 0.9500 |
As1—C7 | 1.946 (5) | C34—C35 | 1.384 (9) |
As1—C13 | 1.948 (5) | C34—H34 | 0.9500 |
As1—C1' | 1.955 (5) | C35—C36 | 1.384 (8) |
As2—C31 | 1.938 (5) | C35—H35 | 0.9500 |
As2—C19 | 1.947 (5) | C36—H36 | 0.9500 |
As2—C19' | 1.947 (5) | C37—C38 | 1.379 (8) |
As2—C25 | 1.947 (5) | C37—C42 | 1.386 (8) |
As3—C49 | 1.940 (6) | C38—C39 | 1.373 (8) |
As3—C37 | 1.941 (6) | C38—H38 | 0.9500 |
As3—C43 | 1.946 (6) | C39—C40 | 1.375 (9) |
As4—C67 | 1.932 (6) | C39—H39 | 0.9500 |
As4—C55 | 1.944 (5) | C40—C41 | 1.395 (10) |
As4—C61 | 1.952 (5) | C40—H40 | 0.9500 |
C1—C2 | 1.3900 | C41—C42 | 1.364 (9) |
C1—C6 | 1.3900 | C41—H41 | 0.9500 |
C2—C3 | 1.3900 | C42—H42 | 0.9500 |
C2—H2 | 0.9500 | C43—C48 | 1.374 (8) |
C3—C4 | 1.3900 | C43—C44 | 1.379 (8) |
C3—H3A | 0.9500 | C44—C45 | 1.400 (9) |
C4—C5 | 1.3900 | C44—H44 | 0.9500 |
C4—H4 | 0.9500 | C45—C46 | 1.369 (9) |
C5—C6 | 1.3900 | C45—H45 | 0.9500 |
C5—H5 | 0.9500 | C46—C47 | 1.361 (9) |
C6—H6 | 0.9500 | C46—H46 | 0.9500 |
C1'—C2' | 1.3900 | C47—C48 | 1.396 (8) |
C1'—C6' | 1.3900 | C47—H47 | 0.9500 |
C2'—C3' | 1.3900 | C48—H48 | 0.9500 |
C2'—H2' | 0.9500 | C49—C54 | 1.377 (8) |
C3'—C4' | 1.3900 | C49—C50 | 1.393 (8) |
C3'—H3' | 0.9500 | C50—C51 | 1.380 (9) |
C4'—C5' | 1.3900 | C50—H50 | 0.9500 |
C4'—H4' | 0.9500 | C51—C52 | 1.375 (10) |
C5'—C6' | 1.3900 | C51—H51 | 0.9500 |
C5'—H5' | 0.9500 | C52—C53 | 1.382 (10) |
C6'—H6' | 0.9500 | C52—H52 | 0.9500 |
C7—C8 | 1.383 (7) | C53—C54 | 1.396 (8) |
C7—C12 | 1.385 (7) | C53—H53 | 0.9500 |
C8—C9 | 1.389 (8) | C54—H54 | 0.9500 |
C8—H8 | 0.9500 | C55—C56 | 1.394 (7) |
C9—C10 | 1.379 (9) | C55—C60 | 1.398 (7) |
C9—H9 | 0.9500 | C56—C57 | 1.387 (8) |
C10—C11 | 1.376 (9) | C56—H56 | 0.9500 |
C10—H10 | 0.9500 | C57—C58 | 1.369 (8) |
C11—C12 | 1.383 (8) | C57—H57 | 0.9500 |
C11—H11 | 0.9500 | C58—C59 | 1.395 (9) |
C12—H12 | 0.9500 | C58—H58 | 0.9500 |
C13—C14 | 1.373 (7) | C59—C60 | 1.373 (8) |
C13—C18 | 1.380 (7) | C59—H59 | 0.9500 |
C14—C15 | 1.389 (7) | C60—H60 | 0.9500 |
C14—H14 | 0.9500 | C61—C62 | 1.369 (8) |
C15—C16 | 1.368 (8) | C61—C66 | 1.369 (7) |
C15—H15 | 0.9500 | C62—C63 | 1.392 (8) |
C16—C17 | 1.369 (9) | C62—H62 | 0.9500 |
C16—H16 | 0.9500 | C63—C64 | 1.334 (10) |
C17—C18 | 1.389 (8) | C63—H63 | 0.9500 |
C17—H17 | 0.9500 | C64—C65 | 1.345 (10) |
C18—H18 | 0.9500 | C64—H64 | 0.9500 |
C19—C20 | 1.3900 | C65—C66 | 1.396 (8) |
C19—C24 | 1.3900 | C65—H65 | 0.9500 |
C20—C21 | 1.3900 | C66—H66 | 0.9500 |
C20—H20 | 0.9500 | C67—C72 | 1.388 (8) |
C21—C22 | 1.3900 | C67—C68 | 1.398 (8) |
C21—H21 | 0.9500 | C68—C69 | 1.394 (9) |
C22—C23 | 1.3900 | C68—H68 | 0.9500 |
C22—H22 | 0.9500 | C69—C70 | 1.376 (11) |
C23—C24 | 1.3900 | C69—H69 | 0.9500 |
C23—H23 | 0.9500 | C70—C71 | 1.357 (10) |
C24—H24 | 0.9500 | C70—H70 | 0.9500 |
C19'—C20' | 1.3900 | C71—C72 | 1.399 (8) |
C19'—C24' | 1.3900 | C71—H71 | 0.9500 |
C20'—C21' | 1.3900 | C72—H72 | 0.9500 |
C20'—H20B | 0.9500 | F1—C74 | 1.318 (8) |
C21'—C22' | 1.3900 | F2—C74 | 1.330 (8) |
C21'—H21B | 0.9500 | F3—C74 | 1.300 (8) |
C22'—C23' | 1.3900 | O1—C73 | 1.223 (8) |
C22'—H22B | 0.9500 | O2—C73 | 1.244 (8) |
C23'—C24' | 1.3900 | O3—C75 | 1.431 (10) |
C23'—H23B | 0.9500 | O3—H3 | 0.8400 |
C24'—H24B | 0.9500 | C73—C74 | 1.501 (9) |
C25—C30 | 1.384 (7) | C75—H75A | 0.9800 |
C25—C26 | 1.388 (7) | C75—H75B | 0.9800 |
C26—C27 | 1.388 (7) | C75—H75C | 0.9800 |
C26—H26 | 0.9500 | F1'—C74' | 1.342 (9) |
C27—C28 | 1.385 (8) | F2'—C74' | 1.359 (9) |
C27—H27 | 0.9500 | F3'—C74' | 1.363 (9) |
C28—C29 | 1.372 (8) | O1'—C73' | 1.244 (8) |
C28—H28 | 0.9500 | O2'—C73' | 1.241 (8) |
C29—C30 | 1.387 (7) | O1W'—H1W1 | 0.8401 |
C29—H29 | 0.9500 | O1W'—H2W2 | 0.8400 |
C30—H30 | 0.9500 | C73'—C74' | 1.509 (9) |
C31—C32 | 1.392 (7) | ||
As3—Ag1—As2 | 109.89 (2) | C29—C28—H28 | 120.4 |
As3—Ag1—As1 | 109.00 (2) | C27—C28—H28 | 120.4 |
As2—Ag1—As1 | 110.713 (19) | C28—C29—C30 | 121.4 (5) |
As3—Ag1—As4 | 108.64 (2) | C28—C29—H29 | 119.3 |
As2—Ag1—As4 | 108.65 (2) | C30—C29—H29 | 119.3 |
As1—Ag1—As4 | 109.92 (2) | C25—C30—C29 | 119.3 (5) |
C1—As1—C7 | 102.1 (3) | C25—C30—H30 | 120.4 |
C1—As1—C13 | 105.3 (3) | C29—C30—H30 | 120.4 |
C7—As1—C13 | 99.5 (2) | C32—C31—C36 | 119.3 (5) |
C7—As1—C1' | 100.6 (3) | C32—C31—As2 | 121.8 (4) |
C13—As1—C1' | 99.9 (4) | C36—C31—As2 | 118.8 (4) |
C1—As1—Ag1 | 110.8 (3) | C33—C32—C31 | 120.1 (5) |
C7—As1—Ag1 | 119.45 (14) | C33—C32—H32 | 119.9 |
C13—As1—Ag1 | 117.58 (15) | C31—C32—H32 | 119.9 |
C1'—As1—Ag1 | 116.3 (3) | C34—C33—C32 | 120.0 (6) |
C31—As2—C19 | 100.8 (4) | C34—C33—H33 | 120.0 |
C31—As2—C19' | 100.5 (4) | C32—C33—H33 | 120.0 |
C31—As2—C25 | 101.8 (2) | C33—C34—C35 | 120.3 (5) |
C19—As2—C25 | 100.1 (3) | C33—C34—H34 | 119.9 |
C19'—As2—C25 | 101.3 (3) | C35—C34—H34 | 119.9 |
C31—As2—Ag1 | 115.77 (14) | C34—C35—C36 | 120.1 (6) |
C19—As2—Ag1 | 120.7 (4) | C34—C35—H35 | 119.9 |
C19'—As2—Ag1 | 120.0 (4) | C36—C35—H35 | 119.9 |
C25—As2—Ag1 | 114.70 (14) | C35—C36—C31 | 120.1 (6) |
C49—As3—C37 | 100.6 (2) | C35—C36—H36 | 119.9 |
C49—As3—C43 | 102.0 (2) | C31—C36—H36 | 119.9 |
C37—As3—C43 | 102.4 (2) | C38—C37—C42 | 120.4 (6) |
C49—As3—Ag1 | 113.53 (15) | C38—C37—As3 | 118.1 (4) |
C37—As3—Ag1 | 118.41 (18) | C42—C37—As3 | 121.5 (5) |
C43—As3—Ag1 | 117.25 (15) | C39—C38—C37 | 120.3 (5) |
C67—As4—C55 | 102.0 (2) | C39—C38—H38 | 119.9 |
C67—As4—C61 | 100.7 (2) | C37—C38—H38 | 119.9 |
C55—As4—C61 | 101.4 (2) | C38—C39—C40 | 120.2 (6) |
C67—As4—Ag1 | 118.22 (18) | C38—C39—H39 | 119.9 |
C55—As4—Ag1 | 119.10 (14) | C40—C39—H39 | 119.9 |
C61—As4—Ag1 | 112.61 (16) | C39—C40—C41 | 118.8 (7) |
C2—C1—C6 | 120.0 | C39—C40—H40 | 120.6 |
C2—C1—As1 | 117.7 (6) | C41—C40—H40 | 120.6 |
C6—C1—As1 | 122.2 (6) | C42—C41—C40 | 121.6 (7) |
C1—C2—C3 | 120.0 | C42—C41—H41 | 119.2 |
C1—C2—H2 | 120.0 | C40—C41—H41 | 119.2 |
C3—C2—H2 | 120.0 | C41—C42—C37 | 118.6 (6) |
C4—C3—C2 | 120.0 | C41—C42—H42 | 120.7 |
C4—C3—H3A | 120.0 | C37—C42—H42 | 120.7 |
C2—C3—H3A | 120.0 | C48—C43—C44 | 119.6 (6) |
C5—C4—C3 | 120.0 | C48—C43—As3 | 122.0 (4) |
C5—C4—H4 | 120.0 | C44—C43—As3 | 118.3 (4) |
C3—C4—H4 | 120.0 | C43—C44—C45 | 119.3 (6) |
C4—C5—C6 | 120.0 | C43—C44—H44 | 120.3 |
C4—C5—H5 | 120.0 | C45—C44—H44 | 120.3 |
C6—C5—H5 | 120.0 | C46—C45—C44 | 120.8 (6) |
C5—C6—C1 | 120.0 | C46—C45—H45 | 119.6 |
C5—C6—H6 | 120.0 | C44—C45—H45 | 119.6 |
C1—C6—H6 | 120.0 | C47—C46—C45 | 119.6 (6) |
C2'—C1'—C6' | 120.0 | C47—C46—H46 | 120.2 |
C2'—C1'—As1 | 117.0 (6) | C45—C46—H46 | 120.2 |
C6'—C1'—As1 | 122.5 (6) | C46—C47—C48 | 120.4 (6) |
C1'—C2'—C3' | 120.0 | C46—C47—H47 | 119.8 |
C1'—C2'—H2' | 120.0 | C48—C47—H47 | 119.8 |
C3'—C2'—H2' | 120.0 | C43—C48—C47 | 120.2 (6) |
C2'—C3'—C4' | 120.0 | C43—C48—H48 | 119.9 |
C2'—C3'—H3' | 120.0 | C47—C48—H48 | 119.9 |
C4'—C3'—H3' | 120.0 | C54—C49—C50 | 120.2 (6) |
C5'—C4'—C3' | 120.0 | C54—C49—As3 | 118.3 (4) |
C5'—C4'—H4' | 120.0 | C50—C49—As3 | 121.4 (4) |
C3'—C4'—H4' | 120.0 | C51—C50—C49 | 119.8 (6) |
C4'—C5'—C6' | 120.0 | C51—C50—H50 | 120.1 |
C4'—C5'—H5' | 120.0 | C49—C50—H50 | 120.1 |
C6'—C5'—H5' | 120.0 | C52—C51—C50 | 120.1 (6) |
C5'—C6'—C1' | 120.0 | C52—C51—H51 | 119.9 |
C5'—C6'—H6' | 120.0 | C50—C51—H51 | 119.9 |
C1'—C6'—H6' | 120.0 | C51—C52—C53 | 120.4 (6) |
C8—C7—C12 | 119.3 (5) | C51—C52—H52 | 119.8 |
C8—C7—As1 | 118.7 (4) | C53—C52—H52 | 119.8 |
C12—C7—As1 | 121.8 (4) | C52—C53—C54 | 119.8 (6) |
C7—C8—C9 | 120.0 (5) | C52—C53—H53 | 120.1 |
C7—C8—H8 | 120.0 | C54—C53—H53 | 120.1 |
C9—C8—H8 | 120.0 | C49—C54—C53 | 119.5 (6) |
C10—C9—C8 | 120.2 (6) | C49—C54—H54 | 120.2 |
C10—C9—H9 | 119.9 | C53—C54—H54 | 120.2 |
C8—C9—H9 | 119.9 | C56—C55—C60 | 118.5 (5) |
C11—C10—C9 | 119.9 (5) | C56—C55—As4 | 118.4 (4) |
C11—C10—H10 | 120.1 | C60—C55—As4 | 123.0 (4) |
C9—C10—H10 | 120.1 | C57—C56—C55 | 120.2 (5) |
C10—C11—C12 | 120.0 (6) | C57—C56—H56 | 119.9 |
C10—C11—H11 | 120.0 | C55—C56—H56 | 119.9 |
C12—C11—H11 | 120.0 | C58—C57—C56 | 120.8 (6) |
C11—C12—C7 | 120.5 (5) | C58—C57—H57 | 119.6 |
C11—C12—H12 | 119.8 | C56—C57—H57 | 119.6 |
C7—C12—H12 | 119.8 | C57—C58—C59 | 119.5 (6) |
C14—C13—C18 | 119.0 (5) | C57—C58—H58 | 120.3 |
C14—C13—As1 | 122.5 (4) | C59—C58—H58 | 120.3 |
C18—C13—As1 | 118.4 (4) | C60—C59—C58 | 120.2 (6) |
C13—C14—C15 | 120.5 (5) | C60—C59—H59 | 119.9 |
C13—C14—H14 | 119.8 | C58—C59—H59 | 119.9 |
C15—C14—H14 | 119.8 | C59—C60—C55 | 120.7 (5) |
C16—C15—C14 | 120.4 (5) | C59—C60—H60 | 119.6 |
C16—C15—H15 | 119.8 | C55—C60—H60 | 119.6 |
C14—C15—H15 | 119.8 | C62—C61—C66 | 118.9 (5) |
C15—C16—C17 | 119.5 (5) | C62—C61—As4 | 118.4 (4) |
C15—C16—H16 | 120.3 | C66—C61—As4 | 122.7 (4) |
C17—C16—H16 | 120.3 | C61—C62—C63 | 119.9 (6) |
C16—C17—C18 | 120.4 (6) | C61—C62—H62 | 120.0 |
C16—C17—H17 | 119.8 | C63—C62—H62 | 120.0 |
C18—C17—H17 | 119.8 | C64—C63—C62 | 120.8 (7) |
C13—C18—C17 | 120.2 (6) | C64—C63—H63 | 119.6 |
C13—C18—H18 | 119.9 | C62—C63—H63 | 119.6 |
C17—C18—H18 | 119.9 | C63—C64—C65 | 120.0 (6) |
C20—C19—C24 | 120.0 | C63—C64—H64 | 120.0 |
C20—C19—As2 | 120.1 (7) | C65—C64—H64 | 120.0 |
C24—C19—As2 | 119.9 (7) | C64—C65—C66 | 120.7 (6) |
C19—C20—C21 | 120.0 | C64—C65—H65 | 119.7 |
C19—C20—H20 | 120.0 | C66—C65—H65 | 119.7 |
C21—C20—H20 | 120.0 | C61—C66—C65 | 119.6 (6) |
C22—C21—C20 | 120.0 | C61—C66—H66 | 120.2 |
C22—C21—H21 | 120.0 | C65—C66—H66 | 120.2 |
C20—C21—H21 | 120.0 | C72—C67—C68 | 119.0 (6) |
C23—C22—C21 | 120.0 | C72—C67—As4 | 118.3 (5) |
C23—C22—H22 | 120.0 | C68—C67—As4 | 122.7 (5) |
C21—C22—H22 | 120.0 | C69—C68—C67 | 119.3 (7) |
C24—C23—C22 | 120.0 | C69—C68—H68 | 120.4 |
C24—C23—H23 | 120.0 | C67—C68—H68 | 120.4 |
C22—C23—H23 | 120.0 | C70—C69—C68 | 121.0 (7) |
C23—C24—C19 | 120.0 | C70—C69—H69 | 119.5 |
C23—C24—H24 | 120.0 | C68—C69—H69 | 119.5 |
C19—C24—H24 | 120.0 | C71—C70—C69 | 120.1 (6) |
C20'—C19'—C24' | 120.0 | C71—C70—H70 | 120.0 |
C20'—C19'—As2 | 117.7 (7) | C69—C70—H70 | 120.0 |
C24'—C19'—As2 | 122.2 (7) | C70—C71—C72 | 120.3 (7) |
C21'—C20'—C19' | 120.0 | C70—C71—H71 | 119.9 |
C21'—C20'—H20B | 120.0 | C72—C71—H71 | 119.9 |
C19'—C20'—H20B | 120.0 | C67—C72—C71 | 120.4 (6) |
C20'—C21'—C22' | 120.0 | C67—C72—H72 | 119.8 |
C20'—C21'—H21B | 120.0 | C71—C72—H72 | 119.8 |
C22'—C21'—H21B | 120.0 | C75—O3—H3 | 106.6 |
C21'—C22'—C23' | 120.0 | O1—C73—O2 | 125.7 (10) |
C21'—C22'—H22B | 120.0 | O1—C73—C74 | 117.8 (9) |
C23'—C22'—H22B | 120.0 | O2—C73—C74 | 116.5 (9) |
C24'—C23'—C22' | 120.0 | F3—C74—F1 | 109.0 (7) |
C24'—C23'—H23B | 120.0 | F3—C74—F2 | 107.1 (7) |
C22'—C23'—H23B | 120.0 | F1—C74—F2 | 108.9 (7) |
C23'—C24'—C19' | 120.0 | F3—C74—C73 | 108.4 (7) |
C23'—C24'—H24B | 120.0 | F1—C74—C73 | 113.4 (8) |
C19'—C24'—H24B | 120.0 | F2—C74—C73 | 109.9 (8) |
C30—C25—C26 | 119.9 (5) | H1W1—O1W'—H2W2 | 109.5 |
C30—C25—As2 | 122.4 (4) | O2'—C73'—O1' | 123.2 (10) |
C26—C25—As2 | 117.7 (4) | O2'—C73'—C74' | 117.2 (10) |
C27—C26—C25 | 120.0 (5) | O1'—C73'—C74' | 119.5 (10) |
C27—C26—H26 | 120.0 | F1'—C74'—F2' | 109.5 (8) |
C25—C26—H26 | 120.0 | F1'—C74'—F3' | 107.9 (9) |
C28—C27—C26 | 120.3 (5) | F2'—C74'—F3' | 108.2 (8) |
C28—C27—H27 | 119.9 | F1'—C74'—C73' | 108.6 (11) |
C26—C27—H27 | 119.9 | F2'—C74'—C73' | 112.2 (9) |
C29—C28—C27 | 119.2 (5) | F3'—C74'—C73' | 110.5 (9) |
As3—Ag1—As1—C1 | 172.1 (3) | C20'—C21'—C22'—C23' | 0.0 |
As2—Ag1—As1—C1 | −67.0 (3) | C21'—C22'—C23'—C24' | 0.0 |
As4—Ag1—As1—C1 | 53.1 (3) | C22'—C23'—C24'—C19' | 0.0 |
As3—Ag1—As1—C7 | 53.82 (17) | C20'—C19'—C24'—C23' | 0.0 |
As2—Ag1—As1—C7 | 174.81 (17) | As2—C19'—C24'—C23' | −176.8 (8) |
As4—Ag1—As1—C7 | −65.15 (17) | C31—As2—C25—C30 | −113.0 (4) |
As3—Ag1—As1—C13 | −66.81 (17) | C19—As2—C25—C30 | −9.6 (6) |
As2—Ag1—As1—C13 | 54.18 (17) | C19'—As2—C25—C30 | −9.6 (6) |
As4—Ag1—As1—C13 | 174.22 (17) | Ag1—As2—C25—C30 | 121.2 (4) |
As3—Ag1—As1—C1' | 174.8 (3) | C31—As2—C25—C26 | 69.3 (4) |
As2—Ag1—As1—C1' | −64.2 (3) | C19—As2—C25—C26 | 172.8 (6) |
As4—Ag1—As1—C1' | 55.9 (3) | C19'—As2—C25—C26 | 172.7 (5) |
As3—Ag1—As2—C31 | −175.46 (16) | Ag1—As2—C25—C26 | −56.5 (4) |
As1—Ag1—As2—C31 | 64.09 (16) | C30—C25—C26—C27 | 0.7 (8) |
As4—Ag1—As2—C31 | −56.72 (16) | As2—C25—C26—C27 | 178.4 (4) |
As3—Ag1—As2—C19 | 62.6 (4) | C25—C26—C27—C28 | −0.5 (9) |
As1—Ag1—As2—C19 | −57.9 (4) | C26—C27—C28—C29 | 0.7 (9) |
As4—Ag1—As2—C19 | −178.7 (4) | C27—C28—C29—C30 | −1.1 (9) |
As3—Ag1—As2—C19' | 63.7 (4) | C26—C25—C30—C29 | −1.0 (8) |
As1—Ag1—As2—C19' | −56.7 (4) | As2—C25—C30—C29 | −178.6 (4) |
As4—Ag1—As2—C19' | −177.6 (4) | C28—C29—C30—C25 | 1.2 (9) |
As3—Ag1—As2—C25 | −57.31 (17) | C19—As2—C31—C32 | −82.9 (5) |
As1—Ag1—As2—C25 | −177.77 (17) | C19'—As2—C31—C32 | −84.1 (5) |
As4—Ag1—As2—C25 | 61.42 (17) | C25—As2—C31—C32 | 20.0 (4) |
As2—Ag1—As3—C49 | −60.46 (19) | Ag1—As2—C31—C32 | 145.1 (4) |
As1—Ag1—As3—C49 | 61.03 (19) | C19—As2—C31—C36 | 94.1 (5) |
As4—Ag1—As3—C49 | −179.20 (19) | C19'—As2—C31—C36 | 92.9 (5) |
As2—Ag1—As3—C37 | 57.22 (19) | C25—As2—C31—C36 | −163.0 (4) |
As1—Ag1—As3—C37 | 178.71 (19) | Ag1—As2—C31—C36 | −37.9 (4) |
As4—Ag1—As3—C37 | −61.53 (19) | C36—C31—C32—C33 | −0.8 (8) |
As2—Ag1—As3—C43 | −179.14 (18) | As2—C31—C32—C33 | 176.1 (4) |
As1—Ag1—As3—C43 | −57.65 (18) | C31—C32—C33—C34 | −0.2 (9) |
As4—Ag1—As3—C43 | 62.12 (18) | C32—C33—C34—C35 | 0.9 (9) |
As3—Ag1—As4—C67 | 53.81 (18) | C33—C34—C35—C36 | −0.5 (9) |
As2—Ag1—As4—C67 | −65.71 (18) | C34—C35—C36—C31 | −0.6 (8) |
As1—Ag1—As4—C67 | 172.99 (18) | C32—C31—C36—C35 | 1.3 (8) |
As3—Ag1—As4—C55 | 178.48 (18) | As2—C31—C36—C35 | −175.8 (4) |
As2—Ag1—As4—C55 | 58.96 (18) | C49—As3—C37—C38 | 77.2 (5) |
As1—Ag1—As4—C55 | −62.33 (18) | C43—As3—C37—C38 | −177.9 (5) |
As3—Ag1—As4—C61 | −63.11 (17) | Ag1—As3—C37—C38 | −47.1 (5) |
As2—Ag1—As4—C61 | 177.37 (17) | C49—As3—C37—C42 | −102.5 (6) |
As1—Ag1—As4—C61 | 56.08 (17) | C43—As3—C37—C42 | 2.5 (6) |
C7—As1—C1—C2 | 78.7 (5) | Ag1—As3—C37—C42 | 133.2 (5) |
C13—As1—C1—C2 | −177.7 (4) | C42—C37—C38—C39 | 1.4 (10) |
C1'—As1—C1—C2 | 155 (5) | As3—C37—C38—C39 | −178.2 (5) |
Ag1—As1—C1—C2 | −49.6 (5) | C37—C38—C39—C40 | −1.0 (11) |
C7—As1—C1—C6 | −104.6 (6) | C38—C39—C40—C41 | 0.9 (13) |
C13—As1—C1—C6 | −1.1 (6) | C39—C40—C41—C42 | −1.4 (15) |
C1'—As1—C1—C6 | −28 (5) | C40—C41—C42—C37 | 1.9 (14) |
Ag1—As1—C1—C6 | 127.1 (5) | C38—C37—C42—C41 | −1.8 (11) |
C6—C1—C2—C3 | 0.0 | As3—C37—C42—C41 | 177.8 (7) |
As1—C1—C2—C3 | 176.7 (7) | C49—As3—C43—C48 | 6.9 (5) |
C1—C2—C3—C4 | 0.0 | C37—As3—C43—C48 | −97.0 (5) |
C2—C3—C4—C5 | 0.0 | Ag1—As3—C43—C48 | 131.5 (4) |
C3—C4—C5—C6 | 0.0 | C49—As3—C43—C44 | −169.8 (4) |
C4—C5—C6—C1 | 0.0 | C37—As3—C43—C44 | 86.3 (5) |
C2—C1—C6—C5 | 0.0 | Ag1—As3—C43—C44 | −45.2 (5) |
As1—C1—C6—C5 | −176.6 (7) | C48—C43—C44—C45 | 0.9 (9) |
C1—As1—C1'—C2' | −5 (5) | As3—C43—C44—C45 | 177.7 (5) |
C7—As1—C1'—C2' | 100.1 (5) | C43—C44—C45—C46 | 0.1 (10) |
C13—As1—C1'—C2' | −158.1 (4) | C44—C45—C46—C47 | −1.2 (10) |
Ag1—As1—C1'—C2' | −30.4 (5) | C45—C46—C47—C48 | 1.3 (10) |
C1—As1—C1'—C6' | −177 (5) | C44—C43—C48—C47 | −0.9 (9) |
C7—As1—C1'—C6' | −71.8 (5) | As3—C43—C48—C47 | −177.5 (5) |
C13—As1—C1'—C6' | 30.0 (5) | C46—C47—C48—C43 | −0.2 (10) |
Ag1—As1—C1'—C6' | 157.6 (4) | C37—As3—C49—C54 | −164.2 (4) |
C6'—C1'—C2'—C3' | 0.0 | C43—As3—C49—C54 | 90.5 (5) |
As1—C1'—C2'—C3' | −172.2 (7) | Ag1—As3—C49—C54 | −36.7 (5) |
C1'—C2'—C3'—C4' | 0.0 | C37—As3—C49—C50 | 12.7 (5) |
C2'—C3'—C4'—C5' | 0.0 | C43—As3—C49—C50 | −92.6 (5) |
C3'—C4'—C5'—C6' | 0.0 | Ag1—As3—C49—C50 | 140.3 (4) |
C4'—C5'—C6'—C1' | 0.0 | C54—C49—C50—C51 | 0.6 (8) |
C2'—C1'—C6'—C5' | 0.0 | As3—C49—C50—C51 | −176.3 (4) |
As1—C1'—C6'—C5' | 171.7 (7) | C49—C50—C51—C52 | 0.1 (9) |
C1—As1—C7—C8 | −160.0 (5) | C50—C51—C52—C53 | −0.4 (9) |
C13—As1—C7—C8 | 91.9 (4) | C51—C52—C53—C54 | 0.0 (9) |
C1'—As1—C7—C8 | −166.0 (5) | C50—C49—C54—C53 | −0.9 (9) |
Ag1—As1—C7—C8 | −37.4 (5) | As3—C49—C54—C53 | 176.0 (4) |
C1—As1—C7—C12 | 23.9 (5) | C52—C53—C54—C49 | 0.6 (9) |
C13—As1—C7—C12 | −84.1 (4) | C67—As4—C55—C56 | 82.8 (4) |
C1'—As1—C7—C12 | 18.0 (5) | C61—As4—C55—C56 | −173.5 (4) |
Ag1—As1—C7—C12 | 146.5 (4) | Ag1—As4—C55—C56 | −49.4 (5) |
C12—C7—C8—C9 | 1.2 (8) | C67—As4—C55—C60 | −98.3 (5) |
As1—C7—C8—C9 | −174.9 (4) | C61—As4—C55—C60 | 5.4 (5) |
C7—C8—C9—C10 | 0.1 (8) | Ag1—As4—C55—C60 | 129.5 (4) |
C8—C9—C10—C11 | −1.8 (9) | C60—C55—C56—C57 | −0.3 (8) |
C9—C10—C11—C12 | 2.2 (9) | As4—C55—C56—C57 | 178.7 (4) |
C10—C11—C12—C7 | −0.9 (8) | C55—C56—C57—C58 | 1.3 (9) |
C8—C7—C12—C11 | −0.8 (8) | C56—C57—C58—C59 | −1.4 (10) |
As1—C7—C12—C11 | 175.2 (4) | C57—C58—C59—C60 | 0.4 (10) |
C1—As1—C13—C14 | −96.6 (5) | C58—C59—C60—C55 | 0.6 (10) |
C7—As1—C13—C14 | 8.9 (5) | C56—C55—C60—C59 | −0.7 (9) |
C1'—As1—C13—C14 | −93.8 (5) | As4—C55—C60—C59 | −179.6 (5) |
Ag1—As1—C13—C14 | 139.5 (4) | C67—As4—C61—C62 | −168.3 (5) |
C1—As1—C13—C18 | 87.1 (6) | C55—As4—C61—C62 | 86.9 (5) |
C7—As1—C13—C18 | −167.4 (5) | Ag1—As4—C61—C62 | −41.4 (5) |
C1'—As1—C13—C18 | 89.9 (6) | C67—As4—C61—C66 | 9.8 (5) |
Ag1—As1—C13—C18 | −36.9 (5) | C55—As4—C61—C66 | −94.9 (5) |
C18—C13—C14—C15 | 1.3 (9) | Ag1—As4—C61—C66 | 136.7 (5) |
As1—C13—C14—C15 | −175.0 (4) | C66—C61—C62—C63 | −1.1 (10) |
C13—C14—C15—C16 | −0.7 (9) | As4—C61—C62—C63 | 177.2 (6) |
C14—C15—C16—C17 | 0.9 (9) | C61—C62—C63—C64 | 2.4 (12) |
C15—C16—C17—C18 | −1.7 (11) | C62—C63—C64—C65 | −2.5 (12) |
C14—C13—C18—C17 | −2.2 (10) | C63—C64—C65—C66 | 1.3 (12) |
As1—C13—C18—C17 | 174.3 (6) | C62—C61—C66—C65 | −0.1 (10) |
C16—C17—C18—C13 | 2.4 (11) | As4—C61—C66—C65 | −178.2 (5) |
C31—As2—C19—C20 | −148.8 (5) | C64—C65—C66—C61 | 0.0 (11) |
C19'—As2—C19—C20 | −75 (37) | C55—As4—C67—C72 | −151.8 (4) |
C25—As2—C19—C20 | 107.0 (5) | C61—As4—C67—C72 | 104.0 (4) |
Ag1—As2—C19—C20 | −19.9 (6) | Ag1—As4—C67—C72 | −19.1 (5) |
C31—As2—C19—C24 | 29.6 (6) | C55—As4—C67—C68 | 32.0 (5) |
C19'—As2—C19—C24 | 104 (37) | C61—As4—C67—C68 | −72.2 (5) |
C25—As2—C19—C24 | −74.6 (6) | Ag1—As4—C67—C68 | 164.7 (4) |
Ag1—As2—C19—C24 | 158.5 (4) | C72—C67—C68—C69 | −2.5 (9) |
C24—C19—C20—C21 | 0.0 | As4—C67—C68—C69 | 173.7 (5) |
As2—C19—C20—C21 | 178.4 (8) | C67—C68—C69—C70 | 1.4 (10) |
C19—C20—C21—C22 | 0.0 | C68—C69—C70—C71 | 0.6 (10) |
C20—C21—C22—C23 | 0.0 | C69—C70—C71—C72 | −1.5 (10) |
C21—C22—C23—C24 | 0.0 | C68—C67—C72—C71 | 1.7 (8) |
C22—C23—C24—C19 | 0.0 | As4—C67—C72—C71 | −174.7 (4) |
C20—C19—C24—C23 | 0.0 | C70—C71—C72—C67 | 0.4 (9) |
As2—C19—C24—C23 | −178.4 (8) | O1—C73—C74—F3 | −31.9 (13) |
C31—As2—C19'—C20' | −173.9 (5) | O2—C73—C74—F3 | 147.7 (11) |
C19—As2—C19'—C20' | 80 (37) | O1—C73—C74—F1 | −153.1 (10) |
C25—As2—C19'—C20' | 81.7 (5) | O2—C73—C74—F1 | 26.5 (14) |
Ag1—As2—C19'—C20' | −45.7 (6) | O1—C73—C74—F2 | 84.7 (12) |
C31—As2—C19'—C24' | 2.9 (6) | O2—C73—C74—F2 | −95.6 (12) |
C19—As2—C19'—C24' | −103 (37) | O2'—C73'—C74'—F1' | 144.6 (12) |
C25—As2—C19'—C24' | −101.5 (6) | O1'—C73'—C74'—F1' | −39.7 (15) |
Ag1—As2—C19'—C24' | 131.1 (5) | O2'—C73'—C74'—F2' | 23.5 (15) |
C24'—C19'—C20'—C21' | 0.0 | O1'—C73'—C74'—F2' | −160.8 (11) |
As2—C19'—C20'—C21' | 176.9 (8) | O2'—C73'—C74'—F3' | −97.3 (13) |
C19'—C20'—C21'—C22' | 0.0 | O1'—C73'—C74'—F3' | 78.5 (14) |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O1 | 0.84 | 1.97 | 2.80 (2) | 175 |
O1w'—H1w1···O1′ | 0.84 | 2.02 | 2.86 (3) | 179 |
Experimental details
Crystal data | |
Chemical formula | [Ag(C18H15As)4](C2F3O2)·0.5CH4O·0.5H2O |
Mr | 1470.80 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 100 |
a, b, c (Å) | 11.9069 (2), 14.5530 (3), 18.5573 (4) |
α, β, γ (°) | 88.893 (2), 85.782 (1), 86.808 (1) |
V (Å3) | 3201.57 (11) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.42 |
Crystal size (mm) | 0.22 × 0.17 × 0.11 |
Data collection | |
Diffractometer | Bruker SMART APEX diffractometer |
Absorption correction | Multi-scan (TWINABS; Bruker, 2009) |
Tmin, Tmax | 0.618, 0.776 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 48380, 14449, 10289 |
Rint | 0.058 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.048, 0.111, 1.03 |
No. of reflections | 14449 |
No. of parameters | 838 |
No. of restraints | 197 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.08, −0.56 |
Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2010).
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3···O1 | 0.84 | 1.97 | 2.80 (2) | 175 |
O1w'—H1w1···O1' | 0.84 | 2.02 | 2.86 (3) | 179 |
Acknowledgements
I thank Dr Kong Mun Lo for providing the crystal and the Ministry of Higher Education of Malaysia (grant No. UM.C/HIR/MOHE/SC/12) for supporting this study.
References
Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191. CrossRef CAS Google Scholar
Bruker (2009). APEX2, SAINT and TWINABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Ng, S. W. (2012). Acta Cryst. E68, m1536. CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar
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Silver trifluoroacetate reacts with triphenylphosphine in a 1:4 stoichiometry in ethanol to from the salt, [Ag(C18H15P)4](CF3CO2).C2H5OH (Ng, 2012). The corresponding reaction with triphenylarsane in methanol medium yielded [Ag(C18H15As)4](CF3CO2).0.5H2O.0.5CH3OH, which has somewhat different solvent molecules (Scheme I, Fig. 1). Four arsane ligands bind to the metal atom; the trifluoacetate anion does not engaged in coordination, and is instead disordered with respect to methanol and water molecules. The disorder is such that the anion occupies two positions, as does the two solvent molecules (Fig. 2). The anion and solvent are engaged in weak hydrogen bonding (Table 1).