A germanium–silver complex containing aGe—Ag bond, Ag[Ge(OC6HPh4-2,3,5,6)3(AgOSO2CF3)]·4C6H6

Weinert, C.S.; Fanwick, P.E.; Rothwell, I.P.

doi:10.1107/S1600536802020585

A germanium–silver complex containing aGe—Ag bond, Ag[Ge(OC₆HPh₄-2,3,5,6)₃(AgOSO₂CF₃)]·4C₆H₆

C. S. Weinert, P. E. Fanwick and I. P. Rothwell

The title compound, tris[μ-2,3,5,6-tetraphenylphenoxy(1−)-1:3κ²O,1κC²](trifluoromethylsulfonato-2κO)disilvergermanium(Ag—Ge) benzene tetrasolvate, Ag[Ge(OC₆HPh₄-2,3,5,6)₃(AgOSO₂CF₃)]·4C₆H₆ or [Ag₂Ge(CF₃O₃S)(C₃₀H₂₁O)₃]·4C₆H₆, is a rare example of a compound containing a Ge^II—Ag^I bond. The anion consists of a Ge atom bound to three tetraphenylphenoxide ligands and to a molecule of silver trifluoromethanesulfonate. The Ag^I counter-ion is encapsulated by the three O atoms of the tetraphenylphenoxide ligands and exhibits π-interactions with the ortho-phenyl rings of these ligands.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802020585/mg6018sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536802020585/mg6018Isup2.hkl Contains datablock I

CCDC reference: 202285

checkCIF report

Key indicators

Single-crystal X-ray study
T = 150 K
Mean (C-C) = 0.004 Å
R factor = 0.039
wR factor = 0.074
Data-to-parameter ratio = 18.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level B:



ABSTM_02  Alert B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
          Tmin and Tmax reported:      0.574     0.814
          Tmin' and Tmax expected:      0.775     0.814
          RR' =      0.740
          Please check that your absorption correction is appropriate.


 Alert Level C:



ABSMU_01  Alert C The ratio of given/expected absorption coefficient lies
          outside the range 0.99 <> 1.01
          Calculated value of mu =     0.838
          Value of mu given      =     0.825

ABSTY_02  Alert C An _exptl_absorpt_correction_type has been given without
          a literature citation. This should be contained in the
          _exptl_absorpt_process_details field.
          Absorption correction given as empirical

General Notes



REFLT_03
         From the CIF: _diffrn_reflns_theta_max           27.90
         From the CIF: _reflns_number_total              21443
         From the CIF: _diffrn_reflns_limit_ max hkl   18.   30.   35.
         From the CIF: _diffrn_reflns_limit_ min hkl    0.    0.  -35.
         TEST1: Expected hkl limits for theta max
         Calculated maximum hkl   18.   32.   35.
         Calculated minimum hkl  -18.  -32.  -35.
          ALERT: Expected hkl max differ from CIF values


 0 Alert Level A = Potentially serious problem

 1 Alert Level B = Potential problem

 2 Alert Level C = Please check

Comment top

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 Ge^II 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 Ge^II/M^I compounds (where M^I is a group 11 metal) have been structurally characterized. These contain Ge^II bound to Cu^I (Orlov et al., 1997; Orlov et al., 1998) and Au^I metal centers (Bauer et al., 1995, 1997; Bauer & Schmidbaur, 1996, 1997; Contel et al., 1996; Tripathi et al., 1998).

The Ag^I 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 Ag^I cation is in a six-coordinate environment.

Experimental top

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.

Computing details top

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).

Figures top

Fig. 1. ORTEP plot highlighting the environment about the silver cation of (I). Displacement ellipsoids are drawn at the 50% probability level.

tris[µ-2,6-diphenylphenoxy(1-)-1:3κ²O,1κC²](trifluoromethylsulfonato- 2κO)disilvergermanium (Ag–Ge) tetrabenzene solvate top

Crystal data top

[Ag₂Ge(CF₃O₃S)(C₄₅H₂₉O)₃]·4C₆H₆	F(000) = 3976
M_r = 1942.36	D_x = 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

Data collection top

Nonius KappaCCD diffractometer	15451 reflections with I > 2σ(I)
ω scans	R_int = 0.060
Absorption correction: empirical (using intensity measurements) ?	θ_max = 27.9°, θ_min = 2.1°
T_min = 0.574, T_max = 0.814	h = 0→18
63826 measured reflections	k = 0→30
21443 independent reflections	l = −35→35

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.039	w = 1/[σ²(F_o²) + (0.0352P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.074	(Δ/σ)_max = 0.003
S = 0.91	Δρ_max = 0.38 e Å⁻³
21401 reflections	Δρ_min = −0.67 e Å⁻³
1153 parameters

Crystal data top

[Ag₂Ge(CF₃O₃S)(C₄₅H₂₉O)₃]·4C₆H₆	V = 9148.4 (4) Å³
M_r = 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)°

Data collection top

Nonius KappaCCD diffractometer	21443 independent reflections
Absorption correction: empirical (using intensity measurements) ?	15451 reflections with I > 2σ(I)
T_min = 0.574, T_max = 0.814	R_int = 0.060
63826 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.039	0 restraints
wR(F²) = 0.074	H-atom parameters constrained
S = 0.91	Δρ_max = 0.38 e Å⁻³
21401 reflections	Δρ_min = −0.67 e Å⁻³
1153 parameters

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

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
M_r	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)
T_min, T_max	0.574, 0.814
No. of measured, independent and observed [I > 2σ(I)] reflections	63826, 21443, 15451
R_int	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
Δρ_max, Δρ_min (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).

Selected geometric parameters (Å, º) top

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)

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
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Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

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