Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803009668/na6228sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803009668/na6228Isup2.hkl |
CCDC reference: 214773
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.019 Å
- R factor = 0.080
- wR factor = 0.210
- Data-to-parameter ratio = 17.5
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_420 Alert C D-H Without Acceptor S1 - H6A ? PLAT_420 Alert C D-H Without Acceptor S2 - H6B ? PLAT_731 Alert C Bond Calc 1.726(19), Rep 1.726(5) .... 3.80 su-Ratio C4 -CL02 1.555 1.555 PLAT_731 Alert C Bond Calc 1.72(2), Rep 1.720(5) .... 4.00 su-Ratio C5 -CL03 1.555 1.555 PLAT_731 Alert C Bond Calc 1.72(2), Rep 1.721(5) .... 4.00 su-Ratio C5 -CL04 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
5 Alert Level C = Please check
The title compound was isolated by the reaction between [Ag2(µ2-dppm)2(MeCN)4](SbF6)2 (Diez et al., 1987) and [Pd(phen)(tdt)] (Scott & Richard, 1996) in an equimolar ratio in dichloromethane under anaerobic condition for 12 h. Well shaped pale yellow crystals suitable for X-ray diffraction study were grown by slow diffusion of diethyl ether into a dichloromethane solution at room temperature.
All H atoms were included in calculated positions, with C—H distances of 0.93 (sp2) and 0.97 Å (sp3), and H–S distances of 1.20 Å. They were included in the refinement in riding motion approximation with Uiso = 1.2Ueq (1.5Ueq for sp3) of the carrier atom.
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994); data reduction: XPREP (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. A view of (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. |
[Ag3(C25H22P2)3(HS)2]SbF6·2CH2Cl2 | F(000) = 3880 |
Mr = 1948.45 | Dx = 1.597 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 8192 reflections |
a = 16.0813 (1) Å | θ = 1.3–25.0° |
b = 18.0049 (2) Å | µ = 1.40 mm−1 |
c = 28.1089 (3) Å | T = 293 K |
β = 95.417 (1)° | Prism, pale yellow |
V = 8102.36 (13) Å3 | 0.72 × 0.60 × 0.46 mm |
Z = 4 |
Siemens SMART CCD diffractometer | 14088 independent reflections |
Radiation source: fine-focus sealed tube | 10084 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
ω scans | θmax = 25.0°, θmin = 1.3° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −10→19 |
Tmin = 0.354, Tmax = 0.525 | k = −13→21 |
25151 measured reflections | l = −33→32 |
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)] = 0.080 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.210 | H-atom parameters constrained |
S = 1.21 | w = 1/[σ2(Fo2) + (0.0537P)2 + 77.3298P] where P = (Fo2 + 2Fc2)/3 |
14088 reflections | (Δ/σ)max = 0.006 |
807 parameters | Δρmax = 1.50 e Å−3 |
4 restraints | Δρmin = −1.23 e Å−3 |
[Ag3(C25H22P2)3(HS)2]SbF6·2CH2Cl2 | V = 8102.36 (13) Å3 |
Mr = 1948.45 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 16.0813 (1) Å | µ = 1.40 mm−1 |
b = 18.0049 (2) Å | T = 293 K |
c = 28.1089 (3) Å | 0.72 × 0.60 × 0.46 mm |
β = 95.417 (1)° |
Siemens SMART CCD diffractometer | 14088 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 10084 reflections with I > 2σ(I) |
Tmin = 0.354, Tmax = 0.525 | Rint = 0.047 |
25151 measured reflections |
R[F2 > 2σ(F2)] = 0.080 | 4 restraints |
wR(F2) = 0.210 | H-atom parameters constrained |
S = 1.21 | w = 1/[σ2(Fo2) + (0.0537P)2 + 77.3298P] where P = (Fo2 + 2Fc2)/3 |
14088 reflections | Δρmax = 1.50 e Å−3 |
807 parameters | Δρmin = −1.23 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Sb | 0.43562 (5) | 0.77857 (6) | 0.55439 (3) | 0.0669 (3) | |
Ag1 | 0.85356 (5) | 0.82543 (5) | 0.75823 (3) | 0.0451 (2) | |
Ag2 | 0.95905 (5) | 0.82429 (5) | 0.66155 (3) | 0.0502 (2) | |
Ag3 | 1.06476 (5) | 0.78051 (5) | 0.77001 (3) | 0.0504 (2) | |
S1 | 0.93674 (15) | 0.70518 (14) | 0.72450 (9) | 0.0439 (6) | |
H6A | 0.9205 | 0.6405 | 0.7192 | 0.053* | |
S2 | 0.98644 (16) | 0.91081 (14) | 0.73817 (9) | 0.0459 (6) | |
H6B | 1.0032 | 0.9754 | 0.7436 | 0.055* | |
P1 | 0.86185 (14) | 0.82298 (15) | 0.84624 (8) | 0.0375 (5) | |
P2 | 0.72572 (15) | 0.81252 (14) | 0.70314 (8) | 0.0378 (5) | |
P3 | 0.82164 (16) | 0.83775 (16) | 0.61517 (9) | 0.0431 (6) | |
P4 | 1.09318 (15) | 0.80107 (15) | 0.62814 (9) | 0.0399 (6) | |
P5 | 1.19248 (15) | 0.77796 (15) | 0.72685 (9) | 0.0395 (6) | |
P6 | 1.04429 (15) | 0.75885 (15) | 0.85566 (9) | 0.0398 (6) | |
C1 | 0.9362 (5) | 0.7533 (6) | 0.8724 (3) | 0.041 (2) | |
H1A | 0.9144 | 0.7045 | 0.8636 | 0.050* | |
H1B | 0.9382 | 0.7572 | 0.9070 | 0.050* | |
C2 | 0.7399 (6) | 0.7836 (5) | 0.6414 (3) | 0.039 (2) | |
H2A | 0.7547 | 0.7314 | 0.6413 | 0.047* | |
H2B | 0.6875 | 0.7896 | 0.6217 | 0.047* | |
C3 | 1.1890 (6) | 0.8241 (6) | 0.6673 (3) | 0.043 (2) | |
H3A | 1.1918 | 0.8775 | 0.6718 | 0.051* | |
H3B | 1.2375 | 0.8091 | 0.6516 | 0.051* | |
C4 | 1.0629 (19) | 1.0853 (8) | 0.6681 (7) | 0.234 (15)* | |
H4A | 1.0891 | 1.0634 | 0.6972 | 0.281* | |
H4B | 1.0042 | 1.0926 | 0.6723 | 0.281* | |
C5 | 1.1936 (11) | 0.5080 (14) | 0.4072 (7) | 0.190 (11)* | |
H5A | 1.2415 | 0.4844 | 0.4245 | 0.228* | |
H5B | 1.2126 | 0.5542 | 0.3942 | 0.228* | |
C111 | 0.8910 (6) | 0.9090 (6) | 0.8772 (4) | 0.048 (2) | |
C112 | 0.8949 (8) | 0.9738 (7) | 0.8509 (4) | 0.064 (3) | |
H11B | 0.8838 | 0.9723 | 0.8179 | 0.077* | |
C113 | 0.9155 (10) | 1.0416 (8) | 0.8735 (6) | 0.090 (5) | |
H11E | 0.9192 | 1.0846 | 0.8555 | 0.108* | |
C114 | 0.9304 (10) | 1.0443 (9) | 0.9230 (6) | 0.091 (5) | |
H11D | 0.9441 | 1.0891 | 0.9382 | 0.109* | |
C115 | 0.9250 (9) | 0.9810 (8) | 0.9491 (5) | 0.075 (4) | |
H11C | 0.9337 | 0.9829 | 0.9823 | 0.091* | |
C116 | 0.9065 (7) | 0.9141 (7) | 0.9268 (4) | 0.062 (3) | |
H11A | 0.9044 | 0.8713 | 0.9452 | 0.075* | |
C121 | 0.7649 (6) | 0.7946 (6) | 0.8712 (4) | 0.045 (2) | |
C122 | 0.7619 (7) | 0.7718 (7) | 0.9189 (4) | 0.060 (3) | |
H12A | 0.8107 | 0.7701 | 0.9395 | 0.072* | |
C123 | 0.6869 (7) | 0.7519 (8) | 0.9353 (5) | 0.074 (4) | |
H12D | 0.6857 | 0.7364 | 0.9668 | 0.088* | |
C124 | 0.6142 (8) | 0.7547 (9) | 0.9060 (5) | 0.081 (4) | |
H12E | 0.5640 | 0.7413 | 0.9175 | 0.097* | |
C125 | 0.6157 (7) | 0.7773 (8) | 0.8597 (5) | 0.073 (4) | |
H12C | 0.5663 | 0.7793 | 0.8397 | 0.088* | |
C126 | 0.6903 (6) | 0.7973 (7) | 0.8425 (4) | 0.058 (3) | |
H12B | 0.6902 | 0.8129 | 0.8110 | 0.069* | |
C211 | 0.6545 (6) | 0.8904 (5) | 0.6991 (3) | 0.040 (2) | |
C212 | 0.6682 (7) | 0.9479 (7) | 0.7316 (4) | 0.061 (3) | |
H21B | 0.7141 | 0.9453 | 0.7543 | 0.073* | |
C213 | 0.6155 (9) | 1.0098 (7) | 0.7314 (6) | 0.080 (4) | |
H21D | 0.6260 | 1.0476 | 0.7537 | 0.096* | |
C214 | 0.5482 (10) | 1.0133 (8) | 0.6978 (6) | 0.085 (5) | |
H21C | 0.5136 | 1.0548 | 0.6967 | 0.102* | |
C215 | 0.5312 (9) | 0.9569 (9) | 0.6659 (5) | 0.085 (4) | |
H21E | 0.4835 | 0.9586 | 0.6445 | 0.102* | |
C216 | 0.5856 (7) | 0.8971 (7) | 0.6658 (4) | 0.066 (3) | |
H21A | 0.5755 | 0.8603 | 0.6427 | 0.079* | |
C221 | 0.6650 (6) | 0.7331 (5) | 0.7222 (3) | 0.038 (2) | |
C222 | 0.7083 (7) | 0.6687 (6) | 0.7358 (4) | 0.054 (3) | |
H22B | 0.7660 | 0.6667 | 0.7351 | 0.065* | |
C223 | 0.6661 (9) | 0.6082 (7) | 0.7503 (5) | 0.077 (4) | |
H22D | 0.6958 | 0.5653 | 0.7594 | 0.092* | |
C224 | 0.5822 (8) | 0.6091 (8) | 0.7518 (5) | 0.073 (4)* | |
H22E | 0.5549 | 0.5667 | 0.7611 | 0.088* | |
C225 | 0.5375 (8) | 0.6714 (8) | 0.7399 (6) | 0.084 (4) | |
H22C | 0.4802 | 0.6725 | 0.7420 | 0.100* | |
C226 | 0.5793 (7) | 0.7342 (7) | 0.7242 (5) | 0.066 (3) | |
H22A | 0.5491 | 0.7767 | 0.7152 | 0.079* | |
C311 | 0.8260 (7) | 0.7952 (7) | 0.5559 (4) | 0.056 (3) | |
C312 | 0.8098 (8) | 0.8336 (9) | 0.5136 (4) | 0.078 (4) | |
H31B | 0.7885 | 0.8816 | 0.5133 | 0.093* | |
C313 | 0.8268 (10) | 0.7972 (14) | 0.4695 (4) | 0.120 (8) | |
H31D | 0.8151 | 0.8213 | 0.4404 | 0.144* | |
C314 | 0.8590 (14) | 0.7298 (13) | 0.4710 (9) | 0.127 (7)* | |
H31F | 0.8723 | 0.7083 | 0.4426 | 0.153* | |
C315 | 0.8737 (11) | 0.6903 (11) | 0.5123 (7) | 0.111 (6)* | |
H31E | 0.8941 | 0.6421 | 0.5120 | 0.133* | |
C316 | 0.8570 (9) | 0.7246 (8) | 0.5552 (5) | 0.076 (4) | |
H31A | 0.8674 | 0.6987 | 0.5838 | 0.091* | |
C321 | 0.7754 (7) | 0.9291 (6) | 0.6047 (4) | 0.054 (3) | |
C322 | 0.8136 (9) | 0.9905 (7) | 0.6266 (5) | 0.072 (4) | |
H32B | 0.8640 | 0.9850 | 0.6454 | 0.086* | |
C323 | 0.7768 (12) | 1.0617 (8) | 0.6207 (6) | 0.093 (5) | |
H32D | 0.8020 | 1.1029 | 0.6359 | 0.112* | |
C324 | 0.7040 (11) | 1.0688 (11) | 0.5923 (6) | 0.100 (5)* | |
H32E | 0.6806 | 1.1158 | 0.5880 | 0.120* | |
C325 | 0.6638 (9) | 1.0102 (9) | 0.5701 (5) | 0.088 (5) | |
H32A | 0.6143 | 1.0172 | 0.5507 | 0.106* | |
C326 | 0.6983 (8) | 0.9389 (8) | 0.5769 (5) | 0.074 (4) | |
H32C | 0.6703 | 0.8979 | 0.5631 | 0.089* | |
C411 | 1.1048 (6) | 0.8548 (6) | 0.5741 (3) | 0.045 (2) | |
C412 | 1.0348 (8) | 0.8602 (9) | 0.5416 (5) | 0.082 (4) | |
H41C | 0.9857 | 0.8366 | 0.5482 | 0.098* | |
C413 | 1.0365 (10) | 0.9000 (9) | 0.4995 (6) | 0.088 (4)* | |
H41E | 0.9890 | 0.9031 | 0.4780 | 0.106* | |
C414 | 1.1080 (10) | 0.9346 (9) | 0.4900 (5) | 0.088 (4) | |
H41A | 1.1089 | 0.9624 | 0.4622 | 0.105* | |
C415 | 1.1766 (10) | 0.9291 (9) | 0.5198 (5) | 0.095 (5) | |
H41D | 1.2256 | 0.9520 | 0.5124 | 0.114* | |
C416 | 1.1752 (8) | 0.8891 (8) | 0.5621 (4) | 0.073 (4) | |
H41B | 1.2237 | 0.8858 | 0.5828 | 0.088* | |
C421 | 1.1129 (6) | 0.7062 (5) | 0.6093 (4) | 0.042 (2) | |
C422 | 1.0635 (8) | 0.6485 (7) | 0.6228 (5) | 0.065 (3) | |
H42B | 1.0196 | 0.6586 | 0.6410 | 0.077* | |
C423 | 1.0779 (10) | 0.5767 (8) | 0.6097 (6) | 0.089 (4) | |
H42D | 1.0433 | 0.5390 | 0.6188 | 0.106* | |
C424 | 1.1425 (10) | 0.5599 (8) | 0.5834 (5) | 0.082 (4) | |
H42E | 1.1528 | 0.5110 | 0.5751 | 0.098* | |
C425 | 1.1919 (9) | 0.6160 (8) | 0.5693 (6) | 0.086 (4) | |
H42C | 1.2359 | 0.6048 | 0.5513 | 0.103* | |
C426 | 1.1777 (8) | 0.6894 (7) | 0.5814 (5) | 0.065 (3) | |
H42A | 1.2111 | 0.7271 | 0.5710 | 0.078* | |
C511 | 1.2820 (6) | 0.8242 (6) | 0.7601 (4) | 0.046 (2) | |
C512 | 1.3536 (7) | 0.8471 (6) | 0.7396 (4) | 0.060 (3) | |
H51C | 1.3567 | 0.8415 | 0.7070 | 0.072* | |
C513 | 1.4206 (7) | 0.8783 (7) | 0.7681 (6) | 0.075 (4) | |
H51B | 1.4691 | 0.8922 | 0.7548 | 0.090* | |
C514 | 1.4140 (9) | 0.8883 (7) | 0.8159 (5) | 0.077 (4) | |
H51D | 1.4584 | 0.9093 | 0.8349 | 0.093* | |
C515 | 1.3443 (9) | 0.8684 (8) | 0.8361 (5) | 0.076 (4)* | |
H51E | 1.3406 | 0.8760 | 0.8685 | 0.092* | |
C516 | 1.2786 (7) | 0.8367 (6) | 0.8080 (4) | 0.056 (3) | |
H51A | 1.2307 | 0.8234 | 0.8220 | 0.067* | |
C521 | 1.2316 (6) | 0.6843 (6) | 0.7174 (4) | 0.046 (2) | |
C522 | 1.1877 (9) | 0.6255 (7) | 0.7346 (5) | 0.071 (4) | |
H52B | 1.1375 | 0.6340 | 0.7476 | 0.086* | |
C523 | 1.2197 (11) | 0.5525 (10) | 0.7322 (6) | 0.100 (5)* | |
H52E | 1.1908 | 0.5131 | 0.7444 | 0.120* | |
C524 | 1.2906 (10) | 0.5395 (10) | 0.7128 (6) | 0.089 (4)* | |
H52D | 1.3112 | 0.4912 | 0.7121 | 0.107* | |
C525 | 1.3336 (9) | 0.5960 (9) | 0.6938 (6) | 0.087 (5) | |
H52C | 1.3818 | 0.5860 | 0.6790 | 0.105* | |
C526 | 1.3042 (7) | 0.6698 (7) | 0.6967 (5) | 0.070 (3) | |
H52A | 1.3340 | 0.7087 | 0.6846 | 0.083* | |
C611 | 1.0875 (6) | 0.6706 (6) | 0.8791 (4) | 0.049 (3) | |
C612 | 1.1532 (8) | 0.6397 (7) | 0.8590 (5) | 0.073 (4) | |
H61A | 1.1757 | 0.6644 | 0.8341 | 0.088* | |
C613 | 1.1876 (11) | 0.5723 (10) | 0.8747 (6) | 0.103 (5)* | |
H61E | 1.2330 | 0.5526 | 0.8609 | 0.123* | |
C614 | 1.1540 (9) | 0.5353 (8) | 0.9105 (6) | 0.089 (5) | |
H61C | 1.1762 | 0.4896 | 0.9207 | 0.107* | |
C615 | 1.0884 (9) | 0.5642 (8) | 0.9317 (5) | 0.082 (4) | |
H61D | 1.0656 | 0.5383 | 0.9560 | 0.099* | |
C616 | 1.0560 (8) | 0.6323 (7) | 0.9169 (5) | 0.067 (3) | |
H61B | 1.0128 | 0.6530 | 0.9322 | 0.081* | |
C621 | 1.0957 (6) | 0.8292 (6) | 0.8955 (3) | 0.042 (2) | |
C622 | 1.1073 (7) | 0.9003 (6) | 0.8784 (4) | 0.056 (3) | |
H62A | 1.0889 | 0.9118 | 0.8469 | 0.068* | |
C623 | 1.1455 (9) | 0.9537 (8) | 0.9074 (5) | 0.084 (4) | |
H62C | 1.1529 | 1.0010 | 0.8953 | 0.101* | |
C624 | 1.1728 (9) | 0.9386 (9) | 0.9535 (5) | 0.077 (4)* | |
H62E | 1.1989 | 0.9753 | 0.9728 | 0.093* | |
C625 | 1.1621 (8) | 0.8702 (9) | 0.9713 (5) | 0.083 (4) | |
H62D | 1.1811 | 0.8604 | 1.0029 | 0.099* | |
C626 | 1.1227 (7) | 0.8133 (7) | 0.9432 (4) | 0.061 (3) | |
H62B | 1.1149 | 0.7664 | 0.9559 | 0.074* | |
F1 | 0.3936 (11) | 0.6861 (8) | 0.5616 (7) | 0.222 (8) | |
Cl01 | 1.0705 (4) | 1.0238 (4) | 0.6219 (2) | 0.151 (2)* | |
F2 | 0.4760 (12) | 0.8702 (7) | 0.5496 (6) | 0.208 (7) | |
Cl02 | 1.1079 (3) | 1.1709 (3) | 0.6601 (2) | 0.1267 (16)* | |
F3 | 0.4648 (8) | 0.7500 (9) | 0.4966 (4) | 0.188 (7) | |
Cl03 | 1.1216 (8) | 0.5280 (8) | 0.4468 (5) | 0.291 (6)* | |
F4 | 0.5366 (8) | 0.7528 (10) | 0.5827 (6) | 0.218 (8) | |
Cl04 | 1.1579 (7) | 0.4512 (7) | 0.3603 (4) | 0.260 (5)* | |
F5 | 0.3993 (9) | 0.8078 (10) | 0.6122 (4) | 0.195 (7) | |
F6 | 0.3304 (10) | 0.8001 (9) | 0.5284 (6) | 0.198 (6)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sb | 0.0529 (5) | 0.0906 (7) | 0.0572 (5) | −0.0049 (4) | 0.0043 (4) | −0.0166 (4) |
Ag1 | 0.0387 (4) | 0.0583 (5) | 0.0375 (4) | 0.0006 (4) | −0.0017 (3) | −0.0018 (4) |
Ag2 | 0.0355 (4) | 0.0709 (6) | 0.0443 (4) | 0.0015 (4) | 0.0038 (3) | −0.0004 (4) |
Ag3 | 0.0385 (4) | 0.0690 (6) | 0.0440 (4) | 0.0018 (4) | 0.0051 (3) | 0.0046 (4) |
S1 | 0.0389 (13) | 0.0388 (13) | 0.0541 (15) | −0.0026 (11) | 0.0048 (11) | −0.0023 (11) |
S2 | 0.0483 (14) | 0.0392 (14) | 0.0503 (15) | −0.0030 (11) | 0.0051 (11) | −0.0032 (11) |
P1 | 0.0333 (12) | 0.0438 (14) | 0.0351 (12) | 0.0032 (11) | 0.0012 (10) | 0.0017 (11) |
P2 | 0.0354 (12) | 0.0414 (14) | 0.0357 (12) | −0.0013 (11) | −0.0016 (10) | 0.0015 (10) |
P3 | 0.0369 (13) | 0.0532 (16) | 0.0387 (13) | −0.0013 (12) | 0.0009 (10) | 0.0007 (12) |
P4 | 0.0333 (12) | 0.0500 (16) | 0.0372 (13) | −0.0007 (11) | 0.0067 (10) | 0.0017 (11) |
P5 | 0.0318 (12) | 0.0466 (15) | 0.0398 (13) | −0.0001 (11) | 0.0023 (10) | 0.0009 (11) |
P6 | 0.0324 (12) | 0.0495 (15) | 0.0373 (13) | 0.0030 (11) | 0.0022 (10) | 0.0024 (11) |
C1 | 0.032 (5) | 0.052 (6) | 0.039 (5) | 0.005 (4) | 0.000 (4) | −0.001 (4) |
C2 | 0.036 (5) | 0.041 (5) | 0.041 (5) | −0.008 (4) | 0.005 (4) | −0.002 (4) |
C3 | 0.039 (5) | 0.047 (6) | 0.044 (5) | −0.004 (5) | 0.010 (4) | 0.004 (5) |
C111 | 0.040 (5) | 0.058 (7) | 0.045 (6) | 0.003 (5) | 0.000 (4) | −0.005 (5) |
C112 | 0.079 (8) | 0.059 (8) | 0.053 (7) | −0.013 (6) | 0.001 (6) | 0.001 (6) |
C113 | 0.118 (13) | 0.055 (9) | 0.097 (12) | −0.014 (8) | 0.014 (10) | −0.003 (8) |
C114 | 0.098 (11) | 0.078 (11) | 0.097 (12) | −0.013 (9) | 0.007 (9) | −0.041 (9) |
C115 | 0.089 (10) | 0.080 (10) | 0.056 (8) | −0.007 (8) | 0.000 (7) | −0.028 (7) |
C116 | 0.069 (8) | 0.066 (8) | 0.050 (7) | −0.003 (6) | −0.008 (6) | 0.002 (6) |
C121 | 0.046 (6) | 0.043 (6) | 0.047 (6) | −0.002 (5) | 0.008 (4) | −0.004 (5) |
C122 | 0.047 (6) | 0.086 (9) | 0.048 (6) | 0.003 (6) | 0.003 (5) | 0.013 (6) |
C123 | 0.053 (7) | 0.105 (11) | 0.065 (8) | −0.005 (7) | 0.012 (6) | 0.014 (7) |
C124 | 0.044 (7) | 0.117 (12) | 0.084 (10) | −0.012 (7) | 0.030 (7) | 0.010 (9) |
C125 | 0.033 (6) | 0.112 (11) | 0.075 (9) | 0.003 (6) | 0.003 (5) | 0.006 (8) |
C126 | 0.031 (5) | 0.086 (9) | 0.055 (6) | 0.002 (5) | 0.001 (5) | 0.001 (6) |
C211 | 0.035 (5) | 0.046 (6) | 0.039 (5) | 0.004 (4) | 0.004 (4) | −0.001 (4) |
C212 | 0.049 (6) | 0.060 (7) | 0.073 (8) | −0.002 (6) | 0.002 (6) | −0.003 (6) |
C213 | 0.084 (10) | 0.049 (8) | 0.110 (12) | 0.010 (7) | 0.022 (9) | −0.025 (7) |
C214 | 0.080 (10) | 0.063 (9) | 0.115 (13) | 0.028 (8) | 0.029 (9) | 0.030 (9) |
C215 | 0.076 (9) | 0.097 (12) | 0.080 (10) | 0.042 (9) | −0.004 (7) | 0.016 (9) |
C216 | 0.061 (7) | 0.079 (9) | 0.057 (7) | 0.024 (7) | −0.006 (6) | 0.000 (6) |
C221 | 0.038 (5) | 0.035 (5) | 0.041 (5) | −0.002 (4) | 0.001 (4) | −0.009 (4) |
C222 | 0.043 (6) | 0.057 (7) | 0.064 (7) | 0.002 (5) | 0.011 (5) | 0.003 (6) |
C223 | 0.077 (9) | 0.051 (7) | 0.108 (11) | 0.003 (7) | 0.035 (8) | 0.012 (7) |
C225 | 0.052 (7) | 0.081 (10) | 0.120 (12) | −0.021 (7) | 0.016 (8) | 0.004 (9) |
C226 | 0.054 (7) | 0.062 (8) | 0.081 (9) | 0.001 (6) | 0.006 (6) | 0.001 (7) |
C311 | 0.044 (6) | 0.075 (8) | 0.049 (6) | −0.007 (6) | 0.006 (5) | −0.001 (6) |
C312 | 0.080 (9) | 0.111 (11) | 0.040 (6) | −0.009 (8) | −0.002 (6) | 0.009 (7) |
C313 | 0.096 (12) | 0.23 (2) | 0.029 (7) | −0.038 (14) | 0.003 (7) | 0.021 (10) |
C316 | 0.094 (10) | 0.076 (9) | 0.059 (8) | 0.001 (8) | 0.019 (7) | −0.021 (7) |
C321 | 0.054 (6) | 0.057 (7) | 0.052 (6) | −0.010 (5) | 0.011 (5) | 0.006 (5) |
C322 | 0.089 (10) | 0.064 (9) | 0.064 (8) | −0.012 (7) | 0.015 (7) | 0.009 (6) |
C323 | 0.150 (15) | 0.045 (8) | 0.089 (11) | −0.025 (9) | 0.037 (10) | 0.000 (7) |
C325 | 0.062 (8) | 0.113 (13) | 0.090 (10) | 0.027 (9) | 0.014 (7) | 0.042 (9) |
C326 | 0.063 (8) | 0.076 (9) | 0.082 (9) | 0.006 (7) | 0.001 (7) | 0.017 (7) |
C411 | 0.047 (6) | 0.045 (6) | 0.043 (5) | −0.002 (5) | 0.009 (4) | 0.007 (5) |
C412 | 0.067 (8) | 0.114 (12) | 0.062 (8) | −0.005 (8) | −0.002 (6) | 0.041 (8) |
C414 | 0.102 (11) | 0.094 (11) | 0.066 (9) | 0.002 (9) | 0.000 (8) | 0.033 (8) |
C415 | 0.097 (11) | 0.121 (13) | 0.067 (9) | −0.040 (10) | 0.005 (8) | 0.040 (9) |
C416 | 0.068 (8) | 0.093 (10) | 0.058 (7) | −0.025 (7) | 0.002 (6) | 0.025 (7) |
C421 | 0.030 (5) | 0.043 (6) | 0.051 (6) | 0.007 (4) | −0.002 (4) | −0.003 (5) |
C422 | 0.065 (8) | 0.049 (7) | 0.082 (9) | −0.003 (6) | 0.017 (6) | −0.004 (6) |
C423 | 0.091 (11) | 0.064 (9) | 0.114 (12) | −0.010 (8) | 0.024 (9) | −0.001 (9) |
C424 | 0.093 (11) | 0.054 (8) | 0.098 (11) | 0.006 (8) | 0.005 (9) | −0.016 (8) |
C425 | 0.066 (8) | 0.075 (10) | 0.122 (13) | 0.002 (8) | 0.028 (8) | −0.019 (9) |
C426 | 0.062 (7) | 0.056 (8) | 0.078 (8) | −0.002 (6) | 0.016 (6) | −0.006 (6) |
C511 | 0.042 (5) | 0.043 (6) | 0.054 (6) | 0.002 (5) | −0.002 (4) | −0.001 (5) |
C512 | 0.056 (7) | 0.061 (7) | 0.064 (7) | −0.009 (6) | 0.014 (6) | −0.006 (6) |
C513 | 0.036 (6) | 0.073 (9) | 0.115 (12) | −0.009 (6) | −0.001 (7) | −0.016 (8) |
C514 | 0.076 (9) | 0.061 (8) | 0.087 (10) | 0.003 (7) | −0.033 (8) | −0.021 (7) |
C516 | 0.056 (7) | 0.058 (7) | 0.053 (7) | −0.008 (5) | −0.003 (5) | −0.002 (5) |
C521 | 0.037 (5) | 0.051 (6) | 0.049 (6) | 0.003 (5) | −0.008 (4) | −0.001 (5) |
C522 | 0.079 (9) | 0.053 (8) | 0.085 (9) | −0.013 (7) | 0.024 (7) | 0.000 (7) |
C525 | 0.067 (9) | 0.093 (11) | 0.102 (11) | 0.020 (8) | 0.004 (8) | −0.030 (9) |
C526 | 0.054 (7) | 0.058 (8) | 0.097 (10) | 0.007 (6) | 0.007 (7) | −0.017 (7) |
C611 | 0.042 (6) | 0.042 (6) | 0.060 (7) | 0.009 (5) | −0.013 (5) | −0.002 (5) |
C612 | 0.057 (7) | 0.069 (8) | 0.094 (10) | 0.025 (7) | 0.004 (7) | 0.010 (7) |
C614 | 0.070 (9) | 0.064 (9) | 0.125 (13) | 0.026 (7) | −0.030 (9) | 0.008 (9) |
C615 | 0.079 (10) | 0.078 (10) | 0.087 (10) | 0.004 (8) | −0.009 (8) | 0.030 (8) |
C616 | 0.059 (7) | 0.071 (8) | 0.073 (8) | 0.019 (6) | 0.010 (6) | 0.019 (7) |
C621 | 0.032 (5) | 0.055 (6) | 0.040 (5) | −0.004 (5) | 0.005 (4) | −0.006 (5) |
C622 | 0.063 (7) | 0.059 (7) | 0.047 (6) | −0.016 (6) | 0.003 (5) | 0.006 (5) |
C623 | 0.095 (11) | 0.063 (9) | 0.096 (11) | −0.030 (8) | 0.016 (9) | 0.001 (8) |
C625 | 0.068 (8) | 0.120 (13) | 0.056 (8) | −0.005 (8) | −0.016 (6) | −0.015 (8) |
C626 | 0.059 (7) | 0.078 (9) | 0.045 (6) | −0.001 (6) | −0.005 (5) | −0.006 (6) |
F1 | 0.230 (17) | 0.152 (13) | 0.29 (2) | −0.089 (12) | 0.057 (15) | −0.010 (13) |
F2 | 0.30 (2) | 0.106 (9) | 0.224 (16) | −0.068 (11) | 0.075 (14) | −0.018 (10) |
F3 | 0.164 (11) | 0.303 (18) | 0.107 (8) | −0.075 (11) | 0.065 (8) | −0.117 (10) |
F4 | 0.123 (10) | 0.263 (17) | 0.245 (17) | 0.069 (11) | −0.096 (10) | −0.113 (14) |
F5 | 0.182 (13) | 0.30 (2) | 0.107 (9) | −0.027 (12) | 0.055 (9) | −0.078 (11) |
Sb—F2 | 1.783 (12) | C224—H22E | 0.9300 |
Sb—F4 | 1.801 (11) | C225—C226 | 1.407 (17) |
Sb—F3 | 1.808 (9) | C225—H22C | 0.9300 |
Sb—F1 | 1.815 (13) | C226—H22A | 0.9300 |
Sb—F6 | 1.820 (17) | C311—C316 | 1.366 (18) |
Sb—F5 | 1.853 (11) | C311—C312 | 1.379 (16) |
Ag1—P2 | 2.465 (2) | C312—C313 | 1.45 (2) |
Ag1—P1 | 2.465 (2) | C312—H31B | 0.9300 |
Ag1—S2 | 2.734 (3) | C313—C314 | 1.32 (3) |
Ag1—S1 | 2.760 (3) | C313—H31D | 0.9300 |
Ag1—Ag2 | 3.3369 (11) | C314—C315 | 1.36 (3) |
Ag2—P4 | 2.468 (2) | C314—H31F | 0.9300 |
Ag2—P3 | 2.469 (3) | C315—C316 | 1.40 (2) |
Ag2—S2 | 2.661 (3) | C315—H31E | 0.9300 |
Ag2—S1 | 2.825 (3) | C316—H31A | 0.9300 |
Ag3—P5 | 2.483 (3) | C321—C322 | 1.380 (17) |
Ag3—P6 | 2.491 (3) | C321—C326 | 1.413 (16) |
Ag3—S1 | 2.686 (3) | C322—C323 | 1.415 (19) |
Ag3—S2 | 2.771 (3) | C322—H32B | 0.9300 |
S1—H6A | 1.2000 | C323—C324 | 1.36 (2) |
S2—H6B | 1.2000 | C323—H32D | 0.9300 |
P1—C111 | 1.816 (11) | C324—C325 | 1.36 (2) |
P1—C1 | 1.838 (9) | C324—H32E | 0.9300 |
P1—C121 | 1.842 (10) | C325—C326 | 1.406 (19) |
P2—C211 | 1.808 (10) | C325—H32A | 0.9300 |
P2—C221 | 1.839 (10) | C326—H32C | 0.9300 |
P2—C2 | 1.847 (9) | C411—C416 | 1.359 (15) |
P3—C321 | 1.818 (12) | C411—C412 | 1.384 (16) |
P3—C311 | 1.842 (12) | C412—C413 | 1.386 (19) |
P3—C2 | 1.845 (9) | C412—H41C | 0.9300 |
P4—C421 | 1.824 (10) | C413—C414 | 1.36 (2) |
P4—C411 | 1.825 (10) | C413—H41E | 0.9300 |
P4—C3 | 1.854 (10) | C414—C415 | 1.32 (2) |
P5—C521 | 1.827 (11) | C414—H41A | 0.9300 |
P5—C511 | 1.840 (10) | C415—C416 | 1.394 (17) |
P5—C3 | 1.865 (9) | C415—H41D | 0.9300 |
P6—C611 | 1.832 (10) | C416—H41B | 0.9300 |
P6—C621 | 1.834 (10) | C421—C422 | 1.383 (15) |
P6—C1 | 1.846 (9) | C421—C426 | 1.395 (15) |
C1—H1A | 0.9700 | C422—C423 | 1.370 (18) |
C1—H1B | 0.9700 | C422—H42B | 0.9300 |
C2—H2A | 0.9700 | C423—C424 | 1.366 (19) |
C2—H2B | 0.9700 | C423—H42D | 0.9300 |
C3—H3A | 0.9700 | C424—C425 | 1.366 (19) |
C3—H3B | 0.9700 | C424—H42E | 0.9300 |
C4—Cl01 | 1.720 (5) | C425—C426 | 1.390 (18) |
C4—Cl02 | 1.726 (5) | C425—H42C | 0.9300 |
C4—H4A | 0.9700 | C426—H42A | 0.9300 |
C4—H4B | 0.9700 | C511—C516 | 1.372 (15) |
C5—Cl03 | 1.720 (5) | C511—C512 | 1.396 (15) |
C5—Cl04 | 1.721 (5) | C512—C513 | 1.400 (16) |
C5—H5A | 0.9700 | C512—H51C | 0.9300 |
C5—H5B | 0.9700 | C513—C514 | 1.369 (19) |
C111—C112 | 1.385 (15) | C513—H51B | 0.9300 |
C111—C116 | 1.395 (15) | C514—C515 | 1.351 (19) |
C112—C113 | 1.400 (18) | C514—H51D | 0.9300 |
C112—H11B | 0.9300 | C515—C516 | 1.380 (17) |
C113—C114 | 1.39 (2) | C515—H51E | 0.9300 |
C113—H11E | 0.9300 | C516—H51A | 0.9300 |
C114—C115 | 1.36 (2) | C521—C526 | 1.378 (16) |
C114—H11D | 0.9300 | C521—C522 | 1.384 (15) |
C115—C116 | 1.377 (17) | C522—C523 | 1.42 (2) |
C115—H11C | 0.9300 | C522—H52B | 0.9300 |
C116—H11A | 0.9300 | C523—C524 | 1.33 (2) |
C121—C126 | 1.381 (14) | C523—H52E | 0.9300 |
C121—C122 | 1.409 (14) | C524—C525 | 1.37 (2) |
C122—C123 | 1.378 (16) | C524—H52D | 0.9300 |
C122—H12A | 0.9300 | C525—C526 | 1.416 (18) |
C123—C124 | 1.365 (18) | C525—H52C | 0.9300 |
C123—H12D | 0.9300 | C526—H52A | 0.9300 |
C124—C125 | 1.366 (18) | C611—C612 | 1.363 (16) |
C124—H12E | 0.9300 | C611—C616 | 1.400 (16) |
C125—C126 | 1.383 (15) | C612—C613 | 1.39 (2) |
C125—H12C | 0.9300 | C612—H61A | 0.9300 |
C126—H12B | 0.9300 | C613—C614 | 1.36 (2) |
C211—C212 | 1.384 (15) | C613—H61E | 0.9300 |
C211—C216 | 1.386 (14) | C614—C615 | 1.36 (2) |
C212—C213 | 1.399 (17) | C614—H61C | 0.9300 |
C212—H21B | 0.9300 | C615—C616 | 1.381 (18) |
C213—C214 | 1.37 (2) | C615—H61D | 0.9300 |
C213—H21D | 0.9300 | C616—H61B | 0.9300 |
C214—C215 | 1.36 (2) | C621—C622 | 1.386 (15) |
C214—H21C | 0.9300 | C621—C626 | 1.399 (14) |
C215—C216 | 1.388 (17) | C622—C623 | 1.369 (17) |
C215—H21E | 0.9300 | C622—H62A | 0.9300 |
C216—H21A | 0.9300 | C623—C624 | 1.356 (19) |
C221—C226 | 1.385 (15) | C623—H62C | 0.9300 |
C221—C222 | 1.389 (14) | C624—C625 | 1.35 (2) |
C222—C223 | 1.365 (16) | C624—H62E | 0.9300 |
C222—H22B | 0.9300 | C625—C626 | 1.408 (17) |
C223—C224 | 1.355 (18) | C625—H62D | 0.9300 |
C223—H22D | 0.9300 | C626—H62B | 0.9300 |
C224—C225 | 1.356 (19) | ||
F2—Sb—F4 | 87.3 (9) | C214—C215—H21E | 120.3 |
F2—Sb—F3 | 93.9 (7) | C216—C215—H21E | 120.3 |
F4—Sb—F3 | 91.4 (7) | C211—C216—C215 | 121.9 (13) |
F2—Sb—F1 | 177.8 (8) | C211—C216—H21A | 119.0 |
F4—Sb—F1 | 92.5 (9) | C215—C216—H21A | 119.0 |
F3—Sb—F1 | 88.3 (8) | C226—C221—C222 | 118.4 (10) |
F2—Sb—F6 | 96.0 (8) | C226—C221—P2 | 124.0 (8) |
F4—Sb—F6 | 176.1 (9) | C222—C221—P2 | 117.6 (7) |
F3—Sb—F6 | 90.6 (7) | C223—C222—C221 | 119.9 (10) |
F1—Sb—F6 | 84.2 (8) | C223—C222—H22B | 120.1 |
F2—Sb—F5 | 87.2 (7) | C221—C222—H22B | 120.1 |
F4—Sb—F5 | 91.8 (7) | C224—C223—C222 | 121.7 (13) |
F3—Sb—F5 | 176.6 (6) | C224—C223—H22D | 119.2 |
F1—Sb—F5 | 90.7 (8) | C222—C223—H22D | 119.2 |
F6—Sb—F5 | 86.1 (7) | C223—C224—C225 | 120.5 (13) |
P2—Ag1—P1 | 126.27 (8) | C223—C224—H22E | 119.7 |
P2—Ag1—S2 | 123.04 (9) | C225—C224—H22E | 119.7 |
P1—Ag1—S2 | 104.35 (8) | C224—C225—C226 | 119.0 (12) |
P2—Ag1—S1 | 96.47 (8) | C224—C225—H22C | 120.5 |
P1—Ag1—S1 | 110.40 (8) | C226—C225—H22C | 120.5 |
S2—Ag1—S1 | 87.51 (8) | C221—C226—C225 | 120.6 (12) |
P2—Ag1—Ag2 | 86.89 (6) | C221—C226—H22A | 119.7 |
P1—Ag1—Ag2 | 146.48 (6) | C225—C226—H22A | 119.7 |
S2—Ag1—Ag2 | 50.81 (6) | C316—C311—C312 | 119.6 (12) |
S1—Ag1—Ag2 | 54.21 (6) | C316—C311—P3 | 116.4 (9) |
P4—Ag2—P3 | 125.91 (9) | C312—C311—P3 | 123.4 (11) |
P4—Ag2—S2 | 108.86 (9) | C311—C312—C313 | 118.4 (15) |
P3—Ag2—S2 | 116.19 (9) | C311—C312—H31B | 120.8 |
P4—Ag2—S1 | 106.08 (8) | C313—C312—H31B | 120.8 |
P3—Ag2—S1 | 104.18 (9) | C314—C313—C312 | 119.5 (17) |
S2—Ag2—S1 | 87.62 (8) | C314—C313—H31D | 120.2 |
P4—Ag2—Ag1 | 147.21 (7) | C312—C313—H31D | 120.2 |
P3—Ag2—Ag1 | 86.04 (6) | C313—C314—C315 | 123 (2) |
S2—Ag2—Ag1 | 52.78 (6) | C313—C314—H31F | 118.5 |
S1—Ag2—Ag1 | 52.42 (5) | C315—C314—H31F | 118.5 |
P5—Ag3—P6 | 131.32 (9) | C314—C315—C316 | 118.1 (19) |
P5—Ag3—S1 | 112.96 (9) | C314—C315—H31E | 120.9 |
P6—Ag3—S1 | 102.47 (9) | C316—C315—H31E | 120.9 |
P5—Ag3—S2 | 103.27 (9) | C311—C316—C315 | 121.3 (15) |
P6—Ag3—S2 | 110.31 (9) | C311—C316—H31A | 119.3 |
S1—Ag3—S2 | 88.23 (8) | C315—C316—H31A | 119.3 |
Ag3—S1—Ag1 | 79.33 (7) | C322—C321—C326 | 118.5 (12) |
Ag3—S1—Ag2 | 77.18 (7) | C322—C321—P3 | 119.6 (9) |
Ag1—S1—Ag2 | 73.38 (7) | C326—C321—P3 | 121.7 (9) |
Ag3—S1—H6A | 134.2 | C321—C322—C323 | 120.5 (14) |
Ag1—S1—H6A | 134.2 | C321—C322—H32B | 119.7 |
Ag2—S1—H6A | 134.2 | C323—C322—H32B | 119.7 |
Ag2—S2—Ag1 | 76.40 (7) | C324—C323—C322 | 118.8 (15) |
Ag2—S2—Ag3 | 78.54 (7) | C324—C323—H32D | 120.6 |
Ag1—S2—Ag3 | 78.33 (7) | C322—C323—H32D | 120.6 |
Ag2—S2—H6B | 133.5 | C325—C324—C323 | 122.9 (17) |
Ag1—S2—H6B | 133.5 | C325—C324—H32E | 118.5 |
Ag3—S2—H6B | 133.5 | C323—C324—H32E | 118.5 |
C111—P1—C1 | 105.1 (5) | C324—C325—C326 | 118.8 (15) |
C111—P1—C121 | 104.1 (5) | C324—C325—H32A | 120.6 |
C1—P1—C121 | 101.6 (5) | C326—C325—H32A | 120.6 |
C111—P1—Ag1 | 116.9 (4) | C325—C326—C321 | 120.2 (14) |
C1—P1—Ag1 | 112.7 (3) | C325—C326—H32C | 119.9 |
C121—P1—Ag1 | 114.8 (3) | C321—C326—H32C | 119.9 |
C211—P2—C221 | 105.7 (4) | C416—C411—C412 | 116.7 (10) |
C211—P2—C2 | 107.1 (4) | C416—C411—P4 | 126.9 (9) |
C221—P2—C2 | 99.8 (4) | C412—C411—P4 | 116.4 (8) |
C211—P2—Ag1 | 116.9 (3) | C411—C412—C413 | 121.2 (13) |
C221—P2—Ag1 | 108.9 (3) | C411—C412—H41C | 119.4 |
C2—P2—Ag1 | 116.6 (3) | C413—C412—H41C | 119.4 |
C321—P3—C311 | 106.3 (5) | C414—C413—C412 | 119.5 (15) |
C321—P3—C2 | 104.3 (5) | C414—C413—H41E | 120.3 |
C311—P3—C2 | 103.4 (5) | C412—C413—H41E | 120.3 |
C321—P3—Ag2 | 120.4 (4) | C415—C414—C413 | 120.8 (14) |
C311—P3—Ag2 | 109.1 (4) | C415—C414—H41A | 119.6 |
C2—P3—Ag2 | 111.9 (3) | C413—C414—H41A | 119.6 |
C421—P4—C411 | 102.7 (5) | C414—C415—C416 | 120.0 (14) |
C421—P4—C3 | 103.0 (4) | C414—C415—H41D | 120.0 |
C411—P4—C3 | 103.3 (4) | C416—C415—H41D | 120.0 |
C421—P4—Ag2 | 116.8 (3) | C411—C416—C415 | 121.8 (12) |
C411—P4—Ag2 | 112.9 (3) | C411—C416—H41B | 119.1 |
C3—P4—Ag2 | 116.3 (3) | C415—C416—H41B | 119.1 |
C521—P5—C511 | 103.1 (4) | C422—C421—C426 | 118.0 (10) |
C521—P5—C3 | 105.2 (5) | C422—C421—P4 | 120.3 (8) |
C511—P5—C3 | 102.1 (5) | C426—C421—P4 | 121.7 (8) |
C521—P5—Ag3 | 113.6 (4) | C423—C422—C421 | 121.4 (12) |
C511—P5—Ag3 | 112.8 (3) | C423—C422—H42B | 119.3 |
C3—P5—Ag3 | 118.3 (3) | C421—C422—H42B | 119.3 |
C611—P6—C621 | 104.2 (5) | C424—C423—C422 | 120.7 (14) |
C611—P6—C1 | 101.3 (5) | C424—C423—H42D | 119.6 |
C621—P6—C1 | 105.2 (4) | C422—C423—H42D | 119.6 |
C611—P6—Ag3 | 113.8 (4) | C423—C424—C425 | 119.1 (13) |
C621—P6—Ag3 | 112.9 (3) | C423—C424—H42E | 120.5 |
C1—P6—Ag3 | 118.0 (3) | C425—C424—H42E | 120.5 |
P1—C1—P6 | 117.0 (5) | C424—C425—C426 | 121.3 (13) |
P1—C1—H1A | 108.1 | C424—C425—H42C | 119.3 |
P6—C1—H1A | 108.1 | C426—C425—H42C | 119.3 |
P1—C1—H1B | 108.1 | C425—C426—C421 | 119.5 (12) |
P6—C1—H1B | 108.1 | C425—C426—H42A | 120.3 |
H1A—C1—H1B | 107.3 | C421—C426—H42A | 120.3 |
P3—C2—P2 | 112.5 (5) | C516—C511—C512 | 117.8 (10) |
P3—C2—H2A | 109.1 | C516—C511—P5 | 118.1 (8) |
P2—C2—H2A | 109.1 | C512—C511—P5 | 124.1 (8) |
P3—C2—H2B | 109.1 | C511—C512—C513 | 120.2 (12) |
P2—C2—H2B | 109.1 | C511—C512—H51C | 119.9 |
H2A—C2—H2B | 107.8 | C513—C512—H51C | 119.9 |
P4—C3—P5 | 112.7 (5) | C514—C513—C512 | 119.1 (12) |
P4—C3—H3A | 109.0 | C514—C513—H51B | 120.4 |
P5—C3—H3A | 109.0 | C512—C513—H51B | 120.4 |
P4—C3—H3B | 109.0 | C515—C514—C513 | 121.4 (12) |
P5—C3—H3B | 109.0 | C515—C514—H51D | 119.3 |
H3A—C3—H3B | 107.8 | C513—C514—H51D | 119.3 |
Cl01—C4—Cl02 | 114.6 (7) | C514—C515—C516 | 119.4 (13) |
Cl01—C4—H4A | 108.6 | C514—C515—H51E | 120.3 |
Cl02—C4—H4A | 108.6 | C516—C515—H51E | 120.3 |
Cl01—C4—H4B | 108.6 | C511—C516—C515 | 122.0 (12) |
Cl02—C4—H4B | 108.6 | C511—C516—H51A | 119.0 |
H4A—C4—H4B | 107.6 | C515—C516—H51A | 119.0 |
Cl03—C5—Cl04 | 115.0 (11) | C526—C521—C522 | 118.8 (11) |
Cl03—C5—H5A | 108.5 | C526—C521—P5 | 123.6 (9) |
Cl04—C5—H5A | 108.5 | C522—C521—P5 | 117.5 (9) |
Cl03—C5—H5B | 108.5 | C521—C522—C523 | 119.7 (13) |
Cl04—C5—H5B | 108.5 | C521—C522—H52B | 120.2 |
H5A—C5—H5B | 107.5 | C523—C522—H52B | 120.2 |
C112—C111—C116 | 117.6 (11) | C524—C523—C522 | 120.8 (17) |
C112—C111—P1 | 119.1 (8) | C524—C523—H52E | 119.6 |
C116—C111—P1 | 123.2 (9) | C522—C523—H52E | 119.6 |
C111—C112—C113 | 120.9 (12) | C523—C524—C525 | 121.0 (17) |
C111—C112—H11B | 119.6 | C523—C524—H52D | 119.5 |
C113—C112—H11B | 119.6 | C525—C524—H52D | 119.5 |
C114—C113—C112 | 119.7 (14) | C524—C525—C526 | 119.4 (14) |
C114—C113—H11E | 120.2 | C524—C525—H52C | 120.3 |
C112—C113—H11E | 120.2 | C526—C525—H52C | 120.3 |
C115—C114—C113 | 119.8 (13) | C521—C526—C525 | 120.3 (13) |
C115—C114—H11D | 120.1 | C521—C526—H52A | 119.9 |
C113—C114—H11D | 120.1 | C525—C526—H52A | 119.9 |
C114—C115—C116 | 120.5 (12) | C612—C611—C616 | 117.6 (11) |
C114—C115—H11C | 119.8 | C612—C611—P6 | 119.2 (10) |
C116—C115—H11C | 119.8 | C616—C611—P6 | 123.2 (8) |
C115—C116—C111 | 121.6 (12) | C611—C612—C613 | 121.7 (14) |
C115—C116—H11A | 119.2 | C611—C612—H61A | 119.1 |
C111—C116—H11A | 119.2 | C613—C612—H61A | 119.1 |
C126—C121—C122 | 117.5 (10) | C614—C613—C612 | 119.3 (16) |
C126—C121—P1 | 119.2 (8) | C614—C613—H61E | 120.3 |
C122—C121—P1 | 123.3 (8) | C612—C613—H61E | 120.3 |
C123—C122—C121 | 120.1 (11) | C613—C614—C615 | 120.9 (14) |
C123—C122—H12A | 119.9 | C613—C614—H61C | 119.5 |
C121—C122—H12A | 119.9 | C615—C614—H61C | 119.5 |
C124—C123—C122 | 121.1 (12) | C614—C615—C616 | 119.5 (14) |
C124—C123—H12D | 119.5 | C614—C615—H61D | 120.3 |
C122—C123—H12D | 119.5 | C616—C615—H61D | 120.3 |
C123—C124—C125 | 119.6 (11) | C615—C616—C611 | 120.9 (12) |
C123—C124—H12E | 120.2 | C615—C616—H61B | 119.6 |
C125—C124—H12E | 120.2 | C611—C616—H61B | 119.6 |
C124—C125—C126 | 120.3 (11) | C622—C621—C626 | 118.8 (10) |
C124—C125—H12C | 119.9 | C622—C621—P6 | 119.5 (8) |
C126—C125—H12C | 119.9 | C626—C621—P6 | 121.7 (9) |
C121—C126—C125 | 121.4 (11) | C623—C622—C621 | 120.6 (11) |
C121—C126—H12B | 119.3 | C623—C622—H62A | 119.7 |
C125—C126—H12B | 119.3 | C621—C622—H62A | 119.7 |
C212—C211—C216 | 116.7 (10) | C624—C623—C622 | 121.0 (13) |
C212—C211—P2 | 118.6 (8) | C624—C623—H62C | 119.5 |
C216—C211—P2 | 124.8 (8) | C622—C623—H62C | 119.5 |
C211—C212—C213 | 122.3 (12) | C625—C624—C623 | 119.8 (14) |
C211—C212—H21B | 118.8 | C625—C624—H62E | 120.1 |
C213—C212—H21B | 118.8 | C623—C624—H62E | 120.1 |
C214—C213—C212 | 118.6 (13) | C624—C625—C626 | 121.6 (13) |
C214—C213—H21D | 120.7 | C624—C625—H62D | 119.2 |
C212—C213—H21D | 120.7 | C626—C625—H62D | 119.2 |
C215—C214—C213 | 121.0 (13) | C621—C626—C625 | 118.2 (12) |
C215—C214—H21C | 119.5 | C621—C626—H62B | 120.9 |
C213—C214—H21C | 119.5 | C625—C626—H62B | 120.9 |
C214—C215—C216 | 119.5 (13) |
Experimental details
Crystal data | |
Chemical formula | [Ag3(C25H22P2)3(HS)2]SbF6·2CH2Cl2 |
Mr | 1948.45 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 16.0813 (1), 18.0049 (2), 28.1089 (3) |
β (°) | 95.417 (1) |
V (Å3) | 8102.36 (13) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.40 |
Crystal size (mm) | 0.72 × 0.60 × 0.46 |
Data collection | |
Diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.354, 0.525 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 25151, 14088, 10084 |
Rint | 0.047 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.080, 0.210, 1.21 |
No. of reflections | 14088 |
No. of parameters | 807 |
No. of restraints | 4 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0537P)2 + 77.3298P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.50, −1.23 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1994), XPREP (Siemens, 1994), SHELXTL (Siemens, 1994), SHELXTL.
Ag1—P2 | 2.465 (2) | Ag2—S2 | 2.661 (3) |
Ag1—P1 | 2.465 (2) | Ag2—S1 | 2.825 (3) |
Ag1—S2 | 2.734 (3) | Ag3—P5 | 2.483 (3) |
Ag1—S1 | 2.760 (3) | Ag3—P6 | 2.491 (3) |
Ag1—Ag2 | 3.3369 (11) | Ag3—S1 | 2.686 (3) |
Ag2—P4 | 2.468 (2) | Ag3—S2 | 2.771 (3) |
Ag2—P3 | 2.469 (3) | ||
P2—Ag1—P1 | 126.27 (8) | P4—Ag2—P3 | 125.91 (9) |
P2—Ag1—S1 | 96.47 (8) | P3—Ag2—S2 | 116.19 (9) |
P2—Ag1—Ag2 | 86.89 (6) | P5—Ag3—S2 | 103.27 (9) |
P1—Ag1—Ag2 | 146.48 (6) | Ag3—S1—Ag1 | 79.33 (7) |
S2—Ag1—Ag2 | 50.81 (6) | Ag3—S1—Ag2 | 77.18 (7) |
S1—Ag1—Ag2 | 54.21 (6) | Ag1—S1—Ag2 | 73.38 (7) |
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There is considerable interest in designing novel metal complexes with mixed phosphorus- and sulfur-containing ligands owing to their unique optical and optoelectronic properties (Yam et al., 2000; Tang et al., 2002). It is well known that S2− and SH− as versatile coordination groups could exhibit various bonding modes to produce metal cluster complexes with diverse structural topologies (Kitagawa et al., 1990; Su et al., 1998). Here we reported the crystal structure of a trisilver complex, [Ag3(µ-dppm)3(µ3-S)2]SbF6, (I), which resulted from the self-assembly between the metal components [Pd(phen)(tdt)] (phen is phenanthroline and tdt is 3,4-toluenedithiolate) and [Ag2(µ2-dppm)2(MeCN)4](SbF6)2 through the disruption of C—S of tdt.
A perspective drawing of the complex cation with the atomic numbering scheme is depicted in Fig. 1 and selected bonding parameters are presented in Table 1. The complex consists of the coordination [Ag3(µ-dppm)3(µ3-S)2]+ cation, an SbF6− anion and dichloromethane solvent molecules. The µ3-SH dicapped trisilver complex exhibits a trigonal bipyramid coordination core, with two µ3-SH ligands in the apices and the three Ag atoms in equatorial sites. The Ag atoms are located at distorted tetrahedral environments with a P2S2 chromophore. The Ag—Ag distances are in the range of 3.337 (1)–3.477 (1) Å, which are shorter than the sum of van der Waals radii for two Ag atoms, indicating a weak metal–metal contact that is operative in the complex. The Ag—S distances are in the range 2.661 (3)–2.825 (3) Å and the Ag—P bond distances are in the range 2.465 (2)–2.491 (3) Å, close to those found in other similar complexes of silver (Albano et al., 1999; Meyer et al., 1989; Lang et al., 1993; Henkel et al., 1988).