Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802020585/mg6018sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802020585/mg6018Isup2.hkl |
CCDC reference: 202285
Compound (I) was isolated from the reaction of 0.23 g (0.26 mmol) of [Ge(OC6HPh4-2,3,5,6)2] with 0.14 g (0.31 mmol) of Ph3Ge(OSO2CF3) in benzene, yielding 0.020 g of (I). Ph3Ge(OSO2CF3) was prepared from Ph3GeCl (1.00 g, 2.94 mmol) and Ag(OSO2CF3) (0.84 g, 3.3 mmol) in benzene in the absence of light and was judged to be pure by 1H and 19F NMR spectroscopic analysis.
Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976) and PLUTON (Spek, 1991); software used to prepare material for publication: CIF VAX in MolEN (Fair, 1990).
Fig. 1. ORTEP plot highlighting the environment about the silver cation of (I). Displacement ellipsoids are drawn at the 50% probability level. |
[Ag2Ge(CF3O3S)(C45H29O)3]·4C6H6 | F(000) = 3976 |
Mr = 1942.36 | Dx = 1.41 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 63826 reflections |
a = 13.9593 (2) Å | θ = 2.1–27.9° |
b = 24.3433 (3) Å | µ = 0.83 mm−1 |
c = 26.9406 (4) Å | T = 150 K |
β = 92.1511 (5)° | Chunk, colorless |
V = 9148.4 (4) Å3 | 0.30 × 0.30 × 0.25 mm |
Z = 4 |
Nonius KappaCCD diffractometer | 15451 reflections with I > 2σ(I) |
ω scans | Rint = 0.060 |
Absorption correction: empirical (using intensity measurements) ? | θmax = 27.9°, θmin = 2.1° |
Tmin = 0.574, Tmax = 0.814 | h = 0→18 |
63826 measured reflections | k = 0→30 |
21443 independent reflections | l = −35→35 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.039 | w = 1/[σ2(Fo2) + (0.0352P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.074 | (Δ/σ)max = 0.003 |
S = 0.91 | Δρmax = 0.38 e Å−3 |
21401 reflections | Δρmin = −0.67 e Å−3 |
1153 parameters |
[Ag2Ge(CF3O3S)(C45H29O)3]·4C6H6 | V = 9148.4 (4) Å3 |
Mr = 1942.36 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.9593 (2) Å | µ = 0.83 mm−1 |
b = 24.3433 (3) Å | T = 150 K |
c = 26.9406 (4) Å | 0.30 × 0.30 × 0.25 mm |
β = 92.1511 (5)° |
Nonius KappaCCD diffractometer | 21443 independent reflections |
Absorption correction: empirical (using intensity measurements) ? | 15451 reflections with I > 2σ(I) |
Tmin = 0.574, Tmax = 0.814 | Rint = 0.060 |
63826 measured reflections |
R[F2 > 2σ(F2)] = 0.039 | 0 restraints |
wR(F2) = 0.074 | H-atom parameters constrained |
S = 0.91 | Δρmax = 0.38 e Å−3 |
21401 reflections | Δρmin = −0.67 e Å−3 |
1153 parameters |
Refinement. Refinement on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R_factor_obs 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 | ||
Ag(1) | −0.437150 (15) | 0.729384 (9) | −0.055894 (8) | 0.03858 (6) | |
Ag(2) | −0.254135 (15) | 0.752632 (8) | 0.134525 (8) | 0.03497 (6) | |
Ge | −0.355393 (18) | 0.739789 (10) | 0.026357 (10) | 0.02507 (7) | |
S(1) | −0.57961 (5) | 0.71372 (3) | −0.16328 (3) | 0.04621 (19) | |
F(11) | −0.59556 (16) | 0.62559 (9) | −0.21880 (8) | 0.0833 (7) | |
F(12) | −0.46593 (15) | 0.67142 (9) | −0.22792 (7) | 0.0796 (6) | |
F(13) | −0.48146 (15) | 0.62172 (8) | −0.16304 (7) | 0.0759 (6) | |
O(1) | −0.30876 (11) | 0.80526 (6) | 0.05248 (6) | 0.0280 (4) | |
O(2) | −0.24494 (11) | 0.70427 (6) | 0.04834 (6) | 0.0281 (4) | |
O(3) | −0.41258 (11) | 0.72295 (6) | 0.08517 (6) | 0.0271 (4) | |
O(11) | −0.49709 (14) | 0.73474 (8) | −0.13506 (7) | 0.0484 (5) | |
O(12) | −0.65153 (14) | 0.69072 (8) | −0.13313 (8) | 0.0536 (6) | |
O(13) | −0.61197 (15) | 0.74821 (9) | −0.20367 (8) | 0.0626 (6) | |
C(1) | −0.5288 (3) | 0.65566 (15) | −0.19441 (12) | 0.0589 (9) | |
C(11) | −0.26267 (17) | 0.84362 (9) | 0.02416 (9) | 0.0270 (6) | |
C(12) | −0.16440 (17) | 0.85272 (9) | 0.03406 (9) | 0.0269 (6) | |
C(14) | −0.16652 (18) | 0.91705 (10) | −0.03387 (10) | 0.0316 (6) | |
C(15) | −0.26415 (18) | 0.91007 (10) | −0.04253 (9) | 0.0301 (6) | |
C(16) | −0.31448 (17) | 0.87248 (9) | −0.01307 (9) | 0.0273 (6) | |
C(21) | −0.22228 (17) | 0.65115 (9) | 0.03561 (10) | 0.0283 (6) | |
C(22) | −0.21540 (18) | 0.61159 (10) | 0.07368 (9) | 0.0297 (6) | |
C(23) | −0.19486 (18) | 0.55698 (10) | 0.06118 (10) | 0.0319 (6) | |
C(24) | −0.18223 (19) | 0.54433 (10) | 0.01144 (10) | 0.0357 (6) | |
C(25) | −0.18761 (19) | 0.58319 (10) | −0.02622 (10) | 0.0335 (6) | |
C(26) | −0.20710 (17) | 0.63809 (10) | −0.01426 (9) | 0.0287 (6) | |
C(31) | −0.50846 (17) | 0.73051 (9) | 0.09178 (9) | 0.0256 (5) | |
C(32) | −0.53537 (17) | 0.76832 (9) | 0.12818 (9) | 0.0271 (5) | |
C(33) | −0.63359 (18) | 0.77866 (9) | 0.13379 (9) | 0.0297 (6) | |
C(34) | −0.69998 (18) | 0.75125 (10) | 0.10295 (10) | 0.0341 (6) | |
C(35) | −0.67409 (18) | 0.71205 (10) | 0.06884 (9) | 0.0305 (6) | |
C(36) | −0.57669 (18) | 0.70001 (9) | 0.06305 (9) | 0.0274 (6) | |
C(121) | −0.11308 (17) | 0.82392 (9) | 0.07609 (10) | 0.0283 (6) | |
C(122) | −0.14055 (19) | 0.83340 (10) | 0.12461 (10) | 0.0344 (6) | |
C(123) | −0.0887 (2) | 0.81031 (11) | 0.16465 (11) | 0.0423 (7) | |
C(124) | −0.0102 (2) | 0.77687 (12) | 0.15649 (12) | 0.0468 (8) | |
C(125) | 0.01561 (19) | 0.76647 (11) | 0.10857 (11) | 0.0415 (7) | |
C(126) | −0.03436 (18) | 0.79004 (10) | 0.06859 (10) | 0.0329 (6) | |
C(131) | −0.01254 (18) | 0.90310 (10) | 0.01266 (10) | 0.0320 (6) | |
C(132) | 0.0504 (2) | 0.89769 (11) | −0.02631 (12) | 0.0461 (7) | |
C(133) | 0.1462 (2) | 0.91047 (13) | −0.01956 (14) | 0.0575 (9) | |
C(134) | 0.1818 (2) | 0.92978 (12) | 0.02558 (15) | 0.0570 (9) | |
C(135) | 0.1211 (2) | 0.93603 (11) | 0.06424 (13) | 0.0485 (8) | |
C(136) | 0.0240 (2) | 0.92269 (10) | 0.05808 (11) | 0.0405 (7) | |
C(13]) | −0.11609 (18) | 0.89009 (10) | 0.00439 (10) | 0.0301 (6) | |
C(151) | −0.31313 (18) | 0.94474 (10) | −0.08139 (10) | 0.0318 (6) | |
C(152) | −0.38866 (19) | 0.97946 (10) | −0.06989 (11) | 0.0374 (7) | |
C(153) | −0.4292 (2) | 1.01414 (11) | −0.10560 (12) | 0.0465 (8) | |
C(154) | −0.3962 (2) | 1.01494 (12) | −0.15280 (12) | 0.0521 (8) | |
C(155) | −0.3220 (2) | 0.98093 (12) | −0.16497 (12) | 0.0531 (8) | |
C(156) | −0.2801 (2) | 0.94613 (11) | −0.12935 (11) | 0.0417 (7) | |
C(161) | −0.41960 (17) | 0.86299 (9) | −0.02090 (10) | 0.0302 (6) | |
C(162) | −0.47898 (19) | 0.86559 (10) | 0.01938 (11) | 0.0383 (7) | |
C(163) | −0.5765 (2) | 0.85451 (12) | 0.01340 (13) | 0.0504 (8) | |
C(164) | −0.6150 (2) | 0.84099 (12) | −0.03258 (13) | 0.0515 (8) | |
C(165) | −0.5577 (2) | 0.83903 (11) | −0.07269 (12) | 0.0460 (8) | |
C(166) | −0.46046 (19) | 0.84945 (10) | −0.06719 (10) | 0.0351 (6) | |
C(221) | −0.23030 (19) | 0.62806 (10) | 0.12642 (10) | 0.0320 (6) | |
C(222) | −0.1652 (2) | 0.66382 (10) | 0.15035 (10) | 0.0351 (6) | |
C(223) | −0.1739 (2) | 0.67710 (11) | 0.20047 (10) | 0.0437 (7) | |
C(224) | −0.2487 (2) | 0.65500 (11) | 0.22679 (11) | 0.0468 (8) | |
C(225) | −0.3128 (2) | 0.62024 (11) | 0.20302 (11) | 0.0458 (8) | |
C(226) | −0.3037 (2) | 0.60620 (11) | 0.15330 (10) | 0.0370 (7) | |
C(231) | −0.18686 (19) | 0.51165 (10) | 0.09811 (10) | 0.0365 (6) | |
C(232) | −0.2278 (2) | 0.46088 (11) | 0.08615 (12) | 0.0471 (8) | |
C(233) | −0.2206 (2) | 0.41717 (13) | 0.11860 (14) | 0.0592 (9) | |
C(234) | −0.1741 (2) | 0.42394 (13) | 0.16424 (13) | 0.0591 (9) | |
C(235) | −0.1337 (2) | 0.47355 (13) | 0.17712 (12) | 0.0545 (9) | |
C(236) | −0.1390 (2) | 0.51703 (11) | 0.14422 (11) | 0.0434 (7) | |
C(251) | −0.1702 (2) | 0.56540 (10) | −0.07811 (10) | 0.0357 (7) | |
C(252) | −0.2268 (2) | 0.52388 (11) | −0.09964 (11) | 0.0467 (8) | |
C(253) | −0.2110 (3) | 0.50626 (13) | −0.14840 (12) | 0.0599 (10) | |
C(254) | −0.1396 (3) | 0.53070 (14) | −0.17460 (13) | 0.0607 (10) | |
C(255) | −0.0834 (2) | 0.57141 (13) | −0.15360 (12) | 0.0550 (9) | |
C(256) | −0.0988 (2) | 0.58885 (12) | −0.10571 (11) | 0.0426 (7) | |
C(261) | −0.21245 (18) | 0.68182 (9) | −0.05287 (9) | 0.0279 (6) | |
C(262) | −0.15895 (18) | 0.72959 (10) | −0.04672 (10) | 0.0338 (6) | |
C(263) | −0.1646 (2) | 0.77096 (11) | −0.08177 (11) | 0.0434 (7) | |
C(264) | −0.2233 (2) | 0.76537 (11) | −0.12411 (11) | 0.0446 (7) | |
C(265) | −0.2765 (2) | 0.71775 (11) | −0.13106 (10) | 0.0396 (7) | |
C(266) | −0.27169 (18) | 0.67656 (10) | −0.09585 (9) | 0.0315 (6) | |
C(321) | −0.45985 (17) | 0.79780 (10) | 0.15834 (9) | 0.0280 (6) | |
C(322) | −0.39520 (18) | 0.76959 (10) | 0.19015 (10) | 0.0321 (6) | |
C(323) | −0.32616 (19) | 0.79805 (11) | 0.21823 (10) | 0.0391 (7) | |
C(324) | −0.3193 (2) | 0.85466 (12) | 0.21432 (11) | 0.0433 (7) | |
C(325) | −0.3837 (2) | 0.88288 (11) | 0.18382 (11) | 0.0406 (7) | |
C(326) | −0.45349 (19) | 0.85499 (10) | 0.15621 (10) | 0.0334 (6) | |
C(331) | −0.67162 (19) | 0.81503 (10) | 0.17295 (10) | 0.0338 (6) | |
C(332) | −0.7462 (2) | 0.85098 (11) | 0.16131 (12) | 0.0435 (7) | |
C(333) | −0.7877 (2) | 0.88189 (12) | 0.19834 (14) | 0.0547 (9) | |
C(334) | −0.7561 (2) | 0.87684 (13) | 0.24687 (14) | 0.0594 (10) | |
C(335) | −0.6820 (2) | 0.84084 (13) | 0.25913 (12) | 0.0526 (8) | |
C(336) | −0.6399 (2) | 0.81035 (11) | 0.22236 (11) | 0.0408 (7) | |
C(351) | −0.75579 (18) | 0.68144 (10) | 0.04349 (10) | 0.0332 (6) | |
C(352) | −0.8156 (2) | 0.70700 (12) | 0.00831 (11) | 0.0444 (7) | |
C(353) | −0.8978 (2) | 0.68105 (13) | −0.01027 (12) | 0.0519 (8) | |
C(354) | −0.9221 (2) | 0.62978 (13) | 0.00671 (12) | 0.0506 (8) | |
C(355) | −0.8636 (2) | 0.60396 (12) | 0.04167 (12) | 0.0466 (8) | |
C(356) | −0.7801 (2) | 0.62924 (11) | 0.05941 (11) | 0.0389 (7) | |
C(361) | −0.54512 (17) | 0.65618 (9) | 0.02874 (10) | 0.0282 (6) | |
C(362) | −0.47681 (19) | 0.61772 (10) | 0.04516 (10) | 0.0332 (6) | |
C(363) | −0.4458 (2) | 0.57634 (10) | 0.01416 (11) | 0.0401 (7) | |
C(364) | −0.4825 (2) | 0.57319 (11) | −0.03420 (11) | 0.0437 (7) | |
C(365) | −0.5492 (2) | 0.61123 (11) | −0.05137 (11) | 0.0400 (7) | |
C(366) | −0.58054 (18) | 0.65251 (10) | −0.02018 (9) | 0.0304 (6) | |
C(614) | 0.0247 (4) | 0.0205 (3) | 0.3152 (2) | 0.125 (2) | |
C(911) | 0.1335 (4) | 0.0848 (2) | 0.2570 (2) | 0.0995 (15) | |
C(912) | 0.1121 (4) | 0.1030 (2) | 0.3025 (3) | 0.127 (2) | |
C(913) | 0.0582 (5) | 0.0709 (4) | 0.3325 (3) | 0.156 (3) | |
C(915) | 0.0454 (3) | 0.00376 (18) | 0.2680 (2) | 0.0860 (13) | |
C(916) | 0.0991 (3) | 0.03582 (18) | 0.23960 (17) | 0.0837 (12) | |
C(921) | 0.0487 (3) | 0.60401 (15) | 0.22929 (17) | 0.0735 (11) | |
C(922) | 0.1008 (3) | 0.62026 (17) | 0.19102 (15) | 0.0770 (12) | |
C(923) | 0.1561 (3) | 0.66672 (19) | 0.19484 (16) | 0.0842 (13) | |
C(924) | 0.1583 (3) | 0.69674 (14) | 0.23920 (17) | 0.0703 (11) | |
C(925) | 0.1029 (3) | 0.67994 (14) | 0.27665 (14) | 0.0614 (9) | |
C(926) | 0.0495 (3) | 0.63375 (15) | 0.27204 (14) | 0.0668 (10) | |
C(931) | 0.2807 (3) | 0.49287 (14) | 0.69942 (15) | 0.0673 (10) | |
C(932) | 0.1967 (3) | 0.46419 (13) | 0.69313 (15) | 0.0615 (10) | |
C(933) | 0.1528 (3) | 0.45978 (13) | 0.64699 (15) | 0.0601 (9) | |
C(934) | 0.1927 (3) | 0.48454 (14) | 0.60673 (15) | 0.0656 (10) | |
C(935) | 0.2772 (3) | 0.51342 (14) | 0.61281 (16) | 0.0691 (10) | |
C(936) | 0.3208 (3) | 0.51776 (14) | 0.65884 (17) | 0.0695 (11) | |
C(941) | 0.0558 (4) | 0.84935 (18) | 0.82725 (17) | 0.0859 (13) | |
C(942) | 0.0036 (3) | 0.8035 (2) | 0.81661 (16) | 0.0840 (13) | |
C(943) | 0.0352 (3) | 0.75306 (18) | 0.83081 (16) | 0.0814 (12) | |
C(944) | 0.1221 (3) | 0.74773 (17) | 0.85571 (15) | 0.0772 (11) | |
C(945) | 0.1751 (3) | 0.7936 (2) | 0.86633 (15) | 0.0821 (12) | |
C(946) | 0.1427 (4) | 0.8443 (2) | 0.85257 (17) | 0.0873 (14) | |
H(14) | −0.1328 | 0.9411 | −0.0548 | 0.038* | |
H(24) | −0.1693 | 0.5073 | 0.0029 | 0.043* | |
H(34) | −0.7660 | 0.7599 | 0.1054 | 0.041* | |
H(122) | −0.1948 | 0.8557 | 0.1304 | 0.041* | |
H(123) | −0.1071 | 0.8175 | 0.1976 | 0.051* | |
H(124) | 0.0254 | 0.7613 | 0.1838 | 0.056* | |
H(125) | 0.0683 | 0.7429 | 0.1029 | 0.050* | |
H(126) | −0.0148 | 0.7831 | 0.0358 | 0.039* | |
H(132) | 0.0268 | 0.8850 | −0.0578 | 0.055* | |
H(133) | 0.1881 | 0.9059 | −0.0462 | 0.069* | |
H(134) | 0.2478 | 0.9387 | 0.0299 | 0.068* | |
H(135) | 0.1454 | 0.9495 | 0.0953 | 0.058* | |
H(136) | −0.0173 | 0.9270 | 0.0850 | 0.049* | |
H(152) | −0.4125 | 0.9793 | −0.0373 | 0.045* | |
H(153) | −0.4805 | 1.0376 | −0.0972 | 0.056* | |
H(154) | −0.4244 | 1.0389 | −0.1770 | 0.063* | |
H(155) | −0.2992 | 0.9812 | −0.1978 | 0.064* | |
H(156) | −0.2284 | 0.9231 | −0.1379 | 0.050* | |
H(162) | −0.4527 | 0.8750 | 0.0513 | 0.046* | |
H(163) | −0.6164 | 0.8563 | 0.0412 | 0.060* | |
H(164) | −0.6815 | 0.8330 | −0.0366 | 0.062* | |
H(165) | −0.5849 | 0.8304 | −0.1046 | 0.055* | |
H(166) | −0.4213 | 0.8474 | −0.0952 | 0.042* | |
H(222) | −0.1145 | 0.6793 | 0.1324 | 0.042* | |
H(223) | −0.1289 | 0.7011 | 0.2165 | 0.052* | |
H(224) | −0.2553 | 0.6639 | 0.2608 | 0.056* | |
H(225) | −0.3644 | 0.6055 | 0.2208 | 0.055* | |
H(226) | −0.3481 | 0.5815 | 0.1378 | 0.044* | |
H(232) | −0.2613 | 0.4563 | 0.0551 | 0.057* | |
H(233) | −0.2476 | 0.3826 | 0.1096 | 0.071* | |
H(234) | −0.1700 | 0.3941 | 0.1869 | 0.071* | |
H(235) | −0.1020 | 0.4780 | 0.2087 | 0.065* | |
H(236) | −0.1098 | 0.5510 | 0.1531 | 0.052* | |
H(252) | −0.2761 | 0.5075 | −0.0813 | 0.056* | |
H(253) | −0.2491 | 0.4778 | −0.1631 | 0.072* | |
H(254) | −0.1292 | 0.5192 | −0.2077 | 0.073* | |
H(255) | −0.0340 | 0.5876 | −0.1720 | 0.066* | |
H(256) | −0.0600 | 0.6172 | −0.0915 | 0.051* | |
H(262) | −0.1179 | 0.7339 | −0.0180 | 0.041* | |
H(263) | −0.1281 | 0.8035 | −0.0768 | 0.052* | |
H(264) | −0.2269 | 0.7939 | −0.1482 | 0.053* | |
H(265) | −0.3164 | 0.7134 | −0.1601 | 0.047* | |
H(266) | −0.3090 | 0.6442 | −0.1008 | 0.038* | |
H(322) | −0.3986 | 0.7307 | 0.1925 | 0.039* | |
H(323) | −0.2835 | 0.7787 | 0.2402 | 0.047* | |
H(324) | −0.2703 | 0.8739 | 0.2326 | 0.052* | |
H(325) | −0.3801 | 0.9218 | 0.1818 | 0.049* | |
H(326) | −0.4977 | 0.8750 | 0.1355 | 0.040* | |
H(332) | −0.7692 | 0.8545 | 0.1278 | 0.052* | |
H(333) | −0.8384 | 0.9066 | 0.1899 | 0.066* | |
H(334) | −0.7847 | 0.8979 | 0.2720 | 0.071* | |
H(335) | −0.6601 | 0.8371 | 0.2928 | 0.063* | |
H(336) | −0.5888 | 0.7860 | 0.2310 | 0.049* | |
H(352) | −0.8000 | 0.7427 | −0.0032 | 0.053* | |
H(353) | −0.9375 | 0.6987 | −0.0348 | 0.062* | |
H(354) | −0.9790 | 0.6123 | −0.0057 | 0.061* | |
H(355) | −0.8805 | 0.5687 | 0.0537 | 0.056* | |
H(356) | −0.7391 | 0.6106 | 0.0827 | 0.047* | |
H(362) | −0.4510 | 0.6199 | 0.0782 | 0.040* | |
H(363) | −0.3997 | 0.5503 | 0.0261 | 0.048* | |
H(364) | −0.4619 | 0.5449 | −0.0556 | 0.052* | |
H(365) | −0.5738 | 0.6092 | −0.0847 | 0.048* | |
H(366) | −0.6265 | 0.6784 | −0.0324 | 0.036* | |
H(614) | −0.0122 | −0.0023 | 0.3358 | 0.150* | |
H(911) | 0.1731 | 0.1064 | 0.2368 | 0.119* | |
H(912) | 0.1343 | 0.1379 | 0.3137 | 0.153* | |
H(913) | 0.0438 | 0.0831 | 0.3649 | 0.187* | |
H(915) | 0.0217 | −0.0304 | 0.2556 | 0.103* | |
H(916) | 0.1134 | 0.0242 | 0.2070 | 0.100* | |
H(921) | 0.0111 | 0.5715 | 0.2265 | 0.088* | |
H(922) | 0.0993 | 0.5995 | 0.1612 | 0.092* | |
H(923) | 0.1925 | 0.6784 | 0.1677 | 0.101* | |
H(924) | 0.1979 | 0.7283 | 0.2430 | 0.084* | |
H(925) | 0.1016 | 0.7008 | 0.3064 | 0.074* | |
H(926) | 0.0122 | 0.6220 | 0.2989 | 0.080* | |
H(931) | 0.3113 | 0.4957 | 0.7314 | 0.081* | |
H(932) | 0.1689 | 0.4473 | 0.7209 | 0.074* | |
H(933) | 0.0947 | 0.4397 | 0.6428 | 0.072* | |
H(934) | 0.1620 | 0.4817 | 0.5748 | 0.079* | |
H(935) | 0.3051 | 0.5303 | 0.5850 | 0.083* | |
H(936) | 0.3788 | 0.5379 | 0.6631 | 0.083* | |
H(941) | 0.0325 | 0.8845 | 0.8173 | 0.103* | |
H(942) | −0.0562 | 0.8068 | 0.7989 | 0.101* | |
H(943) | −0.0028 | 0.7215 | 0.8235 | 0.098* | |
H(944) | 0.1452 | 0.7125 | 0.8655 | 0.093* | |
H(945) | 0.2355 | 0.7901 | 0.8835 | 0.099* | |
H(946) | 0.1800 | 0.8761 | 0.8604 | 0.105* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag(1) | 0.03789 (12) | 0.05013 (13) | 0.02716 (12) | 0.00146 (10) | −0.00630 (9) | 0.00060 (9) |
Ag(2) | 0.03490 (12) | 0.04095 (12) | 0.02869 (12) | 0.00217 (9) | −0.00359 (9) | −0.00146 (9) |
Ge | 0.02307 (14) | 0.02897 (14) | 0.02307 (14) | 0.00039 (10) | −0.00057 (11) | 0.00087 (11) |
S(1) | 0.0379 (4) | 0.0621 (5) | 0.0381 (5) | −0.0011 (4) | −0.0069 (4) | 0.0141 (4) |
F(11) | 0.0887 (17) | 0.0941 (15) | 0.0657 (15) | −0.0182 (12) | −0.0179 (13) | −0.0117 (12) |
F(12) | 0.0651 (14) | 0.1332 (19) | 0.0410 (12) | 0.0003 (12) | 0.0060 (11) | −0.0052 (12) |
F(13) | 0.0900 (16) | 0.0899 (14) | 0.0470 (12) | 0.0372 (12) | −0.0062 (11) | −0.0041 (10) |
O(1) | 0.0256 (9) | 0.0311 (9) | 0.0275 (10) | −0.0006 (7) | 0.0017 (8) | 0.0037 (7) |
O(2) | 0.0283 (10) | 0.0303 (9) | 0.0255 (10) | 0.0042 (7) | −0.0013 (8) | −0.0020 (7) |
O(3) | 0.0222 (9) | 0.0322 (9) | 0.0267 (10) | 0.0012 (7) | −0.0010 (7) | −0.0017 (7) |
O(11) | 0.0424 (12) | 0.0719 (14) | 0.0304 (11) | −0.0053 (10) | −0.0070 (9) | 0.0044 (10) |
O(12) | 0.0396 (12) | 0.0595 (13) | 0.0621 (15) | 0.0030 (10) | 0.0075 (11) | 0.0253 (11) |
O(13) | 0.0543 (14) | 0.0770 (15) | 0.0550 (15) | −0.0080 (11) | −0.0186 (11) | 0.0361 (12) |
C(1) | 0.055 (2) | 0.089 (3) | 0.0322 (19) | −0.0043 (19) | −0.0134 (17) | 0.0013 (17) |
C(11) | 0.0266 (14) | 0.0264 (13) | 0.0284 (15) | −0.0024 (10) | 0.0036 (11) | 0.0002 (10) |
C(12) | 0.0248 (14) | 0.0283 (13) | 0.0277 (15) | 0.0021 (10) | 0.0010 (11) | −0.0009 (10) |
C(14) | 0.0285 (15) | 0.0320 (14) | 0.0348 (17) | −0.0016 (11) | 0.0060 (12) | 0.0044 (11) |
C(15) | 0.0310 (15) | 0.0309 (13) | 0.0286 (15) | 0.0021 (11) | 0.0027 (12) | −0.0003 (11) |
C(16) | 0.0259 (14) | 0.0273 (13) | 0.0285 (15) | 0.0004 (10) | 0.0007 (11) | −0.0006 (10) |
C(21) | 0.0228 (14) | 0.0312 (14) | 0.0309 (16) | 0.0001 (10) | −0.0009 (11) | −0.0033 (11) |
C(22) | 0.0265 (14) | 0.0364 (14) | 0.0257 (15) | 0.0004 (11) | −0.0032 (11) | 0.0001 (11) |
C(23) | 0.0309 (15) | 0.0329 (14) | 0.0314 (16) | 0.0019 (11) | −0.0055 (12) | 0.0000 (11) |
C(24) | 0.0402 (17) | 0.0298 (14) | 0.0368 (17) | 0.0054 (12) | −0.0042 (13) | −0.0032 (12) |
C(25) | 0.0309 (15) | 0.0381 (15) | 0.0313 (16) | 0.0030 (12) | −0.0023 (12) | −0.0045 (12) |
C(26) | 0.0237 (14) | 0.0352 (14) | 0.0269 (15) | 0.0012 (11) | −0.0021 (11) | −0.0020 (11) |
C(31) | 0.0225 (13) | 0.0303 (13) | 0.0239 (14) | −0.0015 (10) | 0.0011 (11) | 0.0036 (10) |
C(32) | 0.0261 (13) | 0.0296 (13) | 0.0256 (14) | −0.0022 (10) | 0.0013 (11) | 0.0033 (10) |
C(33) | 0.0321 (15) | 0.0301 (13) | 0.0270 (15) | −0.0003 (11) | 0.0027 (12) | −0.0023 (11) |
C(34) | 0.0232 (13) | 0.0435 (15) | 0.0358 (16) | 0.0015 (12) | 0.0030 (12) | −0.0033 (12) |
C(35) | 0.0276 (14) | 0.0361 (14) | 0.0275 (15) | −0.0041 (11) | −0.0019 (12) | 0.0026 (11) |
C(36) | 0.0285 (14) | 0.0301 (13) | 0.0234 (14) | −0.0023 (11) | 0.0007 (11) | 0.0016 (10) |
C(121) | 0.0234 (14) | 0.0296 (13) | 0.0317 (16) | −0.0053 (10) | −0.0017 (11) | 0.0003 (11) |
C(122) | 0.0297 (15) | 0.0375 (15) | 0.0359 (17) | −0.0012 (12) | −0.0004 (13) | −0.0016 (12) |
C(123) | 0.0417 (18) | 0.0545 (17) | 0.0303 (17) | −0.0034 (14) | −0.0037 (14) | −0.0019 (13) |
C(124) | 0.0344 (17) | 0.0600 (19) | 0.045 (2) | −0.0015 (14) | −0.0121 (15) | 0.0085 (15) |
C(125) | 0.0261 (15) | 0.0466 (16) | 0.051 (2) | 0.0027 (12) | −0.0040 (14) | 0.0052 (14) |
C(126) | 0.0251 (14) | 0.0368 (14) | 0.0368 (17) | −0.0046 (11) | 0.0006 (12) | 0.0005 (12) |
C(131) | 0.0252 (14) | 0.0292 (13) | 0.0414 (17) | −0.0021 (11) | 0.0008 (12) | 0.0038 (11) |
C(132) | 0.0348 (17) | 0.0529 (18) | 0.051 (2) | −0.0047 (13) | 0.0084 (15) | 0.0001 (15) |
C(133) | 0.0313 (18) | 0.065 (2) | 0.077 (3) | −0.0066 (15) | 0.0161 (18) | 0.0004 (18) |
C(134) | 0.0266 (17) | 0.0520 (19) | 0.092 (3) | −0.0084 (14) | 0.0002 (19) | 0.0062 (18) |
C(135) | 0.0414 (19) | 0.0373 (16) | 0.065 (2) | −0.0094 (13) | −0.0183 (17) | 0.0035 (14) |
C(136) | 0.0362 (17) | 0.0345 (15) | 0.050 (2) | −0.0035 (12) | −0.0034 (14) | −0.0016 (13) |
C(13) | 0.0251 (14) | 0.0336 (14) | 0.0318 (16) | 0.0002 (11) | 0.0021 (12) | −0.0029 (11) |
C(151) | 0.0301 (15) | 0.0286 (13) | 0.0363 (17) | −0.0046 (11) | −0.0026 (12) | 0.0045 (11) |
C(152) | 0.0392 (17) | 0.0335 (14) | 0.0395 (17) | −0.0020 (12) | 0.0006 (13) | 0.0026 (12) |
C(153) | 0.0482 (19) | 0.0340 (15) | 0.057 (2) | 0.0047 (13) | −0.0049 (16) | 0.0067 (14) |
C(154) | 0.056 (2) | 0.0473 (18) | 0.052 (2) | 0.0029 (16) | −0.0121 (17) | 0.0159 (15) |
C(155) | 0.063 (2) | 0.0578 (19) | 0.0380 (19) | −0.0008 (17) | −0.0017 (16) | 0.0170 (15) |
C(156) | 0.0417 (18) | 0.0469 (17) | 0.0366 (18) | −0.0009 (13) | 0.0008 (14) | 0.0069 (13) |
C(161) | 0.0256 (14) | 0.0283 (13) | 0.0367 (17) | 0.0016 (10) | 0.0019 (12) | 0.0058 (11) |
C(162) | 0.0320 (16) | 0.0428 (16) | 0.0402 (18) | 0.0052 (12) | 0.0012 (13) | 0.0047 (13) |
C(163) | 0.0311 (18) | 0.066 (2) | 0.055 (2) | 0.0051 (14) | 0.0093 (16) | 0.0147 (16) |
C(164) | 0.0257 (16) | 0.061 (2) | 0.067 (2) | −0.0024 (14) | −0.0051 (17) | 0.0132 (17) |
C(165) | 0.0379 (18) | 0.0456 (17) | 0.053 (2) | −0.0005 (13) | −0.0169 (16) | 0.0075 (14) |
C(166) | 0.0360 (16) | 0.0339 (14) | 0.0350 (17) | −0.0004 (12) | −0.0021 (13) | 0.0039 (12) |
C(221) | 0.0356 (16) | 0.0321 (14) | 0.0280 (15) | 0.0086 (11) | −0.0028 (12) | 0.0025 (11) |
C(222) | 0.0413 (17) | 0.0343 (14) | 0.0294 (16) | 0.0080 (12) | −0.0025 (13) | −0.0006 (11) |
C(223) | 0.059 (2) | 0.0401 (16) | 0.0312 (17) | 0.0108 (14) | −0.0110 (15) | −0.0027 (13) |
C(224) | 0.070 (2) | 0.0466 (17) | 0.0232 (16) | 0.0122 (16) | −0.0012 (16) | 0.0048 (13) |
C(225) | 0.055 (2) | 0.0475 (17) | 0.0352 (18) | 0.0121 (15) | 0.0081 (15) | 0.0101 (14) |
C(226) | 0.0390 (17) | 0.0394 (15) | 0.0324 (17) | 0.0063 (12) | −0.0022 (13) | 0.0044 (12) |
C(231) | 0.0360 (16) | 0.0375 (15) | 0.0359 (17) | 0.0050 (12) | −0.0004 (13) | 0.0023 (12) |
C(232) | 0.0482 (19) | 0.0418 (17) | 0.051 (2) | −0.0032 (14) | −0.0057 (16) | 0.0075 (14) |
C(233) | 0.060 (2) | 0.0458 (18) | 0.071 (3) | −0.0067 (16) | −0.002 (2) | 0.0153 (17) |
C(234) | 0.062 (2) | 0.056 (2) | 0.060 (2) | 0.0121 (17) | 0.0103 (19) | 0.0276 (17) |
C(235) | 0.066 (2) | 0.058 (2) | 0.040 (2) | 0.0197 (17) | −0.0013 (17) | 0.0083 (15) |
C(236) | 0.0474 (19) | 0.0436 (16) | 0.0389 (18) | 0.0135 (14) | −0.0052 (15) | 0.0011 (13) |
C(251) | 0.0444 (18) | 0.0351 (14) | 0.0270 (16) | 0.0122 (12) | −0.0072 (13) | −0.0044 (11) |
C(252) | 0.060 (2) | 0.0437 (16) | 0.0359 (18) | 0.0095 (15) | −0.0078 (15) | −0.0068 (13) |
C(253) | 0.084 (3) | 0.0493 (19) | 0.045 (2) | 0.0175 (18) | −0.017 (2) | −0.0154 (16) |
C(254) | 0.081 (3) | 0.065 (2) | 0.036 (2) | 0.027 (2) | 0.0020 (19) | −0.0086 (17) |
C(255) | 0.060 (2) | 0.065 (2) | 0.041 (2) | 0.0182 (17) | 0.0071 (17) | −0.0016 (16) |
C(256) | 0.0421 (18) | 0.0519 (17) | 0.0339 (18) | 0.0121 (14) | 0.0012 (14) | −0.0052 (13) |
C(261) | 0.0276 (14) | 0.0314 (13) | 0.0247 (15) | 0.0064 (11) | 0.0035 (11) | −0.0028 (10) |
C(262) | 0.0328 (15) | 0.0403 (15) | 0.0282 (15) | 0.0005 (12) | 0.0007 (12) | −0.0028 (12) |
C(263) | 0.0505 (18) | 0.0409 (16) | 0.0391 (18) | −0.0051 (13) | 0.0069 (15) | 0.0025 (13) |
C(264) | 0.058 (2) | 0.0453 (17) | 0.0308 (17) | −0.0018 (14) | 0.0028 (15) | 0.0093 (13) |
C(265) | 0.0416 (17) | 0.0507 (17) | 0.0263 (16) | 0.0062 (13) | −0.0001 (13) | 0.0007 (13) |
C(266) | 0.0296 (15) | 0.0379 (14) | 0.0269 (15) | 0.0028 (11) | 0.0003 (12) | −0.0039 (11) |
C(321) | 0.0255 (14) | 0.0343 (14) | 0.0244 (15) | −0.0016 (11) | 0.0034 (11) | −0.0038 (11) |
C(322) | 0.0313 (15) | 0.0379 (14) | 0.0270 (15) | 0.0002 (11) | −0.0003 (12) | −0.0024 (11) |
C(323) | 0.0332 (16) | 0.0532 (18) | 0.0306 (16) | 0.0046 (13) | −0.0033 (13) | −0.0050 (13) |
C(324) | 0.0356 (17) | 0.0571 (19) | 0.0371 (18) | −0.0065 (14) | 0.0011 (14) | −0.0181 (14) |
C(325) | 0.0426 (18) | 0.0381 (15) | 0.0414 (18) | −0.0070 (13) | 0.0065 (14) | −0.0114 (13) |
C(326) | 0.0345 (16) | 0.0371 (14) | 0.0289 (16) | 0.0017 (12) | 0.0030 (13) | −0.0042 (11) |
C(331) | 0.0306 (15) | 0.0365 (15) | 0.0347 (17) | −0.0059 (12) | 0.0068 (13) | −0.0062 (12) |
C(332) | 0.0354 (17) | 0.0494 (17) | 0.046 (2) | 0.0032 (13) | 0.0054 (14) | −0.0078 (14) |
C(333) | 0.0425 (19) | 0.0540 (19) | 0.068 (3) | 0.0068 (15) | 0.0074 (18) | −0.0174 (17) |
C(334) | 0.048 (2) | 0.066 (2) | 0.066 (3) | −0.0054 (17) | 0.0221 (19) | −0.0296 (18) |
C(335) | 0.051 (2) | 0.069 (2) | 0.0380 (19) | −0.0110 (17) | 0.0132 (16) | −0.0176 (16) |
C(336) | 0.0397 (17) | 0.0471 (16) | 0.0360 (18) | −0.0044 (13) | 0.0064 (14) | −0.0084 (13) |
C(351) | 0.0271 (15) | 0.0424 (16) | 0.0304 (16) | −0.0005 (11) | 0.0023 (12) | −0.0069 (12) |
C(352) | 0.0334 (17) | 0.0562 (18) | 0.0429 (19) | −0.0044 (13) | −0.0063 (14) | 0.0013 (14) |
C(353) | 0.0374 (18) | 0.072 (2) | 0.045 (2) | 0.0026 (16) | −0.0138 (15) | −0.0022 (16) |
C(354) | 0.0300 (17) | 0.066 (2) | 0.056 (2) | −0.0058 (15) | −0.0039 (15) | −0.0207 (17) |
C(355) | 0.0440 (19) | 0.0437 (17) | 0.052 (2) | −0.0093 (14) | −0.0018 (16) | −0.0101 (14) |
C(356) | 0.0345 (16) | 0.0408 (16) | 0.0407 (18) | −0.0014 (12) | −0.0064 (13) | −0.0058 (13) |
C(361) | 0.0260 (14) | 0.0294 (13) | 0.0292 (15) | −0.0045 (11) | 0.0011 (11) | 0.0015 (11) |
C(362) | 0.0354 (16) | 0.0331 (14) | 0.0306 (16) | −0.0052 (12) | −0.0055 (12) | 0.0023 (11) |
C(363) | 0.0379 (17) | 0.0345 (15) | 0.0471 (19) | 0.0022 (12) | −0.0086 (14) | −0.0055 (13) |
C(364) | 0.0425 (18) | 0.0410 (16) | 0.047 (2) | 0.0048 (13) | −0.0004 (15) | −0.0135 (14) |
C(365) | 0.0442 (18) | 0.0449 (16) | 0.0305 (17) | −0.0011 (13) | −0.0040 (14) | −0.0040 (13) |
C(366) | 0.0316 (15) | 0.0335 (14) | 0.0258 (15) | 0.0002 (11) | −0.0022 (12) | 0.0019 (11) |
C(614) | 0.066 (3) | 0.210 (7) | 0.102 (5) | 0.033 (4) | 0.034 (3) | 0.017 (4) |
C(911) | 0.102 (4) | 0.081 (3) | 0.114 (4) | 0.002 (3) | −0.023 (3) | 0.017 (3) |
C(912) | 0.059 (3) | 0.128 (5) | 0.192 (8) | 0.034 (3) | −0.024 (4) | −0.070 (5) |
C(913) | 0.071 (4) | 0.265 (10) | 0.133 (6) | 0.048 (5) | 0.004 (4) | −0.109 (6) |
C(915) | 0.067 (3) | 0.083 (3) | 0.108 (4) | 0.011 (2) | 0.007 (3) | −0.002 (3) |
C(916) | 0.098 (3) | 0.086 (3) | 0.066 (3) | −0.001 (3) | 0.000 (3) | 0.008 (2) |
C(921) | 0.070 (3) | 0.065 (2) | 0.084 (3) | −0.0047 (19) | −0.016 (2) | −0.013 (2) |
C(922) | 0.105 (4) | 0.073 (3) | 0.051 (3) | 0.037 (2) | −0.012 (2) | −0.015 (2) |
C(923) | 0.091 (3) | 0.093 (3) | 0.071 (3) | 0.041 (3) | 0.029 (3) | 0.033 (3) |
C(924) | 0.058 (2) | 0.053 (2) | 0.099 (3) | 0.0009 (17) | −0.005 (2) | 0.015 (2) |
C(925) | 0.058 (2) | 0.068 (2) | 0.057 (2) | 0.0058 (18) | −0.0145 (19) | −0.0188 (18) |
C(926) | 0.060 (2) | 0.077 (2) | 0.063 (3) | −0.0033 (19) | 0.004 (2) | −0.004 (2) |
C(931) | 0.068 (3) | 0.061 (2) | 0.072 (3) | 0.0105 (19) | −0.011 (2) | 0.0161 (19) |
C(932) | 0.059 (2) | 0.051 (2) | 0.076 (3) | 0.0118 (17) | 0.011 (2) | 0.0184 (18) |
C(933) | 0.052 (2) | 0.0459 (19) | 0.083 (3) | 0.0036 (15) | 0.011 (2) | 0.0003 (18) |
C(934) | 0.069 (3) | 0.064 (2) | 0.064 (3) | 0.0094 (19) | 0.003 (2) | −0.0081 (19) |
C(935) | 0.073 (3) | 0.061 (2) | 0.074 (3) | −0.0016 (19) | 0.018 (2) | 0.012 (2) |
C(936) | 0.054 (2) | 0.060 (2) | 0.094 (3) | −0.0042 (17) | −0.004 (2) | 0.011 (2) |
C(941) | 0.102 (4) | 0.081 (3) | 0.077 (3) | 0.011 (3) | 0.029 (3) | 0.014 (2) |
C(942) | 0.056 (3) | 0.109 (4) | 0.087 (3) | 0.011 (2) | −0.006 (2) | 0.019 (3) |
C(943) | 0.075 (3) | 0.088 (3) | 0.081 (3) | −0.013 (2) | −0.003 (2) | −0.008 (2) |
C(944) | 0.086 (3) | 0.080 (3) | 0.065 (3) | 0.025 (2) | −0.004 (2) | −0.004 (2) |
C(945) | 0.058 (3) | 0.126 (4) | 0.061 (3) | 0.002 (3) | −0.010 (2) | −0.024 (3) |
C(946) | 0.099 (4) | 0.094 (3) | 0.071 (3) | −0.033 (3) | 0.028 (3) | −0.026 (2) |
Ag(1)—O(11) | 2.2654 (19) | C(221)—C(226) | 1.383 (4) |
Ag(1)—Ge | 2.4672 (3) | C(221)—C(222) | 1.399 (4) |
Ag(2)—C(222) | 2.522 (2) | C(222)—C(223) | 1.398 (4) |
Ag(2)—C(122) | 2.546 (2) | C(223)—C(224) | 1.393 (4) |
Ag(2)—C(322) | 2.552 (3) | C(224)—C(225) | 1.373 (4) |
Ge—O(2) | 1.8458 (16) | C(225)—C(226) | 1.393 (4) |
Ge—O(3) | 1.8467 (16) | C(231)—C(236) | 1.394 (4) |
Ge—O(1) | 1.8507 (16) | C(231)—C(232) | 1.394 (4) |
S(1)—O(12) | 1.429 (2) | C(232)—C(233) | 1.378 (4) |
S(1)—O(13) | 1.434 (2) | C(233)—C(234) | 1.379 (5) |
S(1)—O(11) | 1.450 (2) | C(234)—C(235) | 1.372 (4) |
S(1)—C(1) | 1.802 (4) | C(235)—C(236) | 1.381 (4) |
F(11)—C(1) | 1.338 (4) | C(251)—C(256) | 1.389 (4) |
F(12)—C(1) | 1.339 (4) | C(251)—C(252) | 1.395 (4) |
F(13)—C(1) | 1.339 (4) | C(252)—C(253) | 1.407 (4) |
O(1)—C(11) | 1.380 (3) | C(253)—C(254) | 1.378 (5) |
O(2)—C(21) | 1.378 (3) | C(254)—C(255) | 1.373 (5) |
O(3)—C(31) | 1.369 (3) | C(255)—C(256) | 1.383 (4) |
C(11)—C(16) | 1.403 (3) | C(261)—C(262) | 1.389 (3) |
C(11)—C(12) | 1.405 (3) | C(261)—C(266) | 1.403 (3) |
C(12)—C(13) | 1.400 (3) | C(262)—C(263) | 1.381 (4) |
C(12)—C(121) | 1.492 (3) | C(263)—C(264) | 1.385 (4) |
C(14)—C(15) | 1.384 (3) | C(264)—C(265) | 1.386 (4) |
C(14)—C(13) | 1.391 (3) | C(265)—C(266) | 1.380 (4) |
C(15)—C(16) | 1.415 (3) | C(321)—C(326) | 1.396 (3) |
C(15)—C(151) | 1.491 (3) | C(321)—C(322) | 1.401 (3) |
C(16)—C(161) | 1.493 (3) | C(322)—C(323) | 1.388 (4) |
C(21)—C(26) | 1.405 (3) | C(323)—C(324) | 1.386 (4) |
C(21)—C(22) | 1.407 (3) | C(324)—C(325) | 1.379 (4) |
C(22)—C(23) | 1.404 (3) | C(325)—C(326) | 1.381 (4) |
C(22)—C(221) | 1.498 (3) | C(331)—C(332) | 1.387 (4) |
C(23)—C(24) | 1.393 (4) | C(331)—C(336) | 1.391 (4) |
C(23)—C(231) | 1.487 (3) | C(332)—C(333) | 1.393 (4) |
C(24)—C(25) | 1.387 (4) | C(333)—C(334) | 1.370 (5) |
C(25)—C(26) | 1.404 (3) | C(334)—C(335) | 1.385 (4) |
C(25)—C(251) | 1.492 (4) | C(335)—C(336) | 1.386 (4) |
C(26)—C(261) | 1.488 (3) | C(351)—C(352) | 1.387 (4) |
C(31)—C(32) | 1.406 (3) | C(351)—C(356) | 1.387 (4) |
C(31)—C(36) | 1.415 (3) | C(352)—C(353) | 1.387 (4) |
C(32)—C(33) | 1.408 (3) | C(353)—C(354) | 1.376 (4) |
C(32)—C(321) | 1.491 (3) | C(354)—C(355) | 1.375 (4) |
C(33)—C(34) | 1.392 (3) | C(355)—C(356) | 1.387 (4) |
C(33)—C(331) | 1.490 (3) | C(361)—C(366) | 1.393 (3) |
C(34)—C(35) | 1.382 (3) | C(361)—C(362) | 1.396 (3) |
C(35)—C(36) | 1.405 (3) | C(362)—C(363) | 1.388 (4) |
C(35)—C(351) | 1.505 (3) | C(363)—C(364) | 1.384 (4) |
C(36)—C(361) | 1.489 (3) | C(364)—C(365) | 1.380 (4) |
C(121)—C(126) | 1.395 (3) | C(365)—C(366) | 1.391 (3) |
C(121)—C(122) | 1.395 (4) | C(614)—C(915) | 1.376 (7) |
C(122)—C(123) | 1.394 (4) | C(614)—C(913) | 1.386 (8) |
C(123)—C(124) | 1.389 (4) | C(911)—C(912) | 1.346 (7) |
C(124)—C(125) | 1.377 (4) | C(911)—C(916) | 1.362 (6) |
C(125)—C(126) | 1.385 (4) | C(912)—C(913) | 1.370 (9) |
C(131)—C(136) | 1.392 (4) | C(915)—C(916) | 1.343 (5) |
C(131)—C(132) | 1.401 (4) | C(921)—C(922) | 1.343 (5) |
C(131)—C(13) | 1.488 (3) | C(921)—C(926) | 1.360 (5) |
C(132)—C(133) | 1.378 (4) | C(922)—C(923) | 1.371 (6) |
C(133)—C(134) | 1.379 (5) | C(923)—C(924) | 1.400 (5) |
C(134)—C(135) | 1.375 (4) | C(924)—C(925) | 1.357 (5) |
C(135)—C(136) | 1.398 (4) | C(925)—C(926) | 1.352 (5) |
C(151)—C(156) | 1.388 (4) | C(931)—C(932) | 1.369 (5) |
C(151)—C(152) | 1.395 (4) | C(931)—C(936) | 1.386 (5) |
C(152)—C(153) | 1.385 (4) | C(932)—C(933) | 1.370 (5) |
C(153)—C(154) | 1.369 (4) | C(933)—C(934) | 1.377 (5) |
C(154)—C(155) | 1.376 (4) | C(934)—C(935) | 1.377 (5) |
C(155)—C(156) | 1.392 (4) | C(935)—C(936) | 1.365 (5) |
C(161)—C(166) | 1.392 (4) | C(941)—C(942) | 1.358 (6) |
C(161)—C(162) | 1.392 (4) | C(941)—C(946) | 1.375 (6) |
C(162)—C(163) | 1.391 (4) | C(942)—C(943) | 1.354 (5) |
C(163)—C(164) | 1.372 (4) | C(943)—C(944) | 1.371 (5) |
C(164)—C(165) | 1.370 (4) | C(944)—C(945) | 1.364 (6) |
C(165)—C(166) | 1.383 (4) | C(945)—C(946) | 1.362 (6) |
O(11)—Ag(1)—Ge | 169.03 (5) | C(166)—C(161)—C(162) | 118.3 (2) |
C(222)—Ag(2)—C(122) | 112.03 (9) | C(166)—C(161)—C(16) | 122.1 (2) |
C(222)—Ag(2)—C(322) | 115.17 (9) | C(162)—C(161)—C(16) | 119.6 (2) |
C(122)—Ag(2)—C(322) | 115.72 (8) | C(163)—C(162)—C(161) | 120.6 (3) |
O(2)—Ge—O(3) | 90.20 (7) | C(164)—C(163)—C(162) | 120.0 (3) |
O(2)—Ge—O(1) | 90.21 (7) | C(165)—C(164)—C(163) | 120.0 (3) |
O(3)—Ge—O(1) | 91.26 (7) | C(164)—C(165)—C(166) | 120.6 (3) |
O(2)—Ge—Ag(1) | 126.36 (5) | C(165)—C(166)—C(161) | 120.5 (3) |
O(3)—Ge—Ag(1) | 123.20 (5) | C(226)—C(221)—C(222) | 118.7 (3) |
O(1)—Ge—Ag(1) | 125.05 (5) | C(226)—C(221)—C(22) | 121.7 (2) |
O(12)—S(1)—O(13) | 116.91 (13) | C(222)—C(221)—C(22) | 119.5 (2) |
O(12)—S(1)—O(11) | 113.69 (13) | C(223)—C(222)—C(221) | 120.7 (3) |
O(13)—S(1)—O(11) | 114.37 (13) | C(223)—C(222)—Ag(2) | 84.55 (15) |
O(12)—S(1)—C(1) | 104.73 (15) | C(221)—C(222)—Ag(2) | 98.52 (16) |
O(13)—S(1)—C(1) | 102.95 (15) | C(224)—C(223)—C(222) | 119.8 (3) |
O(11)—S(1)—C(1) | 101.67 (14) | C(225)—C(224)—C(223) | 119.3 (3) |
C(11)—O(1)—Ge | 122.48 (15) | C(224)—C(225)—C(226) | 121.2 (3) |
C(21)—O(2)—Ge | 123.82 (14) | C(221)—C(226)—C(225) | 120.4 (3) |
C(31)—O(3)—Ge | 122.55 (14) | C(236)—C(231)—C(232) | 117.9 (3) |
S(1)—O(11)—Ag(1) | 137.01 (12) | C(236)—C(231)—C(23) | 123.2 (2) |
F(11)—C(1)—F(13) | 106.9 (3) | C(232)—C(231)—C(23) | 118.9 (2) |
F(11)—C(1)—F(12) | 106.7 (3) | C(233)—C(232)—C(231) | 121.2 (3) |
F(13)—C(1)—F(12) | 106.3 (3) | C(232)—C(233)—C(234) | 119.6 (3) |
F(11)—C(1)—S(1) | 112.3 (2) | C(235)—C(234)—C(233) | 120.4 (3) |
F(13)—C(1)—S(1) | 112.6 (2) | C(234)—C(235)—C(236) | 120.0 (3) |
F(12)—C(1)—S(1) | 111.6 (2) | C(235)—C(236)—C(231) | 120.8 (3) |
O(1)—C(11)—C(16) | 119.7 (2) | C(256)—C(251)—C(252) | 118.8 (3) |
O(1)—C(11)—C(12) | 118.3 (2) | C(256)—C(251)—C(25) | 121.8 (2) |
C(16)—C(11)—C(12) | 122.0 (2) | C(252)—C(251)—C(25) | 119.4 (3) |
C(13)—C(12)—C(11) | 118.8 (2) | C(251)—C(252)—C(253) | 120.2 (3) |
C(13)—C(12)—C(121) | 120.7 (2) | C(254)—C(253)—C(252) | 119.2 (3) |
C(11)—C(12)—C(121) | 120.5 (2) | C(255)—C(254)—C(253) | 120.9 (3) |
C(15)—C(14)—C(13) | 122.3 (2) | C(254)—C(255)—C(256) | 120.0 (3) |
C(14)—C(15)—C(16) | 119.4 (2) | C(255)—C(256)—C(251) | 120.9 (3) |
C(14)—C(15)—C(151) | 118.1 (2) | C(262)—C(261)—C(266) | 118.2 (2) |
C(16)—C(15)—C(151) | 122.4 (2) | C(262)—C(261)—C(26) | 120.2 (2) |
C(11)—C(16)—C(15) | 118.1 (2) | C(266)—C(261)—C(26) | 121.6 (2) |
C(11)—C(16)—C(161) | 120.1 (2) | C(263)—C(262)—C(261) | 120.8 (3) |
C(15)—C(16)—C(161) | 121.8 (2) | C(262)—C(263)—C(264) | 120.6 (3) |
O(2)—C(21)—C(26) | 119.7 (2) | C(263)—C(264)—C(265) | 119.4 (3) |
O(2)—C(21)—C(22) | 118.1 (2) | C(266)—C(265)—C(264) | 120.2 (3) |
C(26)—C(21)—C(22) | 122.2 (2) | C(265)—C(266)—C(261) | 120.8 (2) |
C(23)—C(22)—C(21) | 118.8 (2) | C(326)—C(321)—C(322) | 118.3 (2) |
C(23)—C(22)—C(221) | 121.2 (2) | C(326)—C(321)—C(32) | 120.2 (2) |
C(21)—C(22)—C(221) | 120.0 (2) | C(322)—C(321)—C(32) | 121.6 (2) |
C(24)—C(23)—C(22) | 118.3 (2) | C(323)—C(322)—C(321) | 120.5 (2) |
C(24)—C(23)—C(231) | 118.1 (2) | C(323)—C(322)—Ag(2) | 82.27 (16) |
C(22)—C(23)—C(231) | 123.6 (2) | C(321)—C(322)—Ag(2) | 102.33 (17) |
C(25)—C(24)—C(23) | 123.2 (2) | C(324)—C(323)—C(322) | 120.3 (3) |
C(24)—C(25)—C(26) | 119.1 (2) | C(325)—C(324)—C(323) | 119.7 (3) |
C(24)—C(25)—C(251) | 118.8 (2) | C(324)—C(325)—C(326) | 120.5 (3) |
C(26)—C(25)—C(251) | 122.1 (2) | C(325)—C(326)—C(321) | 120.8 (3) |
C(25)—C(26)—C(21) | 118.2 (2) | C(332)—C(331)—C(336) | 118.5 (3) |
C(25)—C(26)—C(261) | 121.7 (2) | C(332)—C(331)—C(33) | 119.9 (2) |
C(21)—C(26)—C(261) | 120.1 (2) | C(336)—C(331)—C(33) | 121.3 (2) |
O(3)—C(31)—C(32) | 117.8 (2) | C(331)—C(332)—C(333) | 120.5 (3) |
O(3)—C(31)—C(36) | 120.0 (2) | C(334)—C(333)—C(332) | 120.5 (3) |
C(32)—C(31)—C(36) | 122.2 (2) | C(333)—C(334)—C(335) | 119.7 (3) |
C(31)—C(32)—C(33) | 118.6 (2) | C(334)—C(335)—C(336) | 120.1 (3) |
C(31)—C(32)—C(321) | 119.6 (2) | C(335)—C(336)—C(331) | 120.8 (3) |
C(33)—C(32)—C(321) | 121.8 (2) | C(352)—C(351)—C(356) | 118.3 (2) |
C(34)—C(33)—C(32) | 118.7 (2) | C(352)—C(351)—C(35) | 121.0 (2) |
C(34)—C(33)—C(331) | 117.4 (2) | C(356)—C(351)—C(35) | 120.2 (2) |
C(32)—C(33)—C(331) | 123.8 (2) | C(353)—C(352)—C(351) | 120.7 (3) |
C(35)—C(34)—C(33) | 122.9 (2) | C(354)—C(353)—C(352) | 120.3 (3) |
C(34)—C(35)—C(36) | 119.7 (2) | C(355)—C(354)—C(353) | 119.7 (3) |
C(34)—C(35)—C(351) | 115.5 (2) | C(354)—C(355)—C(356) | 120.2 (3) |
C(36)—C(35)—C(351) | 124.5 (2) | C(351)—C(356)—C(355) | 120.8 (3) |
C(35)—C(36)—C(31) | 117.6 (2) | C(366)—C(361)—C(362) | 118.1 (2) |
C(35)—C(36)—C(361) | 121.9 (2) | C(366)—C(361)—C(36) | 122.0 (2) |
C(31)—C(36)—C(361) | 120.4 (2) | C(362)—C(361)—C(36) | 119.9 (2) |
C(126)—C(121)—C(122) | 118.6 (2) | C(363)—C(362)—C(361) | 121.4 (3) |
C(126)—C(121)—C(12) | 121.8 (2) | C(364)—C(363)—C(362) | 119.6 (3) |
C(122)—C(121)—C(12) | 119.5 (2) | C(365)—C(364)—C(363) | 120.0 (3) |
C(123)—C(122)—C(121) | 120.3 (3) | C(364)—C(365)—C(366) | 120.4 (3) |
C(123)—C(122)—Ag(2) | 85.11 (16) | C(365)—C(366)—C(361) | 120.6 (2) |
C(121)—C(122)—Ag(2) | 99.48 (16) | C(915)—C(614)—C(913) | 119.5 (6) |
C(124)—C(123)—C(122) | 120.2 (3) | C(912)—C(911)—C(916) | 120.9 (5) |
C(125)—C(124)—C(123) | 119.5 (3) | C(911)—C(912)—C(913) | 119.7 (6) |
C(124)—C(125)—C(126) | 120.7 (3) | C(912)—C(913)—C(614) | 119.5 (6) |
C(125)—C(126)—C(121) | 120.6 (3) | C(916)—C(915)—C(614) | 119.7 (5) |
C(136)—C(131)—C(132) | 118.1 (3) | C(915)—C(916)—C(911) | 120.6 (5) |
C(136)—C(131)—C(13) | 121.8 (2) | C(922)—C(921)—C(926) | 120.4 (4) |
C(132)—C(131)—C(13) | 120.1 (3) | C(921)—C(922)—C(923) | 120.3 (4) |
C(133)—C(132)—C(131) | 120.9 (3) | C(922)—C(923)—C(924) | 119.3 (4) |
C(132)—C(133)—C(134) | 120.6 (3) | C(925)—C(924)—C(923) | 118.8 (4) |
C(135)—C(134)—C(133) | 119.6 (3) | C(926)—C(925)—C(924) | 120.7 (4) |
C(134)—C(135)—C(136) | 120.4 (3) | C(925)—C(926)—C(921) | 120.5 (4) |
C(131)—C(136)—C(135) | 120.4 (3) | C(932)—C(931)—C(936) | 119.6 (4) |
C(14)—C(13)—C(12) | 119.2 (2) | C(933)—C(932)—C(931) | 120.3 (4) |
C(14)—C(13)—C(131) | 118.2 (2) | C(932)—C(933)—C(934) | 120.0 (3) |
C(12)—C(13)—C(131) | 122.6 (2) | C(935)—C(934)—C(933) | 120.0 (4) |
C(156)—C(151)—C(152) | 118.2 (2) | C(936)—C(935)—C(934) | 119.9 (4) |
C(156)—C(151)—C(15) | 120.5 (2) | C(935)—C(936)—C(931) | 120.3 (4) |
C(152)—C(151)—C(15) | 121.2 (2) | C(942)—C(941)—C(946) | 119.2 (4) |
C(153)—C(152)—C(151) | 120.5 (3) | C(943)—C(942)—C(941) | 121.3 (4) |
C(154)—C(153)—C(152) | 120.7 (3) | C(942)—C(943)—C(944) | 119.8 (4) |
C(153)—C(154)—C(155) | 119.7 (3) | C(945)—C(944)—C(943) | 119.3 (4) |
C(154)—C(155)—C(156) | 120.2 (3) | C(946)—C(945)—C(944) | 120.9 (4) |
C(151)—C(156)—C(155) | 120.7 (3) | C(945)—C(946)—C(941) | 119.6 (4) |
Experimental details
Crystal data | |
Chemical formula | [Ag2Ge(CF3O3S)(C45H29O)3]·4C6H6 |
Mr | 1942.36 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 150 |
a, b, c (Å) | 13.9593 (2), 24.3433 (3), 26.9406 (4) |
β (°) | 92.1511 (5) |
V (Å3) | 9148.4 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.83 |
Crystal size (mm) | 0.30 × 0.30 × 0.25 |
Data collection | |
Diffractometer | Nonius KappaCCD diffractometer |
Absorption correction | Empirical (using intensity measurements) |
Tmin, Tmax | 0.574, 0.814 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 63826, 21443, 15451 |
Rint | 0.060 |
(sin θ/λ)max (Å−1) | 0.658 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.074, 0.91 |
No. of reflections | 21401 |
No. of parameters | 1153 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.38, −0.67 |
Computer programs: COLLECT (Nonius, 1998), DENZO and SCALEPACK (Otwinowski & Minor, 1997), DENZO and SCALEPACK, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976) and PLUTON (Spek, 1991), CIF VAX in MolEN (Fair, 1990).
Ag(1)—O(11) | 2.2654 (19) | S(1)—O(13) | 1.434 (2) |
Ag(1)—Ge | 2.4672 (3) | S(1)—O(11) | 1.450 (2) |
Ag(2)—C(222) | 2.522 (2) | S(1)—C(1) | 1.802 (4) |
Ag(2)—C(122) | 2.546 (2) | F(11)—C(1) | 1.338 (4) |
Ag(2)—C(322) | 2.552 (3) | F(12)—C(1) | 1.339 (4) |
Ge—O(2) | 1.8458 (16) | F(13)—C(1) | 1.339 (4) |
Ge—O(3) | 1.8467 (16) | O(1)—C(11) | 1.380 (3) |
Ge—O(1) | 1.8507 (16) | O(2)—C(21) | 1.378 (3) |
S(1)—O(12) | 1.429 (2) | O(3)—C(31) | 1.369 (3) |
O(11)—Ag(1)—Ge | 169.03 (5) | O(13)—S(1)—C(1) | 102.95 (15) |
C(222)—Ag(2)—C(122) | 112.03 (9) | O(11)—S(1)—C(1) | 101.67 (14) |
C(222)—Ag(2)—C(322) | 115.17 (9) | C(11)—O(1)—Ge | 122.48 (15) |
C(122)—Ag(2)—C(322) | 115.72 (8) | C(21)—O(2)—Ge | 123.82 (14) |
O(2)—Ge—O(3) | 90.20 (7) | C(31)—O(3)—Ge | 122.55 (14) |
O(2)—Ge—O(1) | 90.21 (7) | S(1)—O(11)—Ag(1) | 137.01 (12) |
O(3)—Ge—O(1) | 91.26 (7) | F(11)—C(1)—F(13) | 106.9 (3) |
O(2)—Ge—Ag(1) | 126.36 (5) | F(11)—C(1)—F(12) | 106.7 (3) |
O(3)—Ge—Ag(1) | 123.20 (5) | F(13)—C(1)—F(12) | 106.3 (3) |
O(1)—Ge—Ag(1) | 125.05 (5) | F(11)—C(1)—S(1) | 112.3 (2) |
O(12)—S(1)—O(13) | 116.91 (13) | F(13)—C(1)—S(1) | 112.6 (2) |
O(12)—S(1)—O(11) | 113.69 (13) | F(12)—C(1)—S(1) | 111.6 (2) |
O(13)—S(1)—O(11) | 114.37 (13) | O(1)—C(11)—C(16) | 119.7 (2) |
O(12)—S(1)—C(1) | 104.73 (15) | O(1)—C(11)—C(12) | 118.3 (2) |
The title compound, (I), was isolated from the reaction of [Ge(OC6HPh4-2,3,5,6)2] with Ph3Ge(OSO2CF3). The Ag atoms undoubtedly result from residual silver in the preparation of Ph3Ge(OSO2CF3) using Ph3GeCl and Ag(OSO2CF3). These complications can be circumvented by the use of triflic acid in place of silver trifluoromethanesulfonate (Uhlig, 1991a,b). The reaction mixture also consisted of an intractable mixture of products, from which only (I) could be isolated and characterized.
Compound (I) contains a four-coordinate GeII metal center consisting of a [Ge(OC6HPh4-2,3,5,6)3]− anion with a coordinated Ag(OSO2CF3) group and an Ag+ cation (Fig. 1). The complex cocrystallizes with four molecules of benzene. The average Ge—O bond length of 1.848 (2) Å is a typical value. The Ge—Ag bond for the coordinated silver trifluoromethanesulfonate is 2.4672 (3) Å. To date, compound (I) represents one of three discrete molecular compounds containing a Ge—-Ag bond. The complexes [HB(3,5-(CF3)2Pz)3]AgGeCl[(Me)2ATl], (II), and [HB(3,5-(CF3)2Pz)3]AgGe(OSO2CF3)[(Me)2ATl], (III) {[HB(3,5-(CF3)2Pz] is hydrotris[3,5-bis(trifluoromethyl)pyrazolyl]borate and [(Me)2ATl] is N-methyl-2-(methylamino)troponiminate}, have been reported (Rasika Dias & Wang, 2000). Both of these species exhibit Ge—Ag distances similar to (I); the Ge–Ag distance is 2.4215 (9) Å for (II) and 2.412 (1) Å for (III). Complex (III) also contains a trifluoromethanesulfonate anion that is bound to the Ge metal center, rather than to the Ag atom as in (I). Other GeII/MI compounds (where MI is a group 11 metal) have been structurally characterized. These contain GeII bound to CuI (Orlov et al., 1997; Orlov et al., 1998) and AuI metal centers (Bauer et al., 1995, 1997; Bauer & Schmidbaur, 1996, 1997; Contel et al., 1996; Tripathi et al., 1998).
The AgI cation of compound (I) is encapsulated by the O atoms of the three tetraphenylphenoxide ligands. The average Ag—O distance is 2.631 (3) Å. There are also short Ag–C contacts of 2.522 (2), 2.536 (2) and 2.522 (3) Å with three of the ortho-C atoms of the phenyl rings of the tetraphenylphenoxide ligands. These contacts arise from interaction of the Ag atom with the pπ electrons of the aromatic rings. Thus, the AgI cation is in a six-coordinate environment.