Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104001556/ta1433sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270104001556/ta1433Isup2.hkl |
CCDC reference: 235318
The title compound was obtained as prismatic crystals from the reaction of silver trifluoroacetate, triphenylphosphine, bis(trifluoroacetic) anhydride and dimethyltin oxide in a 1:4:2:1 ratio. Silver trifluoroacetate (0.22 g, 1 mmol) and triphenylphosphine (1.05 g, 4 mmol) were heated in ethanol (25 ml); bis(trifluoroacetic) anhydride (0.42 g, 2 mmol) and dimethyltin oxide (0.16 g, 1 mmol) were also heated in ethanol (25 ml) until the oxide dissolved completely. The two hot solutions were mixed. The filtered mixture was allowed to cool over a period of 1 d, furnishing the silver stannate. The large prisms were not suitable for diffraction as all had a milky portion in the middle; an irregularly shaped specimen was cut from a large prism for the measurements.
A 2θ-dependent absorption was applied by assuming 2υ*diameter = 0.24. The final difference Fourier map had a large peaks at about 1 Å from the the Sn and Ag atoms. One of the three trifluoromethyl groups is disordered over two sites, and the disorder was refined as a 50:50 disorder. The six C—F distances were restrained to 1.32 (1) Å and the F···F distance was restrained to 2.16 (1) Å. Additionally, the six F atoms for each group were restrained to lie in a plane. The H atoms were placed at calculated positions and were included in the refinements in the riding-model approximation (C—H = 0.94 Å for the aromatic H atoms and 0.97 Å for the aliphatic H atoms). The H-atom displacement parameters were set to 1.2Ueq of the C atoms. The torsion angles of the methyl groups were refined.
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
[Ag(C18H15P)4]2[Sn2(CH3)4(C2F3O2)6] | Z = 1 |
Mr = 3289.54 | F(000) = 1664 |
Triclinic, P1 | Dx = 1.507 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.9439 (6) Å | Cell parameters from 5859 reflections |
b = 14.0499 (6) Å | θ = 2.3–27.7° |
c = 20.7267 (9) Å | µ = 0.78 mm−1 |
α = 100.370 (1)° | T = 223 K |
β = 99.429 (1)° | Irregular block, colorless |
γ = 95.899 (1)° | 0.31 × 0.25 × 0.20 mm |
V = 3623.6 (3) Å3 |
Bruker APEX area-detector diffractometer | 16043 independent reflections |
Radiation source: fine-focus sealed tube | 11658 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
ϕ and ω scan | θmax = 27.5°, θmin = 1.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −16→16 |
Tmin = 0.672, Tmax = 0.837 | k = −18→18 |
31408 measured reflections | l = −26→26 |
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) = 0.113 | H-atom parameters constrained |
S = 0.92 | w = 1/[σ2(Fo2) + (0.058P)2] where P = (Fo2 + 2Fc2)/3 |
16043 reflections | (Δ/σ)max = 0.001 |
939 parameters | Δρmax = 1.39 e Å−3 |
15 restraints | Δρmin = −0.83 e Å−3 |
[Ag(C18H15P)4]2[Sn2(CH3)4(C2F3O2)6] | γ = 95.899 (1)° |
Mr = 3289.54 | V = 3623.6 (3) Å3 |
Triclinic, P1 | Z = 1 |
a = 12.9439 (6) Å | Mo Kα radiation |
b = 14.0499 (6) Å | µ = 0.78 mm−1 |
c = 20.7267 (9) Å | T = 223 K |
α = 100.370 (1)° | 0.31 × 0.25 × 0.20 mm |
β = 99.429 (1)° |
Bruker APEX area-detector diffractometer | 16043 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 11658 reflections with I > 2σ(I) |
Tmin = 0.672, Tmax = 0.837 | Rint = 0.031 |
31408 measured reflections |
R[F2 > 2σ(F2)] = 0.048 | 15 restraints |
wR(F2) = 0.113 | H-atom parameters constrained |
S = 0.92 | Δρmax = 1.39 e Å−3 |
16043 reflections | Δρmin = −0.83 e Å−3 |
939 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sn | 0.47439 (2) | 0.37240 (2) | 0.399750 (13) | 0.04302 (9) | |
Ag | 0.854661 (19) | 0.772858 (18) | 0.211129 (12) | 0.02934 (7) | |
P1 | 0.91374 (7) | 0.87396 (6) | 0.12589 (4) | 0.02685 (18) | |
P2 | 0.64793 (6) | 0.73477 (6) | 0.18460 (4) | 0.02718 (19) | |
P3 | 0.92937 (7) | 0.60420 (6) | 0.19892 (4) | 0.02687 (18) | |
P4 | 0.91833 (7) | 0.87582 (6) | 0.33351 (4) | 0.02861 (19) | |
F1 | 0.8323 (10) | 0.5074 (7) | 0.5769 (5) | 0.117 (5) | 0.50 |
F2 | 0.7756 (10) | 0.3558 (7) | 0.5613 (6) | 0.130 (6) | 0.50 |
F3 | 0.8556 (8) | 0.4093 (9) | 0.4912 (5) | 0.108 (5) | 0.50 |
F1' | 0.8031 (9) | 0.4794 (8) | 0.5946 (4) | 0.106 (4) | 0.50 |
F2' | 0.7970 (8) | 0.3390 (5) | 0.5363 (5) | 0.084 (3) | 0.50 |
F3' | 0.8670 (7) | 0.4615 (9) | 0.5051 (5) | 0.107 (5) | 0.50 |
F4 | 0.1075 (2) | 0.2683 (3) | 0.33188 (15) | 0.1142 (13) | |
F5 | 0.1467 (3) | 0.1819 (2) | 0.24693 (19) | 0.1100 (12) | |
F6 | 0.0926 (2) | 0.3139 (3) | 0.24010 (16) | 0.0959 (10) | |
F7 | 0.5110 (4) | 0.0680 (3) | 0.2171 (2) | 0.1600 (19) | |
F8 | 0.4461 (3) | 0.1762 (4) | 0.18131 (17) | 0.154 (2) | |
F9 | 0.6053 (3) | 0.1938 (3) | 0.22205 (19) | 0.1468 (19) | |
O1 | 0.6522 (2) | 0.3832 (2) | 0.43902 (14) | 0.0528 (7) | |
O2 | 0.6305 (3) | 0.5039 (3) | 0.51809 (15) | 0.0712 (9) | |
O3 | 0.3113 (2) | 0.3202 (2) | 0.35532 (13) | 0.0552 (7) | |
O4 | 0.3039 (3) | 0.3523 (3) | 0.25356 (16) | 0.0877 (12) | |
O5 | 0.5197 (2) | 0.28646 (19) | 0.31912 (13) | 0.0490 (7) | |
O6 | 0.4441 (3) | 0.1389 (2) | 0.3231 (2) | 0.0941 (13) | |
C1 | 0.8705 (2) | 0.9942 (2) | 0.12955 (17) | 0.0294 (7) | |
C2 | 0.8702 (3) | 1.0505 (3) | 0.1913 (2) | 0.0431 (9) | |
H2 | 0.8923 | 1.0262 | 0.2300 | 0.052* | |
C3 | 0.8381 (3) | 1.1416 (3) | 0.1973 (2) | 0.0571 (12) | |
H3 | 0.8395 | 1.1798 | 0.2397 | 0.068* | |
C4 | 0.8038 (3) | 1.1763 (3) | 0.1400 (3) | 0.0604 (13) | |
H4 | 0.7801 | 1.2378 | 0.1434 | 0.072* | |
C5 | 0.8044 (3) | 1.1217 (3) | 0.0793 (2) | 0.0519 (11) | |
H5 | 0.7821 | 1.1462 | 0.0407 | 0.062* | |
C6 | 0.8372 (3) | 1.0306 (3) | 0.0729 (2) | 0.0400 (9) | |
H6 | 0.8369 | 0.9935 | 0.0303 | 0.048* | |
C7 | 1.0565 (3) | 0.8999 (2) | 0.13510 (16) | 0.0288 (7) | |
C8 | 1.1148 (3) | 0.8256 (3) | 0.1457 (2) | 0.0439 (9) | |
H8 | 1.0803 | 0.7649 | 0.1490 | 0.053* | |
C9 | 1.2234 (3) | 0.8396 (3) | 0.1516 (2) | 0.0550 (11) | |
H9 | 1.2626 | 0.7884 | 0.1586 | 0.066* | |
C10 | 1.2738 (3) | 0.9281 (3) | 0.1471 (2) | 0.0541 (11) | |
H10 | 1.3477 | 0.9382 | 0.1516 | 0.065* | |
C11 | 1.2162 (3) | 1.0017 (3) | 0.1363 (2) | 0.0585 (12) | |
H11 | 1.2510 | 1.0623 | 0.1331 | 0.070* | |
C12 | 1.1080 (3) | 0.9884 (3) | 0.1300 (2) | 0.0455 (10) | |
H12 | 1.0693 | 1.0396 | 0.1222 | 0.055* | |
C13 | 0.8732 (3) | 0.8196 (2) | 0.03750 (16) | 0.0297 (7) | |
C14 | 0.9431 (3) | 0.8119 (3) | −0.00643 (17) | 0.0383 (8) | |
H14 | 1.0152 | 0.8353 | 0.0092 | 0.046* | |
C15 | 0.9081 (3) | 0.7701 (3) | −0.07298 (19) | 0.0471 (10) | |
H15 | 0.9565 | 0.7653 | −0.1023 | 0.057* | |
C16 | 0.8037 (3) | 0.7358 (3) | −0.0967 (2) | 0.0517 (11) | |
H16 | 0.7799 | 0.7069 | −0.1420 | 0.062* | |
C17 | 0.7342 (3) | 0.7440 (3) | −0.0537 (2) | 0.0594 (12) | |
H17 | 0.6620 | 0.7216 | −0.0698 | 0.071* | |
C18 | 0.7686 (3) | 0.7848 (3) | 0.01294 (19) | 0.0481 (10) | |
H18 | 0.7198 | 0.7888 | 0.0420 | 0.058* | |
C19 | 0.5884 (2) | 0.7655 (2) | 0.25729 (16) | 0.0287 (7) | |
C20 | 0.6262 (3) | 0.7310 (3) | 0.31400 (17) | 0.0359 (8) | |
H20 | 0.6769 | 0.6877 | 0.3128 | 0.043* | |
C21 | 0.5894 (3) | 0.7599 (3) | 0.37201 (19) | 0.0508 (11) | |
H21 | 0.6150 | 0.7357 | 0.4101 | 0.061* | |
C22 | 0.5165 (3) | 0.8233 (3) | 0.3754 (2) | 0.0565 (12) | |
H22 | 0.4926 | 0.8429 | 0.4155 | 0.068* | |
C23 | 0.4781 (3) | 0.8583 (3) | 0.3197 (2) | 0.0501 (10) | |
H23 | 0.4279 | 0.9021 | 0.3217 | 0.060* | |
C24 | 0.5130 (3) | 0.8291 (3) | 0.26097 (18) | 0.0365 (8) | |
H24 | 0.4856 | 0.8525 | 0.2228 | 0.044* | |
C25 | 0.5964 (2) | 0.6067 (2) | 0.15031 (17) | 0.0319 (8) | |
C26 | 0.6312 (3) | 0.5628 (3) | 0.09392 (18) | 0.0390 (9) | |
H26 | 0.6761 | 0.6000 | 0.0737 | 0.047* | |
C27 | 0.6006 (3) | 0.4654 (3) | 0.0676 (2) | 0.0537 (11) | |
H27 | 0.6239 | 0.4363 | 0.0290 | 0.064* | |
C28 | 0.5363 (3) | 0.4106 (3) | 0.0969 (3) | 0.0667 (14) | |
H28 | 0.5170 | 0.3435 | 0.0791 | 0.080* | |
C29 | 0.4992 (3) | 0.4525 (3) | 0.1524 (2) | 0.0606 (13) | |
H29 | 0.4541 | 0.4147 | 0.1721 | 0.073* | |
C30 | 0.5292 (3) | 0.5513 (3) | 0.1789 (2) | 0.0430 (9) | |
H30 | 0.5038 | 0.5807 | 0.2165 | 0.052* | |
C31 | 0.5761 (3) | 0.7966 (3) | 0.12532 (16) | 0.0309 (7) | |
C32 | 0.4893 (3) | 0.7509 (3) | 0.07824 (18) | 0.0417 (9) | |
H32 | 0.4663 | 0.6842 | 0.0749 | 0.050* | |
C33 | 0.4358 (3) | 0.8028 (3) | 0.0358 (2) | 0.0540 (11) | |
H33 | 0.3772 | 0.7710 | 0.0032 | 0.065* | |
C34 | 0.4680 (3) | 0.8997 (3) | 0.0411 (2) | 0.0541 (11) | |
H34 | 0.4311 | 0.9347 | 0.0124 | 0.065* | |
C35 | 0.5539 (3) | 0.9469 (3) | 0.0883 (2) | 0.0498 (10) | |
H35 | 0.5755 | 1.0139 | 0.0920 | 0.060* | |
C36 | 0.6085 (3) | 0.8954 (3) | 0.13019 (18) | 0.0393 (9) | |
H36 | 0.6678 | 0.9273 | 0.1621 | 0.047* | |
C37 | 0.8860 (3) | 0.5191 (2) | 0.24914 (16) | 0.0301 (7) | |
C38 | 0.9539 (3) | 0.4870 (3) | 0.29654 (19) | 0.0408 (9) | |
H38 | 1.0269 | 0.5081 | 0.3037 | 0.049* | |
C39 | 0.9152 (3) | 0.4241 (3) | 0.3335 (2) | 0.0527 (11) | |
H39 | 0.9621 | 0.4019 | 0.3654 | 0.063* | |
C40 | 0.8100 (4) | 0.3940 (3) | 0.3243 (2) | 0.0510 (11) | |
H40 | 0.7841 | 0.3518 | 0.3502 | 0.061* | |
C41 | 0.7412 (3) | 0.4253 (3) | 0.2772 (2) | 0.0524 (11) | |
H41 | 0.6684 | 0.4032 | 0.2701 | 0.063* | |
C42 | 0.7790 (3) | 0.4886 (3) | 0.2406 (2) | 0.0437 (9) | |
H42 | 0.7315 | 0.5115 | 0.2095 | 0.052* | |
C43 | 0.8995 (2) | 0.5292 (2) | 0.11468 (16) | 0.0284 (7) | |
C44 | 0.8864 (3) | 0.5753 (3) | 0.06148 (18) | 0.0389 (9) | |
H44 | 0.8945 | 0.6439 | 0.0693 | 0.047* | |
C45 | 0.8615 (3) | 0.5229 (3) | −0.00337 (19) | 0.0498 (10) | |
H45 | 0.8511 | 0.5556 | −0.0392 | 0.060* | |
C46 | 0.8521 (3) | 0.4232 (3) | −0.0153 (2) | 0.0496 (10) | |
H46 | 0.8357 | 0.3872 | −0.0594 | 0.060* | |
C47 | 0.8666 (3) | 0.3758 (3) | 0.0372 (2) | 0.0485 (10) | |
H47 | 0.8605 | 0.3072 | 0.0289 | 0.058* | |
C48 | 0.8903 (3) | 0.4282 (2) | 0.10212 (18) | 0.0385 (8) | |
H48 | 0.9002 | 0.3952 | 0.1378 | 0.046* | |
C49 | 1.0725 (2) | 0.6158 (2) | 0.22105 (16) | 0.0291 (7) | |
C50 | 1.1326 (3) | 0.5512 (3) | 0.1915 (2) | 0.0420 (9) | |
H50 | 1.0999 | 0.4989 | 0.1567 | 0.050* | |
C51 | 1.2409 (3) | 0.5635 (3) | 0.2130 (2) | 0.0548 (11) | |
H51 | 1.2816 | 0.5201 | 0.1921 | 0.066* | |
C52 | 1.2894 (3) | 0.6382 (3) | 0.2644 (2) | 0.0503 (10) | |
H52 | 1.3631 | 0.6459 | 0.2788 | 0.060* | |
C53 | 1.2310 (3) | 0.7009 (3) | 0.2945 (2) | 0.0514 (11) | |
H53 | 1.2637 | 0.7518 | 0.3302 | 0.062* | |
C54 | 1.1233 (3) | 0.6899 (3) | 0.27253 (19) | 0.0425 (9) | |
H54 | 1.0835 | 0.7344 | 0.2934 | 0.051* | |
C55 | 0.8861 (3) | 0.8118 (2) | 0.39839 (16) | 0.0308 (7) | |
C56 | 0.8572 (3) | 0.8581 (3) | 0.45632 (17) | 0.0355 (8) | |
H56 | 0.8535 | 0.9255 | 0.4635 | 0.043* | |
C57 | 0.8339 (3) | 0.8057 (3) | 0.50347 (18) | 0.0411 (9) | |
H57 | 0.8138 | 0.8379 | 0.5424 | 0.049* | |
C58 | 0.8395 (3) | 0.7086 (3) | 0.4946 (2) | 0.0510 (10) | |
H58 | 0.8235 | 0.6735 | 0.5271 | 0.061* | |
C59 | 0.8692 (4) | 0.6618 (3) | 0.4373 (2) | 0.0565 (12) | |
H59 | 0.8741 | 0.5945 | 0.4309 | 0.068* | |
C60 | 0.8915 (3) | 0.7133 (3) | 0.38981 (19) | 0.0452 (10) | |
H60 | 0.9109 | 0.6807 | 0.3508 | 0.054* | |
C61 | 0.8638 (3) | 0.9897 (2) | 0.35458 (16) | 0.0311 (7) | |
C62 | 0.9234 (3) | 1.0777 (3) | 0.38586 (19) | 0.0444 (9) | |
H62 | 0.9975 | 1.0822 | 0.3954 | 0.053* | |
C63 | 0.8752 (3) | 1.1596 (3) | 0.4034 (2) | 0.0504 (10) | |
H63 | 0.9169 | 1.2196 | 0.4240 | 0.060* | |
C64 | 0.7678 (3) | 1.1540 (3) | 0.3911 (2) | 0.0485 (10) | |
H64 | 0.7354 | 1.2093 | 0.4044 | 0.058* | |
C65 | 0.7074 (3) | 1.0679 (3) | 0.3594 (2) | 0.0514 (11) | |
H65 | 0.6334 | 1.0642 | 0.3499 | 0.062* | |
C66 | 0.7549 (3) | 0.9857 (3) | 0.3412 (2) | 0.0434 (9) | |
H66 | 0.7127 | 0.9265 | 0.3195 | 0.052* | |
C67 | 1.0604 (3) | 0.9149 (2) | 0.35946 (17) | 0.0318 (8) | |
C68 | 1.1184 (3) | 0.8999 (3) | 0.41823 (19) | 0.0430 (9) | |
H68 | 1.0850 | 0.8664 | 0.4462 | 0.052* | |
C69 | 1.2253 (3) | 0.9340 (3) | 0.4360 (2) | 0.0525 (11) | |
H69 | 1.2644 | 0.9226 | 0.4755 | 0.063* | |
C70 | 1.2744 (3) | 0.9845 (3) | 0.3961 (2) | 0.0513 (11) | |
H70 | 1.3465 | 1.0095 | 0.4091 | 0.062* | |
C71 | 1.2188 (3) | 0.9982 (3) | 0.3377 (2) | 0.0490 (10) | |
H71 | 1.2530 | 1.0315 | 0.3099 | 0.059* | |
C72 | 1.1127 (3) | 0.9639 (3) | 0.31900 (19) | 0.0407 (9) | |
H72 | 1.0752 | 0.9736 | 0.2784 | 0.049* | |
C73 | 0.4916 (4) | 0.5019 (3) | 0.3648 (2) | 0.0573 (12) | |
H73a | 0.5459 | 0.5486 | 0.3957 | 0.086* | |
H73b | 0.4252 | 0.5285 | 0.3610 | 0.086* | |
H73c | 0.5119 | 0.4891 | 0.3213 | 0.086* | |
C74 | 0.4543 (4) | 0.2896 (3) | 0.4708 (2) | 0.0579 (12) | |
H74a | 0.4719 | 0.2248 | 0.4561 | 0.087* | |
H74b | 0.3813 | 0.2849 | 0.4767 | 0.087* | |
H74c | 0.5003 | 0.3204 | 0.5128 | 0.087* | |
C75 | 0.6807 (3) | 0.4412 (3) | 0.4935 (2) | 0.0483 (10) | |
C76 | 0.7883 (4) | 0.4301 (3) | 0.5323 (2) | 0.0650 (13) | |
C77 | 0.2668 (4) | 0.3204 (3) | 0.2971 (2) | 0.0549 (11) | |
C78 | 0.1518 (4) | 0.2711 (4) | 0.2806 (2) | 0.0629 (13) | |
C79 | 0.4884 (3) | 0.1979 (3) | 0.2973 (2) | 0.0539 (11) | |
C80 | 0.5142 (4) | 0.1639 (4) | 0.2278 (3) | 0.0712 (15) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn | 0.05393 (18) | 0.04473 (16) | 0.02979 (14) | 0.00111 (13) | 0.01053 (12) | 0.00660 (12) |
Ag | 0.02927 (14) | 0.03025 (14) | 0.02860 (14) | 0.00349 (10) | 0.00593 (10) | 0.00600 (11) |
P1 | 0.0289 (4) | 0.0268 (4) | 0.0259 (4) | 0.0027 (4) | 0.0064 (3) | 0.0075 (4) |
P2 | 0.0234 (4) | 0.0301 (5) | 0.0269 (4) | 0.0030 (4) | 0.0042 (3) | 0.0036 (4) |
P3 | 0.0272 (4) | 0.0251 (4) | 0.0299 (5) | 0.0048 (3) | 0.0082 (4) | 0.0063 (4) |
P4 | 0.0319 (5) | 0.0281 (4) | 0.0237 (4) | 0.0030 (4) | 0.0032 (4) | 0.0021 (3) |
F1 | 0.095 (8) | 0.103 (7) | 0.115 (10) | −0.005 (5) | −0.046 (7) | −0.012 (7) |
F2 | 0.178 (11) | 0.133 (11) | 0.102 (9) | 0.031 (8) | 0.024 (7) | 0.083 (8) |
F3 | 0.058 (6) | 0.156 (11) | 0.098 (7) | 0.023 (6) | −0.004 (5) | 0.009 (7) |
F1' | 0.098 (8) | 0.135 (10) | 0.061 (5) | 0.029 (7) | −0.034 (5) | −0.009 (6) |
F2' | 0.097 (6) | 0.069 (5) | 0.078 (6) | 0.020 (4) | −0.017 (5) | 0.019 (4) |
F3' | 0.044 (4) | 0.160 (11) | 0.132 (11) | −0.009 (6) | 0.000 (5) | 0.092 (9) |
F4 | 0.064 (2) | 0.214 (4) | 0.0577 (19) | −0.007 (2) | 0.0125 (16) | 0.022 (2) |
F5 | 0.099 (3) | 0.068 (2) | 0.136 (3) | −0.0066 (18) | −0.002 (2) | −0.020 (2) |
F6 | 0.069 (2) | 0.131 (3) | 0.091 (2) | 0.0325 (19) | 0.0007 (17) | 0.032 (2) |
F7 | 0.239 (6) | 0.087 (3) | 0.138 (4) | 0.020 (3) | 0.059 (4) | −0.038 (3) |
F8 | 0.139 (4) | 0.264 (6) | 0.059 (2) | 0.083 (4) | −0.001 (2) | 0.019 (3) |
F9 | 0.085 (3) | 0.212 (5) | 0.110 (3) | −0.039 (3) | 0.062 (2) | −0.061 (3) |
O1 | 0.0495 (17) | 0.0635 (19) | 0.0419 (16) | 0.0018 (14) | 0.0099 (13) | 0.0031 (14) |
O2 | 0.075 (2) | 0.083 (2) | 0.053 (2) | 0.0151 (19) | 0.0156 (17) | −0.0003 (18) |
O3 | 0.0525 (18) | 0.072 (2) | 0.0376 (16) | 0.0057 (15) | 0.0016 (13) | 0.0091 (14) |
O4 | 0.089 (3) | 0.119 (3) | 0.045 (2) | −0.021 (2) | −0.0024 (18) | 0.025 (2) |
O5 | 0.0615 (18) | 0.0413 (16) | 0.0405 (15) | −0.0050 (14) | 0.0184 (13) | −0.0027 (12) |
O6 | 0.102 (3) | 0.051 (2) | 0.137 (4) | −0.006 (2) | 0.062 (3) | 0.013 (2) |
C1 | 0.0253 (17) | 0.0282 (17) | 0.0355 (19) | 0.0009 (14) | 0.0074 (14) | 0.0084 (15) |
C2 | 0.045 (2) | 0.039 (2) | 0.046 (2) | 0.0053 (18) | 0.0154 (18) | 0.0059 (18) |
C3 | 0.060 (3) | 0.042 (2) | 0.070 (3) | 0.009 (2) | 0.027 (2) | −0.002 (2) |
C4 | 0.049 (3) | 0.032 (2) | 0.111 (4) | 0.0135 (19) | 0.027 (3) | 0.028 (3) |
C5 | 0.042 (2) | 0.046 (2) | 0.074 (3) | 0.0086 (19) | 0.009 (2) | 0.030 (2) |
C6 | 0.037 (2) | 0.037 (2) | 0.048 (2) | 0.0048 (16) | 0.0063 (17) | 0.0183 (18) |
C7 | 0.0290 (18) | 0.0332 (18) | 0.0251 (17) | 0.0034 (14) | 0.0073 (14) | 0.0063 (14) |
C8 | 0.040 (2) | 0.040 (2) | 0.054 (2) | 0.0059 (17) | 0.0083 (18) | 0.0161 (19) |
C9 | 0.037 (2) | 0.057 (3) | 0.073 (3) | 0.016 (2) | 0.004 (2) | 0.019 (2) |
C10 | 0.027 (2) | 0.065 (3) | 0.067 (3) | 0.000 (2) | 0.0089 (19) | 0.010 (2) |
C11 | 0.038 (2) | 0.047 (3) | 0.090 (4) | −0.006 (2) | 0.012 (2) | 0.020 (2) |
C12 | 0.039 (2) | 0.035 (2) | 0.064 (3) | 0.0033 (17) | 0.0093 (19) | 0.0156 (19) |
C13 | 0.0351 (19) | 0.0276 (17) | 0.0267 (17) | 0.0032 (14) | 0.0034 (14) | 0.0092 (14) |
C14 | 0.036 (2) | 0.050 (2) | 0.0303 (19) | 0.0029 (17) | 0.0073 (16) | 0.0101 (17) |
C15 | 0.053 (3) | 0.058 (3) | 0.033 (2) | 0.009 (2) | 0.0162 (18) | 0.0080 (19) |
C16 | 0.064 (3) | 0.055 (3) | 0.030 (2) | 0.000 (2) | 0.002 (2) | 0.0036 (19) |
C17 | 0.041 (2) | 0.083 (3) | 0.042 (2) | −0.016 (2) | −0.0006 (19) | 0.002 (2) |
C18 | 0.039 (2) | 0.061 (3) | 0.038 (2) | −0.0073 (19) | 0.0110 (18) | −0.0015 (19) |
C19 | 0.0237 (17) | 0.0294 (17) | 0.0295 (18) | −0.0053 (14) | 0.0039 (13) | 0.0025 (14) |
C20 | 0.037 (2) | 0.0340 (19) | 0.035 (2) | −0.0037 (16) | 0.0034 (16) | 0.0098 (16) |
C21 | 0.058 (3) | 0.062 (3) | 0.029 (2) | −0.013 (2) | 0.0050 (19) | 0.0137 (19) |
C22 | 0.057 (3) | 0.070 (3) | 0.037 (2) | −0.007 (2) | 0.023 (2) | −0.007 (2) |
C23 | 0.044 (2) | 0.055 (3) | 0.052 (3) | 0.009 (2) | 0.022 (2) | 0.000 (2) |
C24 | 0.0316 (19) | 0.042 (2) | 0.035 (2) | 0.0040 (16) | 0.0073 (15) | 0.0053 (16) |
C25 | 0.0188 (16) | 0.0341 (19) | 0.039 (2) | 0.0040 (14) | 0.0010 (14) | 0.0009 (15) |
C26 | 0.0297 (19) | 0.045 (2) | 0.039 (2) | 0.0061 (16) | 0.0044 (16) | 0.0010 (17) |
C27 | 0.040 (2) | 0.055 (3) | 0.056 (3) | 0.004 (2) | 0.010 (2) | −0.018 (2) |
C28 | 0.045 (3) | 0.040 (2) | 0.100 (4) | −0.007 (2) | 0.020 (3) | −0.024 (2) |
C29 | 0.043 (2) | 0.043 (2) | 0.088 (4) | −0.007 (2) | 0.022 (2) | −0.007 (2) |
C30 | 0.032 (2) | 0.037 (2) | 0.054 (2) | −0.0023 (16) | 0.0125 (18) | −0.0065 (18) |
C31 | 0.0287 (18) | 0.044 (2) | 0.0228 (17) | 0.0076 (15) | 0.0084 (14) | 0.0083 (15) |
C32 | 0.042 (2) | 0.041 (2) | 0.039 (2) | 0.0093 (18) | −0.0004 (17) | 0.0044 (17) |
C33 | 0.051 (3) | 0.067 (3) | 0.038 (2) | 0.017 (2) | −0.0068 (19) | 0.007 (2) |
C34 | 0.061 (3) | 0.065 (3) | 0.046 (3) | 0.021 (2) | 0.011 (2) | 0.027 (2) |
C35 | 0.060 (3) | 0.048 (2) | 0.052 (3) | 0.009 (2) | 0.025 (2) | 0.024 (2) |
C36 | 0.035 (2) | 0.048 (2) | 0.037 (2) | 0.0018 (17) | 0.0105 (16) | 0.0138 (18) |
C37 | 0.0346 (19) | 0.0260 (17) | 0.0323 (18) | 0.0059 (14) | 0.0115 (15) | 0.0064 (14) |
C38 | 0.038 (2) | 0.044 (2) | 0.045 (2) | 0.0075 (17) | 0.0099 (17) | 0.0164 (18) |
C39 | 0.059 (3) | 0.059 (3) | 0.051 (3) | 0.018 (2) | 0.014 (2) | 0.031 (2) |
C40 | 0.070 (3) | 0.042 (2) | 0.054 (3) | 0.010 (2) | 0.032 (2) | 0.022 (2) |
C41 | 0.042 (2) | 0.054 (3) | 0.069 (3) | 0.001 (2) | 0.023 (2) | 0.023 (2) |
C42 | 0.033 (2) | 0.047 (2) | 0.057 (3) | 0.0070 (17) | 0.0115 (18) | 0.020 (2) |
C43 | 0.0258 (17) | 0.0273 (17) | 0.0326 (18) | 0.0044 (14) | 0.0081 (14) | 0.0048 (14) |
C44 | 0.046 (2) | 0.034 (2) | 0.039 (2) | 0.0074 (17) | 0.0158 (17) | 0.0075 (17) |
C45 | 0.075 (3) | 0.047 (2) | 0.031 (2) | 0.013 (2) | 0.013 (2) | 0.0113 (18) |
C46 | 0.058 (3) | 0.049 (2) | 0.038 (2) | 0.004 (2) | 0.0129 (19) | −0.0045 (19) |
C47 | 0.056 (3) | 0.031 (2) | 0.057 (3) | 0.0036 (18) | 0.018 (2) | −0.0020 (19) |
C48 | 0.048 (2) | 0.0295 (19) | 0.039 (2) | 0.0066 (17) | 0.0096 (17) | 0.0061 (16) |
C49 | 0.0276 (17) | 0.0303 (18) | 0.0330 (18) | 0.0050 (14) | 0.0094 (14) | 0.0118 (15) |
C50 | 0.037 (2) | 0.040 (2) | 0.049 (2) | 0.0098 (17) | 0.0109 (17) | 0.0009 (18) |
C51 | 0.036 (2) | 0.058 (3) | 0.072 (3) | 0.020 (2) | 0.017 (2) | 0.003 (2) |
C52 | 0.028 (2) | 0.060 (3) | 0.063 (3) | 0.0065 (19) | 0.0043 (19) | 0.014 (2) |
C53 | 0.036 (2) | 0.054 (3) | 0.055 (3) | −0.0024 (19) | 0.0011 (19) | −0.003 (2) |
C54 | 0.035 (2) | 0.040 (2) | 0.050 (2) | 0.0075 (17) | 0.0108 (18) | −0.0026 (18) |
C55 | 0.0316 (18) | 0.0329 (18) | 0.0262 (17) | 0.0031 (15) | 0.0022 (14) | 0.0054 (14) |
C56 | 0.041 (2) | 0.0331 (19) | 0.0303 (19) | 0.0030 (16) | 0.0059 (16) | 0.0017 (15) |
C57 | 0.039 (2) | 0.055 (2) | 0.0271 (19) | 0.0027 (18) | 0.0085 (16) | 0.0033 (17) |
C58 | 0.064 (3) | 0.052 (3) | 0.039 (2) | 0.000 (2) | 0.011 (2) | 0.019 (2) |
C59 | 0.091 (3) | 0.032 (2) | 0.053 (3) | 0.013 (2) | 0.023 (2) | 0.014 (2) |
C60 | 0.068 (3) | 0.034 (2) | 0.036 (2) | 0.0145 (19) | 0.0176 (19) | 0.0042 (17) |
C61 | 0.0365 (19) | 0.0304 (18) | 0.0254 (17) | 0.0048 (15) | 0.0058 (14) | 0.0027 (14) |
C62 | 0.039 (2) | 0.036 (2) | 0.051 (2) | 0.0036 (17) | 0.0019 (18) | −0.0041 (18) |
C63 | 0.054 (3) | 0.029 (2) | 0.062 (3) | 0.0008 (18) | 0.009 (2) | −0.0019 (19) |
C64 | 0.060 (3) | 0.033 (2) | 0.059 (3) | 0.016 (2) | 0.020 (2) | 0.0131 (19) |
C65 | 0.040 (2) | 0.042 (2) | 0.074 (3) | 0.0132 (19) | 0.008 (2) | 0.014 (2) |
C66 | 0.039 (2) | 0.031 (2) | 0.055 (2) | 0.0017 (17) | −0.0015 (18) | 0.0054 (18) |
C67 | 0.0313 (18) | 0.0325 (18) | 0.0282 (18) | 0.0037 (15) | 0.0047 (14) | −0.0018 (14) |
C68 | 0.041 (2) | 0.049 (2) | 0.037 (2) | 0.0074 (18) | 0.0076 (17) | 0.0027 (18) |
C69 | 0.037 (2) | 0.070 (3) | 0.042 (2) | 0.013 (2) | −0.0038 (18) | −0.004 (2) |
C70 | 0.029 (2) | 0.056 (3) | 0.060 (3) | 0.0050 (19) | 0.010 (2) | −0.013 (2) |
C71 | 0.043 (2) | 0.048 (2) | 0.053 (3) | −0.0013 (19) | 0.019 (2) | −0.002 (2) |
C72 | 0.039 (2) | 0.045 (2) | 0.037 (2) | 0.0059 (18) | 0.0095 (17) | 0.0042 (17) |
C73 | 0.088 (3) | 0.039 (2) | 0.044 (2) | 0.005 (2) | 0.011 (2) | 0.0101 (19) |
C74 | 0.067 (3) | 0.067 (3) | 0.044 (2) | −0.001 (2) | 0.011 (2) | 0.028 (2) |
C75 | 0.050 (3) | 0.055 (3) | 0.039 (2) | −0.001 (2) | 0.010 (2) | 0.010 (2) |
C76 | 0.072 (4) | 0.065 (3) | 0.052 (3) | 0.001 (3) | −0.004 (3) | 0.015 (3) |
C77 | 0.062 (3) | 0.058 (3) | 0.039 (2) | 0.004 (2) | 0.006 (2) | 0.000 (2) |
C78 | 0.056 (3) | 0.080 (4) | 0.048 (3) | 0.019 (3) | 0.004 (2) | −0.001 (3) |
C79 | 0.037 (2) | 0.056 (3) | 0.066 (3) | 0.005 (2) | 0.011 (2) | 0.004 (2) |
C80 | 0.060 (3) | 0.066 (3) | 0.069 (3) | 0.005 (3) | 0.012 (3) | −0.033 (3) |
Sn—C73 | 2.081 (4) | C28—H28 | 0.9400 |
Sn—C74 | 2.065 (4) | C29—C30 | 1.386 (5) |
Sn—O1 | 2.291 (3) | C29—H29 | 0.9400 |
Sn—O2i | 2.818 (3) | C30—H30 | 0.9400 |
Sn—O3 | 2.155 (3) | C31—C32 | 1.376 (5) |
Sn—O5 | 2.082 (3) | C31—C36 | 1.388 (5) |
Ag—P1 | 2.6167 (9) | C32—C33 | 1.387 (5) |
Ag—P2 | 2.6204 (9) | C32—H32 | 0.9400 |
Ag—P3 | 2.6363 (9) | C33—C34 | 1.362 (6) |
Ag—P4 | 2.6373 (9) | C33—H33 | 0.9400 |
P1—C7 | 1.818 (3) | C34—C35 | 1.376 (6) |
P1—C13 | 1.820 (3) | C34—H34 | 0.9400 |
P1—C1 | 1.826 (3) | C35—C36 | 1.381 (5) |
P2—C19 | 1.807 (3) | C35—H35 | 0.9400 |
P2—C31 | 1.818 (3) | C36—H36 | 0.9400 |
P2—C25 | 1.824 (3) | C37—C38 | 1.378 (5) |
P3—C49 | 1.817 (3) | C37—C42 | 1.379 (5) |
P3—C37 | 1.825 (3) | C38—C39 | 1.378 (5) |
P3—C43 | 1.828 (3) | C38—H38 | 0.9400 |
P4—C61 | 1.825 (3) | C39—C40 | 1.355 (6) |
P4—C55 | 1.825 (3) | C39—H39 | 0.9400 |
P4—C67 | 1.826 (3) | C40—C41 | 1.374 (6) |
F1—C76 | 1.304 (7) | C40—H40 | 0.9400 |
F2—C76 | 1.304 (7) | C41—C42 | 1.372 (5) |
F3—C76 | 1.332 (8) | C41—H41 | 0.9400 |
F1'—C76 | 1.326 (7) | C42—H42 | 0.9400 |
F2'—C76 | 1.312 (7) | C43—C44 | 1.373 (5) |
F3'—C76 | 1.317 (7) | C43—C48 | 1.384 (4) |
F4—C78 | 1.291 (5) | C44—C45 | 1.381 (5) |
F5—C78 | 1.309 (5) | C44—H44 | 0.9400 |
F6—C78 | 1.312 (5) | C45—C46 | 1.366 (5) |
F7—C80 | 1.321 (6) | C45—H45 | 0.9400 |
F8—C80 | 1.243 (6) | C46—C47 | 1.372 (6) |
F9—C80 | 1.243 (5) | C46—H46 | 0.9400 |
O1—C75 | 1.244 (5) | C47—C48 | 1.382 (5) |
O2—C75 | 1.234 (5) | C47—H47 | 0.9400 |
O3—C77 | 1.249 (5) | C48—H48 | 0.9400 |
O4—C77 | 1.220 (5) | C49—C54 | 1.373 (5) |
O5—C79 | 1.245 (5) | C49—C50 | 1.381 (5) |
O6—C79 | 1.210 (5) | C50—C51 | 1.383 (5) |
C1—C2 | 1.379 (5) | C50—H50 | 0.9400 |
C1—C6 | 1.387 (5) | C51—C52 | 1.369 (6) |
C2—C3 | 1.377 (5) | C51—H51 | 0.9400 |
C2—H2 | 0.9400 | C52—C53 | 1.354 (5) |
C3—C4 | 1.388 (6) | C52—H52 | 0.9400 |
C3—H3 | 0.9400 | C53—C54 | 1.377 (5) |
C4—C5 | 1.354 (6) | C53—H53 | 0.9400 |
C4—H4 | 0.9400 | C54—H54 | 0.9400 |
C5—C6 | 1.379 (5) | C55—C60 | 1.374 (5) |
C5—H5 | 0.9400 | C55—C56 | 1.386 (5) |
C6—H6 | 0.9400 | C56—C57 | 1.377 (5) |
C7—C8 | 1.377 (5) | C56—H56 | 0.9400 |
C7—C12 | 1.379 (5) | C57—C58 | 1.355 (5) |
C8—C9 | 1.381 (5) | C57—H57 | 0.9400 |
C8—H8 | 0.9400 | C58—C59 | 1.383 (5) |
C9—C10 | 1.370 (6) | C58—H58 | 0.9400 |
C9—H9 | 0.9400 | C59—C60 | 1.373 (5) |
C10—C11 | 1.364 (6) | C59—H59 | 0.9400 |
C10—H10 | 0.9400 | C60—H60 | 0.9400 |
C11—C12 | 1.375 (5) | C61—C62 | 1.377 (5) |
C11—H11 | 0.9400 | C61—C66 | 1.385 (5) |
C12—H12 | 0.9400 | C62—C63 | 1.385 (5) |
C13—C18 | 1.371 (5) | C62—H62 | 0.9400 |
C13—C14 | 1.384 (5) | C63—C64 | 1.364 (6) |
C14—C15 | 1.379 (5) | C63—H63 | 0.9400 |
C14—H14 | 0.9400 | C64—C65 | 1.363 (6) |
C15—C16 | 1.366 (6) | C64—H64 | 0.9400 |
C15—H15 | 0.9400 | C65—C66 | 1.385 (5) |
C16—C17 | 1.364 (6) | C65—H65 | 0.9400 |
C16—H16 | 0.9400 | C66—H66 | 0.9400 |
C17—C18 | 1.377 (5) | C67—C68 | 1.385 (5) |
C17—H17 | 0.9400 | C67—C72 | 1.391 (5) |
C18—H18 | 0.9400 | C68—C69 | 1.382 (5) |
C19—C20 | 1.387 (5) | C68—H68 | 0.9400 |
C19—C24 | 1.391 (5) | C69—C70 | 1.371 (6) |
C20—C21 | 1.374 (5) | C69—H69 | 0.9400 |
C20—H20 | 0.9400 | C70—C71 | 1.360 (6) |
C21—C22 | 1.364 (6) | C70—H70 | 0.9400 |
C21—H21 | 0.9400 | C71—C72 | 1.374 (5) |
C22—C23 | 1.373 (6) | C71—H71 | 0.9400 |
C22—H22 | 0.9400 | C72—H72 | 0.9400 |
C23—C24 | 1.376 (5) | C73—H73a | 0.9700 |
C23—H23 | 0.9400 | C73—H73b | 0.9700 |
C24—H24 | 0.9400 | C73—H73c | 0.9700 |
C25—C30 | 1.382 (5) | C74—H74a | 0.9700 |
C25—C26 | 1.386 (5) | C74—H74b | 0.9700 |
C26—C27 | 1.369 (5) | C74—H74c | 0.9700 |
C26—H26 | 0.9400 | C75—C76 | 1.527 (6) |
C27—C28 | 1.364 (6) | C77—C78 | 1.533 (6) |
C27—H27 | 0.9400 | C79—C80 | 1.536 (6) |
C28—C29 | 1.377 (6) | ||
C73—Sn—C74 | 154.6 (2) | C31—C36—H36 | 119.9 |
C73—Sn—O1 | 92.9 (2) | C38—C37—C42 | 118.7 (3) |
C73—Sn—O2i | 77.3 (1) | C38—C37—P3 | 123.4 (3) |
C73—Sn—O3 | 99.5 (2) | C42—C37—P3 | 117.8 (3) |
C73—Sn—O5 | 95.5 (1) | C39—C38—C37 | 120.2 (4) |
C74—Sn—O1 | 86.2 (1) | C39—C38—H38 | 119.9 |
C74—Sn—O2i | 79.9 (2) | C37—C38—H38 | 119.9 |
C74—Sn—O3 | 86.9 (1) | C40—C39—C38 | 120.5 (4) |
C74—Sn—O5 | 109.2 (2) | C40—C39—H39 | 119.8 |
O1—Sn—O2i | 114.0 (1) | C38—C39—H39 | 119.8 |
O1—Sn—O3 | 164.2 (1) | C39—C40—C41 | 120.0 (4) |
O1—Sn—O5 | 79.7 (1) | C39—C40—H40 | 120.0 |
O2i—Sn—O3 | 78.7 (1) | C41—C40—H40 | 120.0 |
O2i—Sn—O5 | 164.6 (1) | C42—C41—C40 | 119.9 (4) |
O3—Sn—O5 | 89.3 (1) | C42—C41—H41 | 120.1 |
P1—Ag—P2 | 108.16 (3) | C40—C41—H41 | 120.1 |
P1—Ag—P3 | 111.35 (3) | C41—C42—C37 | 120.6 (4) |
P1—Ag—P4 | 109.45 (3) | C41—C42—H42 | 119.7 |
P2—Ag—P3 | 107.36 (3) | C37—C42—H42 | 119.7 |
P2—Ag—P4 | 109.94 (3) | C44—C43—C48 | 118.6 (3) |
P3—Ag—P4 | 110.51 (3) | C44—C43—P3 | 118.3 (3) |
C7—P1—C13 | 102.48 (15) | C48—C43—P3 | 123.1 (3) |
C7—P1—C1 | 103.44 (15) | C43—C44—C45 | 121.2 (3) |
C13—P1—C1 | 101.84 (15) | C43—C44—H44 | 119.4 |
C7—P1—Ag | 113.19 (11) | C45—C44—H44 | 119.4 |
C13—P1—Ag | 117.39 (11) | C46—C45—C44 | 119.8 (4) |
C1—P1—Ag | 116.52 (11) | C46—C45—H45 | 120.1 |
C19—P2—C31 | 102.57 (15) | C44—C45—H45 | 120.1 |
C19—P2—C25 | 104.58 (15) | C45—C46—C47 | 119.9 (4) |
C31—P2—C25 | 102.41 (16) | C45—C46—H46 | 120.1 |
C19—P2—Ag | 113.11 (10) | C47—C46—H46 | 120.1 |
C31—P2—Ag | 117.91 (11) | C46—C47—C48 | 120.4 (4) |
C25—P2—Ag | 114.59 (10) | C46—C47—H47 | 119.8 |
C49—P3—C37 | 102.65 (15) | C48—C47—H47 | 119.8 |
C49—P3—C43 | 103.67 (15) | C47—C48—C43 | 120.1 (4) |
C37—P3—C43 | 102.48 (15) | C47—C48—H48 | 119.9 |
C49—P3—Ag | 113.79 (11) | C43—C48—H48 | 119.9 |
C37—P3—Ag | 117.34 (11) | C54—C49—C50 | 118.0 (3) |
C43—P3—Ag | 115.09 (11) | C54—C49—P3 | 118.1 (3) |
C61—P4—C55 | 101.87 (15) | C50—C49—P3 | 123.7 (3) |
C61—P4—C67 | 102.37 (15) | C51—C50—C49 | 120.0 (4) |
C55—P4—C67 | 103.14 (15) | C51—C50—H50 | 120.0 |
C61—P4—Ag | 117.20 (11) | C49—C50—H50 | 120.0 |
C55—P4—Ag | 113.99 (11) | C52—C51—C50 | 120.7 (4) |
C67—P4—Ag | 116.21 (11) | C52—C51—H51 | 119.6 |
C75—O1—Sn | 112.0 (3) | C50—C51—H51 | 119.6 |
C77—O3—Sn | 127.0 (3) | C53—C52—C51 | 119.8 (4) |
C79—O5—Sn | 125.5 (3) | C53—C52—H52 | 120.1 |
C2—C1—C6 | 118.8 (3) | C51—C52—H52 | 120.1 |
C2—C1—P1 | 118.4 (3) | C52—C53—C54 | 119.8 (4) |
C6—C1—P1 | 122.7 (3) | C52—C53—H53 | 120.1 |
C3—C2—C1 | 121.2 (4) | C54—C53—H53 | 120.1 |
C3—C2—H2 | 119.4 | C49—C54—C53 | 121.8 (3) |
C1—C2—H2 | 119.4 | C49—C54—H54 | 119.1 |
C2—C3—C4 | 119.2 (4) | C53—C54—H54 | 119.1 |
C2—C3—H3 | 120.4 | C60—C55—C56 | 118.3 (3) |
C4—C3—H3 | 120.4 | C60—C55—P4 | 118.6 (3) |
C5—C4—C3 | 119.9 (4) | C56—C55—P4 | 123.1 (3) |
C5—C4—H4 | 120.0 | C57—C56—C55 | 120.3 (3) |
C3—C4—H4 | 120.0 | C57—C56—H56 | 119.8 |
C4—C5—C6 | 121.2 (4) | C55—C56—H56 | 119.8 |
C4—C5—H5 | 119.4 | C58—C57—C56 | 121.0 (4) |
C6—C5—H5 | 119.4 | C58—C57—H57 | 119.5 |
C5—C6—C1 | 119.7 (4) | C56—C57—H57 | 119.5 |
C5—C6—H6 | 120.1 | C57—C58—C59 | 119.2 (4) |
C1—C6—H6 | 120.1 | C57—C58—H58 | 120.4 |
C8—C7—C12 | 119.1 (3) | C59—C58—H58 | 120.4 |
C8—C7—P1 | 117.5 (3) | C60—C59—C58 | 120.1 (4) |
C12—C7—P1 | 123.4 (3) | C60—C59—H59 | 120.0 |
C7—C8—C9 | 120.5 (4) | C58—C59—H59 | 120.0 |
C7—C8—H8 | 119.7 | C59—C60—C55 | 121.1 (4) |
C9—C8—H8 | 119.7 | C59—C60—H60 | 119.5 |
C10—C9—C8 | 119.9 (4) | C55—C60—H60 | 119.5 |
C10—C9—H9 | 120.1 | C62—C61—C66 | 118.2 (3) |
C8—C9—H9 | 120.1 | C62—C61—P4 | 124.3 (3) |
C11—C10—C9 | 119.7 (4) | C66—C61—P4 | 117.4 (3) |
C11—C10—H10 | 120.1 | C61—C62—C63 | 120.6 (4) |
C9—C10—H10 | 120.1 | C61—C62—H62 | 119.7 |
C10—C11—C12 | 120.9 (4) | C63—C62—H62 | 119.7 |
C10—C11—H11 | 119.5 | C64—C63—C62 | 120.5 (4) |
C12—C11—H11 | 119.5 | C64—C63—H63 | 119.8 |
C11—C12—C7 | 119.9 (4) | C62—C63—H63 | 119.8 |
C11—C12—H12 | 120.1 | C65—C64—C63 | 119.8 (4) |
C7—C12—H12 | 120.1 | C65—C64—H64 | 120.1 |
C18—C13—C14 | 118.1 (3) | C63—C64—H64 | 120.1 |
C18—C13—P1 | 118.8 (3) | C64—C65—C66 | 120.2 (4) |
C14—C13—P1 | 123.1 (3) | C64—C65—H65 | 119.9 |
C15—C14—C13 | 120.6 (3) | C66—C65—H65 | 119.9 |
C15—C14—H14 | 119.7 | C65—C66—C61 | 120.7 (4) |
C13—C14—H14 | 119.7 | C65—C66—H66 | 119.6 |
C16—C15—C14 | 120.5 (4) | C61—C66—H66 | 119.6 |
C16—C15—H15 | 119.7 | C68—C67—C72 | 118.2 (3) |
C14—C15—H15 | 119.7 | C68—C67—P4 | 123.2 (3) |
C15—C16—C17 | 119.1 (4) | C72—C67—P4 | 118.6 (3) |
C15—C16—H16 | 120.4 | C69—C68—C67 | 120.3 (4) |
C17—C16—H16 | 120.4 | C69—C68—H68 | 119.8 |
C16—C17—C18 | 120.7 (4) | C67—C68—H68 | 119.8 |
C16—C17—H17 | 119.6 | C70—C69—C68 | 120.3 (4) |
C18—C17—H17 | 119.6 | C70—C69—H69 | 119.8 |
C13—C18—C17 | 120.8 (4) | C68—C69—H69 | 119.8 |
C13—C18—H18 | 119.6 | C71—C70—C69 | 119.9 (4) |
C17—C18—H18 | 119.6 | C71—C70—H70 | 120.0 |
C20—C19—C24 | 118.3 (3) | C69—C70—H70 | 120.0 |
C20—C19—P2 | 118.4 (3) | C70—C71—C72 | 120.4 (4) |
C24—C19—P2 | 123.0 (3) | C70—C71—H71 | 119.8 |
C21—C20—C19 | 120.0 (4) | C72—C71—H71 | 119.8 |
C21—C20—H20 | 120.0 | C71—C72—C67 | 120.7 (4) |
C19—C20—H20 | 120.0 | C71—C72—H72 | 119.6 |
C22—C21—C20 | 121.2 (4) | C67—C72—H72 | 119.6 |
C22—C21—H21 | 119.4 | Sn—C73—H73a | 109.5 |
C20—C21—H21 | 119.4 | Sn—C73—H73b | 109.5 |
C21—C22—C23 | 119.6 (4) | H73a—C73—H73b | 109.5 |
C21—C22—H22 | 120.2 | Sn—C73—H73c | 109.5 |
C23—C22—H22 | 120.2 | H73a—C73—H73c | 109.5 |
C22—C23—C24 | 120.0 (4) | H73b—C73—H73c | 109.5 |
C22—C23—H23 | 120.0 | Sn—C74—H74a | 109.5 |
C24—C23—H23 | 120.0 | Sn—C74—H74b | 109.5 |
C23—C24—C19 | 120.8 (4) | H74a—C74—H74b | 109.5 |
C23—C24—H24 | 119.6 | Sn—C74—H74c | 109.5 |
C19—C24—H24 | 119.6 | H74a—C74—H74c | 109.5 |
C30—C25—C26 | 119.1 (3) | H74b—C74—H74c | 109.5 |
C30—C25—P2 | 123.8 (3) | O2—C75—O1 | 126.3 (4) |
C26—C25—P2 | 117.0 (3) | O2—C75—C76 | 119.1 (4) |
C27—C26—C25 | 120.3 (4) | O1—C75—C76 | 114.6 (4) |
C27—C26—H26 | 119.8 | F1—C76—F2 | 109.4 (7) |
C25—C26—H26 | 119.8 | F2—C76—F3' | 130.6 (8) |
C28—C27—C26 | 120.3 (4) | F2'—C76—F3' | 107.1 (7) |
C28—C27—H27 | 119.9 | F2'—C76—F1' | 105.9 (6) |
C26—C27—H27 | 119.9 | F3'—C76—F1' | 107.9 (7) |
C27—C28—C29 | 120.7 (4) | F1—C76—F3 | 107.7 (7) |
C27—C28—H28 | 119.7 | F2—C76—F3 | 106.7 (7) |
C29—C28—H28 | 119.7 | F1—C76—C75 | 113.8 (7) |
C28—C29—C30 | 119.2 (4) | F2—C76—C75 | 108.0 (7) |
C28—C29—H29 | 120.4 | F2'—C76—C75 | 112.4 (5) |
C30—C29—H29 | 120.4 | F3'—C76—C75 | 112.4 (6) |
C25—C30—C29 | 120.4 (4) | F1'—C76—C75 | 110.7 (6) |
C25—C30—H30 | 119.8 | F3—C76—C75 | 111.0 (6) |
C29—C30—H30 | 119.8 | O4—C77—O3 | 128.4 (4) |
C32—C31—C36 | 119.2 (3) | O4—C77—C78 | 118.5 (4) |
C32—C31—P2 | 122.9 (3) | O3—C77—C78 | 113.1 (4) |
C36—C31—P2 | 117.8 (3) | F4—C78—F6 | 107.5 (4) |
C31—C32—C33 | 120.2 (4) | F4—C78—F5 | 109.0 (5) |
C31—C32—H32 | 119.9 | F6—C78—F5 | 104.2 (4) |
C33—C32—H32 | 119.9 | F4—C78—C77 | 114.7 (4) |
C34—C33—C32 | 120.1 (4) | F6—C78—C77 | 111.4 (4) |
C34—C33—H33 | 119.9 | F5—C78—C77 | 109.5 (4) |
C32—C33—H33 | 119.9 | O6—C79—O5 | 129.6 (5) |
C33—C34—C35 | 120.5 (4) | O6—C79—C80 | 118.9 (4) |
C33—C34—H34 | 119.8 | O5—C79—C80 | 111.5 (4) |
C35—C34—H34 | 119.8 | F9—C80—F8 | 112.5 (6) |
C34—C35—C36 | 119.7 (4) | F9—C80—F7 | 103.9 (5) |
C34—C35—H35 | 120.1 | F8—C80—F7 | 103.0 (5) |
C36—C35—H35 | 120.1 | F9—C80—C79 | 114.5 (4) |
C35—C36—C31 | 120.2 (4) | F8—C80—C79 | 113.7 (4) |
C35—C36—H36 | 119.9 | F7—C80—C79 | 108.0 (5) |
P2—Ag—P1—C7 | −176.63 (12) | C25—P2—C31—C36 | −169.7 (3) |
P3—Ag—P1—C7 | −58.88 (12) | Ag—P2—C31—C36 | −42.9 (3) |
P4—Ag—P1—C7 | 63.60 (12) | C36—C31—C32—C33 | 0.7 (5) |
P2—Ag—P1—C13 | −57.51 (13) | P2—C31—C32—C33 | 177.9 (3) |
P3—Ag—P1—C13 | 60.24 (13) | C31—C32—C33—C34 | −1.0 (6) |
P4—Ag—P1—C13 | −177.28 (12) | C32—C33—C34—C35 | 0.4 (7) |
P2—Ag—P1—C1 | 63.61 (12) | C33—C34—C35—C36 | 0.5 (6) |
P3—Ag—P1—C1 | −178.65 (12) | C34—C35—C36—C31 | −0.8 (6) |
P4—Ag—P1—C1 | −56.16 (12) | C32—C31—C36—C35 | 0.1 (5) |
P1—Ag—P2—C19 | −129.71 (12) | P2—C31—C36—C35 | −177.2 (3) |
P3—Ag—P2—C19 | 110.02 (12) | C49—P3—C37—C38 | 7.0 (3) |
P4—Ag—P2—C19 | −10.24 (12) | C43—P3—C37—C38 | 114.3 (3) |
P1—Ag—P2—C31 | −10.11 (13) | Ag—P3—C37—C38 | −118.6 (3) |
P3—Ag—P2—C31 | −130.38 (13) | C49—P3—C37—C42 | −175.6 (3) |
P4—Ag—P2—C31 | 109.35 (13) | C43—P3—C37—C42 | −68.3 (3) |
P1—Ag—P2—C25 | 110.55 (13) | Ag—P3—C37—C42 | 58.9 (3) |
P3—Ag—P2—C25 | −9.73 (13) | C42—C37—C38—C39 | 1.3 (6) |
P4—Ag—P2—C25 | −129.99 (13) | P3—C37—C38—C39 | 178.7 (3) |
P1—Ag—P3—C49 | 65.73 (12) | C37—C38—C39—C40 | −0.8 (6) |
P2—Ag—P3—C49 | −176.05 (12) | C38—C39—C40—C41 | 0.8 (7) |
P4—Ag—P3—C49 | −56.14 (12) | C39—C40—C41—C42 | −1.5 (6) |
P1—Ag—P3—C37 | −174.44 (13) | C40—C41—C42—C37 | 2.0 (6) |
P2—Ag—P3—C37 | −56.22 (13) | C38—C37—C42—C41 | −1.9 (6) |
P4—Ag—P3—C37 | 63.69 (13) | P3—C37—C42—C41 | −179.5 (3) |
P1—Ag—P3—C43 | −53.72 (12) | C49—P3—C43—C44 | −96.2 (3) |
P2—Ag—P3—C43 | 64.50 (12) | C37—P3—C43—C44 | 157.3 (3) |
P4—Ag—P3—C43 | −175.60 (11) | Ag—P3—C43—C44 | 28.7 (3) |
P1—Ag—P4—C61 | 63.22 (13) | C49—P3—C43—C48 | 83.3 (3) |
P2—Ag—P4—C61 | −55.45 (13) | C37—P3—C43—C48 | −23.3 (3) |
P3—Ag—P4—C61 | −173.79 (13) | Ag—P3—C43—C48 | −151.8 (3) |
P1—Ag—P4—C55 | −177.97 (12) | C48—C43—C44—C45 | 1.9 (5) |
P2—Ag—P4—C55 | 63.35 (12) | P3—C43—C44—C45 | −178.6 (3) |
P3—Ag—P4—C55 | −54.99 (12) | C43—C44—C45—C46 | −1.6 (6) |
P1—Ag—P4—C67 | −58.21 (13) | C44—C45—C46—C47 | 0.5 (6) |
P2—Ag—P4—C67 | −176.89 (13) | C45—C46—C47—C48 | 0.3 (6) |
P3—Ag—P4—C67 | 64.77 (13) | C46—C47—C48—C43 | 0.0 (6) |
C74—Sn—O1—C75 | −75.3 (3) | C44—C43—C48—C47 | −1.1 (5) |
O5—Sn—O1—C75 | 174.4 (3) | P3—C43—C48—C47 | 179.5 (3) |
C73—Sn—O1—C75 | 79.3 (3) | C37—P3—C49—C54 | −92.2 (3) |
O3—Sn—O1—C75 | −139.5 (4) | C43—P3—C49—C54 | 161.4 (3) |
O2i—Sn—O1—C75 | 1.9 (3) | Ag—P3—C49—C54 | 35.6 (3) |
C74—Sn—O3—C77 | −161.2 (4) | C37—P3—C49—C50 | 84.1 (3) |
O5—Sn—O3—C77 | −51.9 (4) | C43—P3—C49—C50 | −22.3 (3) |
C73—Sn—O3—C77 | 43.5 (4) | Ag—P3—C49—C50 | −148.0 (3) |
O1—Sn—O3—C77 | −97.1 (5) | C54—C49—C50—C51 | −1.3 (6) |
O2i—Sn—O3—C77 | 118.5 (4) | P3—C49—C50—C51 | −177.7 (3) |
C74—Sn—O5—C79 | 35.5 (4) | C49—C50—C51—C52 | 1.3 (6) |
C73—Sn—O5—C79 | −150.3 (4) | C50—C51—C52—C53 | −0.2 (7) |
O3—Sn—O5—C79 | −50.9 (3) | C51—C52—C53—C54 | −0.9 (7) |
O1—Sn—O5—C79 | 117.8 (3) | C50—C49—C54—C53 | 0.3 (6) |
O2i—Sn—O5—C79 | −88.9 (5) | P3—C49—C54—C53 | 176.9 (3) |
C7—P1—C1—C2 | −85.9 (3) | C52—C53—C54—C49 | 0.8 (6) |
C13—P1—C1—C2 | 168.0 (3) | C61—P4—C55—C60 | 164.2 (3) |
Ag—P1—C1—C2 | 39.0 (3) | C67—P4—C55—C60 | −89.9 (3) |
C7—P1—C1—C6 | 94.8 (3) | Ag—P4—C55—C60 | 37.0 (3) |
C13—P1—C1—C6 | −11.3 (3) | C61—P4—C55—C56 | −16.3 (3) |
Ag—P1—C1—C6 | −140.4 (3) | C67—P4—C55—C56 | 89.5 (3) |
C6—C1—C2—C3 | −0.4 (5) | Ag—P4—C55—C56 | −143.6 (3) |
P1—C1—C2—C3 | −179.8 (3) | C60—C55—C56—C57 | −0.5 (5) |
C1—C2—C3—C4 | 1.2 (6) | P4—C55—C56—C57 | −179.9 (3) |
C2—C3—C4—C5 | −1.5 (6) | C55—C56—C57—C58 | 0.5 (6) |
C3—C4—C5—C6 | 1.0 (6) | C56—C57—C58—C59 | 0.0 (6) |
C4—C5—C6—C1 | −0.2 (6) | C57—C58—C59—C60 | −0.6 (7) |
C2—C1—C6—C5 | −0.1 (5) | C58—C59—C60—C55 | 0.7 (7) |
P1—C1—C6—C5 | 179.3 (3) | C56—C55—C60—C59 | −0.1 (6) |
C13—P1—C7—C8 | −85.2 (3) | P4—C55—C60—C59 | 179.3 (3) |
C1—P1—C7—C8 | 169.2 (3) | C55—P4—C61—C62 | 103.3 (3) |
Ag—P1—C7—C8 | 42.2 (3) | C67—P4—C61—C62 | −3.2 (4) |
C13—P1—C7—C12 | 92.8 (3) | Ag—P4—C61—C62 | −131.6 (3) |
C1—P1—C7—C12 | −12.8 (3) | C55—P4—C61—C66 | −73.2 (3) |
Ag—P1—C7—C12 | −139.8 (3) | C67—P4—C61—C66 | −179.7 (3) |
C12—C7—C8—C9 | 0.4 (6) | Ag—P4—C61—C66 | 51.9 (3) |
P1—C7—C8—C9 | 178.5 (3) | C66—C61—C62—C63 | 0.1 (6) |
C7—C8—C9—C10 | 0.3 (6) | P4—C61—C62—C63 | −176.4 (3) |
C8—C9—C10—C11 | −0.7 (7) | C61—C62—C63—C64 | 1.2 (6) |
C9—C10—C11—C12 | 0.3 (7) | C62—C63—C64—C65 | −2.0 (7) |
C10—C11—C12—C7 | 0.4 (7) | C63—C64—C65—C66 | 1.5 (7) |
C8—C7—C12—C11 | −0.7 (6) | C64—C65—C66—C61 | −0.2 (6) |
P1—C7—C12—C11 | −178.7 (3) | C62—C61—C66—C65 | −0.6 (6) |
C7—P1—C13—C18 | 176.0 (3) | P4—C61—C66—C65 | 176.1 (3) |
C1—P1—C13—C18 | −77.1 (3) | C61—P4—C67—C68 | 101.9 (3) |
Ag—P1—C13—C18 | 51.3 (3) | C55—P4—C67—C68 | −3.6 (3) |
C7—P1—C13—C14 | −4.1 (3) | Ag—P4—C67—C68 | −129.1 (3) |
C1—P1—C13—C14 | 102.7 (3) | C61—P4—C67—C72 | −76.8 (3) |
Ag—P1—C13—C14 | −128.8 (3) | C55—P4—C67—C72 | 177.7 (3) |
C18—C13—C14—C15 | −0.1 (5) | Ag—P4—C67—C72 | 52.2 (3) |
P1—C13—C14—C15 | −179.9 (3) | C72—C67—C68—C69 | 0.7 (5) |
C13—C14—C15—C16 | 0.1 (6) | P4—C67—C68—C69 | −178.0 (3) |
C14—C15—C16—C17 | 0.5 (7) | C67—C68—C69—C70 | 1.1 (6) |
C15—C16—C17—C18 | −1.1 (7) | C68—C69—C70—C71 | −2.2 (6) |
C14—C13—C18—C17 | −0.5 (6) | C69—C70—C71—C72 | 1.5 (6) |
P1—C13—C18—C17 | 179.3 (3) | C70—C71—C72—C67 | 0.3 (6) |
C16—C17—C18—C13 | 1.2 (7) | C68—C67—C72—C71 | −1.4 (5) |
C31—P2—C19—C20 | −178.9 (3) | P4—C67—C72—C71 | 177.4 (3) |
C25—P2—C19—C20 | 74.5 (3) | Sn—O1—C75—O2 | −16.6 (5) |
Ag—P2—C19—C20 | −50.9 (3) | Sn—O1—C75—C76 | 162.7 (3) |
C31—P2—C19—C24 | −4.7 (3) | O2—C75—C76—F1 | −21.3 (9) |
C25—P2—C19—C24 | −111.3 (3) | O1—C75—C76—F1 | 159.3 (7) |
Ag—P2—C19—C24 | 123.3 (3) | O2—C75—C76—F2 | 100.4 (7) |
C24—C19—C20—C21 | −0.3 (5) | O1—C75—C76—F2 | −79.0 (7) |
P2—C19—C20—C21 | 174.2 (3) | O2—C75—C76—F2' | 130.5 (7) |
C19—C20—C21—C22 | −0.6 (6) | O1—C75—C76—F2' | −48.8 (7) |
C20—C21—C22—C23 | 0.6 (6) | O2—C75—C76—F3' | −108.6 (7) |
C21—C22—C23—C24 | 0.2 (6) | O1—C75—C76—F3' | 72.1 (8) |
C22—C23—C24—C19 | −1.0 (6) | O2—C75—C76—F1' | 12.2 (8) |
C20—C19—C24—C23 | 1.0 (5) | O1—C75—C76—F1' | −167.1 (7) |
P2—C19—C24—C23 | −173.2 (3) | O2—C75—C76—F3 | −142.9 (7) |
C19—P2—C25—C30 | −1.7 (3) | O1—C75—C76—F3 | 37.7 (7) |
C31—P2—C25—C30 | −108.4 (3) | Sn—O3—C77—O4 | −2.5 (7) |
Ag—P2—C25—C30 | 122.7 (3) | Sn—O3—C77—C78 | 175.9 (3) |
C19—P2—C25—C26 | −178.8 (3) | O4—C77—C78—F4 | −158.2 (5) |
C31—P2—C25—C26 | 74.5 (3) | O3—C77—C78—F4 | 23.1 (6) |
Ag—P2—C25—C26 | −54.4 (3) | O4—C77—C78—F6 | −35.8 (6) |
C30—C25—C26—C27 | −0.9 (5) | O3—C77—C78—F6 | 145.6 (4) |
P2—C25—C26—C27 | 176.4 (3) | O4—C77—C78—F5 | 78.9 (6) |
C25—C26—C27—C28 | −0.6 (6) | O3—C77—C78—F5 | −99.7 (5) |
C26—C27—C28—C29 | 1.6 (7) | Sn—O5—C79—O6 | −15.6 (7) |
C27—C28—C29—C30 | −0.9 (7) | Sn—O5—C79—C80 | 165.3 (3) |
C26—C25—C30—C29 | 1.5 (6) | O6—C79—C80—F9 | −134.1 (6) |
P2—C25—C30—C29 | −175.6 (3) | O5—C79—C80—F9 | 45.0 (7) |
C28—C29—C30—C25 | −0.6 (7) | O6—C79—C80—F8 | 94.6 (7) |
C19—P2—C31—C32 | −95.2 (3) | O5—C79—C80—F8 | −86.2 (6) |
C25—P2—C31—C32 | 13.0 (3) | O6—C79—C80—F7 | −19.0 (7) |
Ag—P2—C31—C32 | 139.8 (3) | O5—C79—C80—F7 | 160.1 (4) |
C19—P2—C31—C36 | 82.0 (3) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Ag(C18H15P)4]2[Sn2(CH3)4(C2F3O2)6] |
Mr | 3289.54 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 223 |
a, b, c (Å) | 12.9439 (6), 14.0499 (6), 20.7267 (9) |
α, β, γ (°) | 100.370 (1), 99.429 (1), 95.899 (1) |
V (Å3) | 3623.6 (3) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.78 |
Crystal size (mm) | 0.31 × 0.25 × 0.20 |
Data collection | |
Diffractometer | Bruker APEX area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.672, 0.837 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 31408, 16043, 11658 |
Rint | 0.031 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.048, 0.113, 0.92 |
No. of reflections | 16043 |
No. of parameters | 939 |
No. of restraints | 15 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.39, −0.83 |
Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.
Sn—C73 | 2.081 (4) | Sn—O2i | 2.818 (3) |
Sn—C74 | 2.065 (4) | Sn—O3 | 2.155 (3) |
Sn—O1 | 2.291 (3) | Sn—O5 | 2.082 (3) |
C73—Sn—C74 | 154.6 (2) | C74—Sn—O5 | 109.2 (2) |
C73—Sn—O1 | 92.9 (2) | O1—Sn—O2i | 114.0 (1) |
C73—Sn—O2i | 77.3 (1) | O1—Sn—O3 | 164.2 (1) |
C73—Sn—O3 | 99.5 (2) | O1—Sn—O5 | 79.7 (1) |
C73—Sn—O5 | 95.5 (1) | O2i—Sn—O3 | 78.7 (1) |
C74—Sn—O1 | 86.2 (1) | O2i—Sn—O5 | 164.6 (1) |
C74—Sn—O2i | 79.9 (2) | O3—Sn—O5 | 89.3 (1) |
C74—Sn—O3 | 86.9 (1) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Tetrakis(triphenylphosphine)silver(I) bis(trifluoroacetato)triphenylstannate (Ng & Rae, 2003) illustrates the use of an extremely bulky metal-bearing counter-ion to stabilize the di(carboxylato)triorganostannate anion. Such an anion, which was first synthesized in expectation of enhanced aqueous solubility owing to the ionic nature of the complex, was documented as the tetramethylammonium bis(trifluoroacetato)triphenylstannate salt (Ng & Kumar Das, 1997); other ammonium stannates have also been characterized (Ng, 1998; Ng & Hook, 1999). The trifluoroacetato group is a strong electron-withdrawing group that can bind to a neutral triorganotin fluoroacetate molecule; the nature of the organic radical is probably not important as a bis(trifluoroacetato)tricyclohexylstannate is also known (Ng, 1999). In these stannates, the carboxylate anion behaves as a unidentate group that bonds covalently to the Sn atom, but the Sn—O bond is weaker than the covalent Sn—O bonds found in the neutral triorganotin carboxylates (Ng et al., 1988). Apart from the trifluoroacetate anion, a limited number of carboxylate anions also display this property of affording organostannates (Ng & Kumar Das, 1999). In contrast, the related bis(oxalato)diorganostannate dianion does not require special assistance, as stability is conferred by the chelating nature of the dicarboxylate group (Xu et al., 2003). The investigations on the di(carboxylato)triorganostannates are now extended to the analogous tri(carboxylato)diorganostannates.
The structural chemistry of organotin carboxylates (Tiekink, 1991; Tiekink, 1994; Holloway & Melnik, 2000) has only one example of a stannate, tetramethylammonium triacetatodimethylstannate, which crystallizes as an air-sensitive chloroform solvate (Lockhart et al., 1987). The sole example contrasts with the numerous examples of the neutral diorganotin dicarboxylates, which, with the possible exceptions of dimethyltin diformate (Mistry et al., 1990) and dimethyltin bis(trifluoroacetate) (Mistry et al., 1995), exist as monomeric molecules in having the chelated Sn atom in a skew-trapezoidal enviroment.
Tetraammonium triacetatodimethylstannate possesses two chelating acetate groups [2.291 (1) and 2.525 (3) Å, and 2.271 (8) and 2.520 (9) Å]; the third acetate group is unidentate [2.113 (9) Å], the double-bonded carbonyl O atom being about 3.5 Å from the Sn atom (Lockhart et al., 1987). In the trifluoroacetate analog, the negative charge of the stannate group is balanced by the positive charge of the tetrakis(triphenylphosphine)silver cation. The three carboxylate groups of the stannate ion are unidentate, but the carbonyl O atom of one of them widens the (CH3)2Sn skeleton [C—Sn—C = 154.6 (2)°] across a center of inversion, so that the Sn atoms in the dianoinic entity are formally six-coordinate in a distorted-octahedral geometry (Fig. 1). The dianion features an eight-membered → Sn–O–C═O→ Sn–O–C═O→ ring, but the carboxylate bridge [Sn←O 2.818 (3) Å] is weak and is much longer than those [Sn←O = 2.619 (4) and 2.700 (4) Å] found in the six-coordinate polymeric parent Lewis acid (Mistry et al., 1995). Such a ring has only been documented previously in tetranuclear (OH)2(Cl3CCO2)6[Sn(C6H5)2]4, for which the covalent and dative Sn—O bonds [2.185 (6) and 2.361 (7) Å] are similar to one another (Alcock & Roe, 1989). There are no significant interactions between the cation and anion in the unit cell. The ability of two trifluoroacetatodimethylstannate ions to aggregate into a dianion can be attributed to enhanced Lewis acidity brought about by the electron-withdrawing trifluoroacetate group. Evidence of enhanced Lewis acidity of diorganotin bis(fluoroacetates) comes from the isolation of stable complexes with α,α'-diminine ligands (Garner et al., 1975; Ng et al., 1999). The trifluoroacetato group is probably comparable in its electron-withdrawing ability with, for example, the chloride ion; several trichlorodimethylstannates that are doubly chlorine-bridged into dianions are known (Lanfranchi et al., 1986; Matsubayashi et al., 1985; Teoh et al., 1992).