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The title compound, cis-di-μ-perfluoro­heptan­oato-κ4O:O′-bis[dicarbonyl(dimethyl sulfoxide-κS)ruthenium(I)](RuRu), [Ru2(C7F13O2)2(C2H6OS)2(CO)4], is a sawhorse-type di­nuclear ruthenium complex with two bridging perfluoro­heptan­oate ligands, and with two dimethyl sulfoxide (DMSO) ligands in the axial positions coordinating via the S atoms. It is a new example of a compound with an aliphatic fluorinated carboxyl­ate ligand. The Ru—Ru bond distance of 2.6908 (3) Å indicates a direct Ru—Ru inter­action. The com­pound is an active catalyst in transvinyl­ation of propionic acid with vinyl acetate.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229614006354/eg3153sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229614006354/eg3153Isup2.hkl
Contains datablock I

CCDC reference: 993034

Introduction top

Ruthenium(I) sawhorse-type complexes of the general composition [Ru2(µ,η2-RCOO)2L2(CO)4] (RCOO- is a carboxyl­ate ligand and L is a donor ligand) have been known since the 1960s (Crooks et al., 1969). Established applications of these compounds include catalysis of alkene isomerization (Salvini et al., 2000) and hydrogenation reactions (Johnpeter et al., 2013; Salvini et al., 2003, 2005), as well as the synthesis of molecular cages and macrocycles (Shiu et al., 2002; Süss-Fink et al., 1990; Auzias et al., 2007). In addition, carboxyl­ate-bridged Ru2(CO)4 complexes derived from biologically active acids have been employed in cytotoxicity studies (Auzias et al., 2006, 2009). The common synthetic route to complexes of this type entails refluxing Ru3(CO)12 with the respective carb­oxy­lic acid to form polymeric [Ru(CO)2(RCOO)]n, which may be broken down to the typical dimeric structure upon addition of a donor ligand such as tetra­hydro­furan (THF), phosphines, carb­oxy­lic acids etc. (Crooks et al., 1969; Auzias et al., 2009; Therrien & Süss-Fink, 2009). The title compound [Ru2{µ,η2-CF3(CF2)5COO}2(DMSO)2(CO)4], (I), was synthesized according to this route in 80% yield.

Experimental top

Synthesis and crystallization top

Ru3(CO)12 (50 mg, 0.08 mmol, 0.33 equivalents) and perfluoro­heptanoic acid (171 mg, 0.24 mmol, 1.0 equivalent) were dissolved in toluene (2 ml) and stirred for 12 h at 373 K in a Schlenk tube. The red solution was concentrated in vacuo to give a dark-red oil. Di­methyl sulfoxide (DMSO) (2.5 ml) was added and the resulting yellow precipitate was separated from excess DMSO, washed with pentane (3 × 3 ml) and dried in vacuo to yield 114 mg (80%) of (I). Recrystallization from hot nitro­methane and storage at 277 K for several weeks yielded crystals suitable for single-crystal X-ray diffraction. A selected crystal was fixed on the top of a glass fibre using perfluorinated ether and transferred to the diffractometer.

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. H atoms could not be located in difference Fourier maps and were calculated in ideal positions (riding model), with C—H = 0.98 Å and Uiso(H) = 1.5Ueq(C) for methyl groups. Split-layer position refinement was used for fluorinated atoms C5 and C6 and the corresponding F atoms, and for atoms F11, F12 and F13 connected to C7. Restraints were applied to the C4—C5, C4—C5A, C5—C6, C5A—C6A, C6—C7 and C6A—C7 bonds to ensure similar bond lengths within the disordered part of the fluorinated side chain.

Comment top

In the title binuclear sawhorse-type complex, (I) (Scheme 1 and Fig. 1), both RuI centres are coordinated in a distorted o­cta­hedral geometry and the axial positions along the Ru—Ru axis are occupied by two di­methyl sulfoxide (DMSO) molecules coordinating via the S atoms. The DMSO ligands are tilted towards one another and oriented away from the carbonyl groups, with Ru2—Ru1—S1 and Ru1—Ru2—S2 bond angles well below 180° at 165.14 (2) and 164.70 (2)°, respectively, resulting in a bent geometry of the central part of the complex. This was also observed for the only other carboxyl­ate-bridged Ru—Ru dinuclear complex with DMSO in the axial position (Ziriakus et al., 2013) and for structurally similar complexes with axial N-donor ligands (Dorta et al., 2004; Kepert et al., 2000, 2003). The Ru—Ru bond distance is 2.6908 (3) Å, supporting both a direct Ru—Ru inter­action and the formal oxidation state +I for both Ru atoms. The perfluoro­heptanoate ligands are slightly twisted with respect to the Ru—Ru axis (by approximately 15°), which is illustrated by the O1—Ru1—Ru2—O2 and O3—Ru1—Ru2—O4 torsion angles (see Table 2). The O1—Ru1—O3 and O2—Ru2—O4 bond angles of 81.59 (6) and 81.57 (7)°, respectively, highlight the contorted distribution of the ligands around the Ru centres, with both carboxyl­ate ligands in close proximity to one another. This is also reflected in the O2—Ru2—C18 [97.20 (10)°] and O3—Ru1—C15 [96.76 (10)°] bond angles, which are well above the ideal value of 90°.

A view of the three-dimensional packing of the unit cell is given in Fig. 2. In a multilamellar assembly of bilayers, the fluorinated aliphatic chains form lipophilic layers inter­sected by more hydro­philic sheets of the central Ru2(DMSO)2(CO)4 scaffolds. These planar structures are oriented parallel to the ab plane. Single molecules are connected via the terminal DMSO ligands, which show weak inter­action with the CH3, CF2 and CO groups of neighbouring molecules to form an alternating chain structure.

A recent study from our group reports on the relevance of ruthenium carbonyl carboxyl­ates for transvinyl­ation (Ziriakus et al., 2013). Even though dinuclear sawhorse-type Ru complexes were found to exhibit mediocre activity compared with mononuclear compounds, a change in activity due to the electronic effect of the fluorination of the bridging carboxyl­ate ligands may be anti­cipated. Thus, complex (I) was tested for activity in transvinyl­ation catalysis and compared with the previously reported activities of other ruthenium carbonyl carboxyl­ates from Ziriakus et al. (2013). For the sake of comparison, the same conditions were applied; 0.3 mol% of (I) was used in a model catalytic system, with propionic acid and vinyl acetate as model substrates (Scheme 2). The results of the catalytic investigation of (I) are depicted in Fig. 3.

It is evident that (I) exhibits a slightly higher activity (TOF = 36.3 h-1 and TON4h = 113) in transvinyl­ation catalysis compared with the structurally analogous complex (III) (TOF = 29.1 h-1 and TON4h = 70.9), indicating a beneficial effect of bridging perfluoro­heptanoate over bridging propionate ligands. The activity of (I) is similar to that of (IV) (TOF = 38.5 h-1 and TON4h = 105), but lower than that of (II) (TOF = 153 h-1 and TON4h = 205), which is the most active transvinyl­ation catalyst to date in this model system (see Ziriakus et al., 2013).

Related literature top

For related literature, see: Auzias et al. (2006, 2007, 2009); Crooks et al. (1969); Dorta et al. (2004); Johnpeter et al. (2013); Kepert et al. (2000, 2003); Süss-Fink, Neumann, Frank & Stoeckli-Evans (1990); Salvini et al. (2000, 2003, 2005); Shiu et al. (2002); Ziriakus et al. (2013).

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) and SHELXLE (Hübschle et al., 2011); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: PLATON (Spek, 2009) and enCIFer (Allen et al., 2004).

Figures top
[Figure 1] Fig. 1. A perspective view of (I), showing the atom-numbering scheme. H atoms have been omitted for clarity. Displacement ellipsoids are drawn at the 50% probability level.
[Figure 2] Fig. 2. The crystal packing of (I), highlighting the layered arrangement in the crystal structure. The view is along the a axis.
[Figure 3] Fig. 3. The catalytic activity of (I) compared with the recently investigated complexes (II), (III) and (IV) (see Ziriakus et al., 2013).
Di-µ-perfluoroheptanoato-κ4O:O'-bis[dicarbonyl(dimethyl sulfoxide-κS)ruthenium(I)](RuRu) top
Crystal data top
[Ru2(C7F13O2)2(C2H6OS)2(CO)4]Z = 4
Mr = 1196.60F(000) = 2312
Triclinic, P1Dx = 2.194 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.3430 (5) ÅCell parameters from 9908 reflections
b = 14.1199 (8) Åθ = 2.4–25.4°
c = 25.3010 (13) ŵ = 1.13 mm1
α = 101.243 (3)°T = 123 K
β = 90.478 (2)°Plate, yellow
γ = 90.830 (2)°0.34 × 0.29 × 0.09 mm
V = 3623.5 (3) Å3
Data collection top
Bruker APEXII CCD area-detector
diffractometer
13225 independent reflections
Radiation source: rotating anode FR59111061 reflections with I > 2σ(I)
MONTEL optic monochromatorRint = 0.038
Detector resolution: 16 pixels mm-1θmax = 25.5°, θmin = 0.8°
ϕ and ω rotation scansh = 1212
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
k = 1717
Tmin = 0.703, Tmax = 0.901l = 3030
86914 measured reflections
Refinement top
Refinement on F224 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H-atom parameters constrained
wR(F2) = 0.053 W = 1/[Σ2(FO2) + (0.017P)2 + 4.1637P] WHERE P = (FO2 + 2FC2)/3
S = 1.04(Δ/σ)max = 0.003
13225 reflectionsΔρmax = 0.73 e Å3
1225 parametersΔρmin = 0.48 e Å3
Crystal data top
[Ru2(C7F13O2)2(C2H6OS)2(CO)4]γ = 90.830 (2)°
Mr = 1196.60V = 3623.5 (3) Å3
Triclinic, P1Z = 4
a = 10.3430 (5) ÅMo Kα radiation
b = 14.1199 (8) ŵ = 1.13 mm1
c = 25.3010 (13) ÅT = 123 K
α = 101.243 (3)°0.34 × 0.29 × 0.09 mm
β = 90.478 (2)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer
13225 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2008)
11061 reflections with I > 2σ(I)
Tmin = 0.703, Tmax = 0.901Rint = 0.038
86914 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02624 restraints
wR(F2) = 0.053H-atom parameters constrained
S = 1.04Δρmax = 0.73 e Å3
13225 reflectionsΔρmin = 0.48 e Å3
1225 parameters
Special details top

Experimental. Diffractometer operator: S. Haslinger; scanspeed: 10 s per frame; dx: 50 mm; 4781 frames measured in 13 data sets; phi-scans with delta_phi = 0.5; omega-scans with delta_omega = 0.5

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement on F2 for ALL reflections except those 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 > 2sigma(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
xyzUiso*/UeqOcc. (<1)
Ru10.60216 (2)0.58258 (2)0.12074 (2)0.0127 (1)
Ru20.64672 (2)0.39401 (2)0.11657 (2)0.0122 (1)
S10.56564 (6)0.75348 (5)0.14932 (3)0.0179 (2)
S20.68802 (6)0.23862 (4)0.13857 (3)0.0159 (2)
F10.26700 (14)0.50776 (12)0.24491 (6)0.0297 (5)
F5_a0.2817 (5)0.5917 (4)0.3605 (3)0.0310 (14)0.628 (8)
F20.41797 (16)0.43090 (11)0.27899 (6)0.0278 (5)
F6_a0.4706 (6)0.5327 (3)0.3734 (5)0.0292 (16)0.628 (8)
F30.37259 (15)0.67473 (10)0.27848 (6)0.0267 (5)
F7_a0.4076 (5)0.6868 (2)0.44466 (13)0.0322 (13)0.628 (8)
F40.56105 (14)0.61608 (11)0.29221 (6)0.0248 (5)
F8_a0.5782 (4)0.7042 (3)0.39778 (19)0.0319 (15)0.628 (8)
F9_a0.4685 (15)0.8273 (10)0.3489 (8)0.038 (3)0.628 (8)
F10_a0.2751 (5)0.7906 (4)0.37161 (18)0.0407 (16)0.628 (8)
F11_a0.3258 (6)0.8671 (5)0.4740 (3)0.062 (2)0.628 (8)
F12_a0.5273 (4)0.8850 (3)0.45917 (15)0.0478 (14)0.628 (8)
F13_a0.3831 (7)0.9637 (3)0.42456 (19)0.068 (2)0.628 (8)
F141.00533 (14)0.54337 (11)0.23500 (6)0.0226 (5)
F150.86255 (15)0.64368 (10)0.27606 (6)0.0234 (5)
F160.72683 (14)0.46325 (11)0.29010 (6)0.0225 (5)
F170.91623 (15)0.39990 (10)0.27240 (6)0.0242 (5)
F180.81325 (16)0.58954 (11)0.37173 (6)0.0293 (6)
F191.01409 (16)0.56885 (13)0.34746 (7)0.0352 (6)
F201.02140 (16)0.39698 (14)0.37010 (7)0.0417 (7)
F210.94700 (18)0.50438 (13)0.43611 (7)0.0404 (7)
F220.69452 (16)0.43283 (12)0.39924 (7)0.0328 (6)
F230.79316 (18)0.31420 (12)0.34837 (6)0.0363 (6)
F240.8010 (2)0.39196 (13)0.48775 (7)0.0501 (7)
F250.7261 (2)0.26216 (13)0.43748 (8)0.0511 (8)
F260.9311 (2)0.29041 (14)0.44228 (8)0.0516 (8)
O10.45599 (16)0.56635 (12)0.17825 (7)0.0161 (6)
O20.53618 (16)0.42348 (12)0.18871 (7)0.0145 (5)
O30.72314 (16)0.59471 (12)0.19014 (7)0.0149 (5)
O40.80192 (16)0.44397 (12)0.17269 (7)0.0163 (6)
O50.81244 (19)0.59689 (14)0.04123 (8)0.0295 (7)
O60.82802 (19)0.36050 (14)0.02313 (8)0.0269 (7)
O70.40063 (18)0.55926 (14)0.03337 (7)0.0243 (7)
O80.42844 (18)0.33223 (14)0.03798 (8)0.0267 (7)
O90.43004 (17)0.78509 (13)0.15173 (8)0.0272 (7)
O100.82475 (17)0.20993 (13)0.14008 (8)0.0252 (6)
C10.4699 (2)0.49679 (18)0.20175 (10)0.0143 (8)
C5_a0.4482 (5)0.7009 (3)0.39626 (17)0.0200 (17)0.628 (8)
C20.3955 (2)0.50655 (17)0.25538 (11)0.0184 (8)
C6_a0.3983 (8)0.8003 (6)0.3881 (3)0.031 (3)0.628 (8)
C30.4322 (2)0.60135 (19)0.29515 (11)0.0180 (8)
C40.3989 (3)0.6056 (2)0.35480 (12)0.0258 (10)
C70.4160 (4)0.8799 (2)0.43693 (14)0.0427 (14)
C80.7929 (2)0.52813 (18)0.19907 (10)0.0143 (8)
C90.8796 (2)0.55198 (18)0.25015 (11)0.0169 (8)
C100.8550 (2)0.48343 (18)0.29027 (10)0.0168 (8)
C110.8985 (3)0.5238 (2)0.34888 (11)0.0215 (9)
C120.9181 (3)0.4503 (2)0.38693 (11)0.0269 (10)
C130.8044 (3)0.3824 (2)0.39324 (12)0.0266 (10)
C140.8165 (4)0.3308 (2)0.44152 (13)0.0379 (11)
C150.7335 (3)0.59113 (19)0.07179 (11)0.0192 (9)
C160.7565 (3)0.37436 (18)0.05813 (11)0.0174 (9)
C170.4810 (3)0.56787 (18)0.06541 (11)0.0170 (8)
C180.5095 (3)0.35627 (18)0.06906 (11)0.0167 (8)
C190.6536 (3)0.8229 (2)0.11006 (15)0.0439 (13)
C200.6392 (3)0.7975 (2)0.21298 (13)0.0350 (11)
C210.6001 (3)0.14406 (19)0.09581 (13)0.0330 (10)
C220.6163 (3)0.2312 (2)0.20082 (12)0.0308 (11)
F8A_b0.2484 (7)0.7408 (7)0.3679 (3)0.038 (3)0.372 (8)
F9A_b0.5670 (7)0.7473 (7)0.4160 (4)0.042 (3)0.372 (8)
F10A_b0.491 (2)0.8055 (16)0.3492 (12)0.038 (5)0.372 (8)
F11A_b0.3899 (13)0.8625 (8)0.4838 (4)0.063 (4)0.372 (8)
F12A_b0.5264 (7)0.9367 (7)0.4407 (4)0.074 (3)0.372 (8)
F13A_b0.3320 (9)0.9220 (7)0.4152 (4)0.066 (3)0.372 (8)
C5A_b0.3558 (11)0.7065 (4)0.3890 (3)0.033 (4)0.372 (8)
C6A_b0.4572 (14)0.7817 (9)0.3953 (5)0.034 (4)0.372 (8)
F7A_b0.3263 (10)0.6867 (5)0.4374 (3)0.046 (3)0.372 (8)
F5A_b0.2711 (8)0.5523 (6)0.3523 (5)0.030 (3)0.372 (8)
F6A_b0.4748 (8)0.5635 (6)0.3763 (8)0.025 (3)0.372 (8)
Ru31.14814 (2)0.07387 (2)0.11504 (2)0.0118 (1)
Ru41.11084 (2)0.11282 (2)0.12081 (2)0.0123 (1)
S31.18730 (6)0.24686 (4)0.13675 (3)0.0148 (2)
S41.07349 (6)0.26119 (4)0.15343 (3)0.0155 (2)
F270.76121 (14)0.04046 (11)0.23580 (6)0.0259 (5)
F280.90667 (15)0.14613 (10)0.27437 (6)0.0269 (5)
F290.86243 (15)0.09899 (10)0.27480 (6)0.0234 (5)
F301.04475 (14)0.02140 (11)0.29587 (6)0.0231 (5)
F310.94656 (19)0.09898 (12)0.37466 (7)0.0395 (6)
F320.74883 (17)0.06624 (13)0.34568 (7)0.0420 (7)
F330.74842 (17)0.10568 (14)0.36849 (7)0.0421 (7)
F340.8105 (2)0.00699 (14)0.43595 (7)0.0483 (7)
F350.98641 (18)0.17171 (13)0.35359 (7)0.0398 (7)
F361.06813 (18)0.04878 (14)0.40987 (7)0.0449 (7)
F371.0422 (2)0.22266 (18)0.44463 (9)0.0710 (10)
F380.8373 (2)0.21276 (14)0.43900 (8)0.0560 (8)
F390.9453 (2)0.10335 (15)0.49203 (7)0.0633 (9)
F401.34747 (15)0.03819 (10)0.28313 (6)0.0234 (5)
F411.49772 (14)0.03320 (10)0.24442 (6)0.0234 (5)
F421.38693 (15)0.20034 (10)0.26741 (6)0.0221 (5)
F431.19998 (14)0.13640 (10)0.28134 (6)0.0219 (5)
F441.27356 (16)0.09557 (11)0.37188 (6)0.0294 (6)
F451.47816 (15)0.11555 (11)0.35620 (6)0.0308 (6)
F461.25369 (16)0.29611 (11)0.35424 (6)0.0285 (5)
F471.46200 (16)0.30010 (11)0.36740 (6)0.0313 (6)
F481.20619 (18)0.24864 (13)0.44652 (7)0.0411 (7)
F491.40812 (19)0.21463 (13)0.45933 (7)0.0429 (7)
F501.3125 (2)0.38584 (13)0.51804 (7)0.0486 (7)
F511.2894 (2)0.43735 (13)0.44387 (7)0.0545 (8)
F521.4769 (2)0.40003 (15)0.46927 (8)0.0601 (8)
O111.03706 (16)0.09262 (12)0.18707 (7)0.0141 (5)
O120.96046 (16)0.06006 (12)0.17643 (7)0.0164 (6)
O131.30604 (16)0.06924 (12)0.17059 (7)0.0159 (6)
O141.22650 (16)0.06841 (11)0.19155 (7)0.0139 (5)
O151.31790 (18)0.04632 (14)0.01768 (8)0.0264 (7)
O161.32611 (19)0.17312 (14)0.04322 (8)0.0284 (7)
O170.91459 (18)0.06657 (13)0.04345 (7)0.0229 (6)
O180.92277 (19)0.16774 (14)0.02908 (8)0.0284 (7)
O191.32438 (17)0.27913 (13)0.14241 (7)0.0229 (6)
O200.93693 (17)0.29231 (13)0.15567 (8)0.0246 (6)
C230.9700 (2)0.02632 (18)0.19955 (10)0.0141 (8)
C240.8880 (2)0.05284 (18)0.25063 (11)0.0183 (8)
C250.9155 (2)0.01085 (18)0.29277 (11)0.0183 (8)
C260.8659 (3)0.0282 (2)0.35017 (11)0.0269 (10)
C270.8467 (3)0.0454 (2)0.38809 (12)0.0316 (11)
C280.9631 (3)0.1064 (2)0.39848 (12)0.0333 (11)
C290.9457 (4)0.1618 (3)0.44528 (13)0.0423 (14)
C301.2936 (2)0.00720 (18)0.19966 (10)0.0139 (8)
C311.3693 (2)0.03029 (18)0.25378 (11)0.0168 (8)
C321.3290 (2)0.12926 (18)0.28744 (11)0.0169 (8)
C331.3587 (3)0.14722 (19)0.34863 (11)0.0203 (9)
C341.3511 (3)0.25529 (19)0.37658 (11)0.0214 (9)
C351.3293 (3)0.2719 (2)0.43778 (12)0.0268 (10)
C361.3533 (3)0.3766 (2)0.46768 (12)0.0363 (11)
C371.2519 (3)0.05578 (18)0.05464 (11)0.0161 (8)
C381.2454 (3)0.15058 (18)0.07394 (11)0.0178 (8)
C391.0037 (3)0.07068 (17)0.07090 (10)0.0152 (8)
C400.9971 (3)0.14638 (18)0.06355 (11)0.0165 (8)
C411.1103 (3)0.30870 (19)0.09078 (12)0.0276 (10)
C421.1055 (3)0.29945 (19)0.19636 (11)0.0228 (9)
C431.1620 (3)0.35975 (19)0.11754 (12)0.0298 (10)
C441.1455 (3)0.2523 (2)0.21816 (11)0.0242 (9)
H21C0.630200.138300.058700.0490*
H22A0.524200.246200.199500.0460*
H22B0.659000.277600.229800.0460*
H22C0.625800.165700.207800.0460*
H19A0.624400.805700.072400.0660*
H19B0.746100.809700.112300.0660*
H19C0.639100.891700.123800.0660*
H20A0.731300.782000.211400.0530*
H20B0.597400.767300.240300.0530*
H20C0.629600.867700.222500.0530*
H21A0.507700.158700.097300.0490*
H21B0.614000.083100.107900.0490*
H41A1.148400.289300.055000.0410*
H41B1.122200.378500.103200.0410*
H41C1.017700.292400.088700.0410*
H42A1.118500.369700.203300.0340*
H42B1.139900.273800.226800.0340*
H42C1.012900.284000.192000.0340*
H43A1.133400.373800.079800.0450*
H43B1.147000.416700.133500.0450*
H43C1.254500.343100.119500.0450*
H44A1.134600.313900.230000.0360*
H44B1.103700.201100.243800.0360*
H44C1.237800.236900.216400.0360*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0117 (1)0.0127 (1)0.0144 (1)0.0005 (1)0.0000 (1)0.0040 (1)
Ru20.0115 (1)0.0118 (1)0.0128 (1)0.0002 (1)0.0001 (1)0.0015 (1)
S10.0139 (3)0.0144 (3)0.0261 (4)0.0011 (3)0.0005 (3)0.0060 (3)
S20.0137 (3)0.0133 (3)0.0205 (4)0.0020 (3)0.0009 (3)0.0024 (3)
F10.0111 (8)0.0432 (10)0.0322 (10)0.0047 (7)0.0031 (7)0.0015 (8)
F5_a0.024 (2)0.039 (3)0.026 (2)0.015 (2)0.0083 (15)0.003 (3)
F20.0433 (11)0.0189 (8)0.0235 (9)0.0016 (7)0.0120 (8)0.0090 (7)
F6_a0.053 (3)0.011 (3)0.027 (2)0.0065 (19)0.0040 (17)0.012 (3)
F30.0368 (10)0.0208 (9)0.0235 (9)0.0124 (7)0.0022 (7)0.0062 (7)
F7_a0.047 (3)0.0326 (17)0.0168 (17)0.0021 (18)0.0019 (17)0.0045 (12)
F40.0197 (9)0.0295 (9)0.0245 (9)0.0054 (7)0.0006 (7)0.0037 (7)
F8_a0.0236 (19)0.032 (3)0.035 (3)0.0061 (17)0.0066 (16)0.0062 (17)
F9_a0.066 (6)0.027 (4)0.022 (3)0.002 (3)0.003 (3)0.010 (3)
F10_a0.035 (3)0.043 (3)0.038 (2)0.023 (2)0.0100 (17)0.008 (2)
F11_a0.089 (5)0.054 (3)0.036 (3)0.032 (3)0.010 (3)0.008 (2)
F12_a0.076 (3)0.032 (2)0.032 (2)0.001 (2)0.0192 (19)0.0013 (17)
F13_a0.136 (6)0.023 (3)0.042 (2)0.023 (3)0.025 (3)0.001 (2)
F140.0122 (8)0.0288 (9)0.0279 (9)0.0025 (6)0.0020 (7)0.0083 (7)
F150.0280 (9)0.0147 (8)0.0249 (9)0.0005 (6)0.0072 (7)0.0021 (7)
F160.0157 (8)0.0290 (9)0.0229 (9)0.0032 (7)0.0015 (6)0.0056 (7)
F170.0317 (10)0.0198 (8)0.0215 (9)0.0108 (7)0.0060 (7)0.0041 (7)
F180.0416 (11)0.0200 (9)0.0235 (9)0.0059 (7)0.0012 (8)0.0032 (7)
F190.0251 (10)0.0494 (11)0.0314 (10)0.0156 (8)0.0119 (8)0.0100 (8)
F200.0273 (10)0.0627 (13)0.0407 (11)0.0221 (9)0.0023 (8)0.0225 (10)
F210.0462 (12)0.0522 (12)0.0224 (10)0.0081 (9)0.0136 (8)0.0075 (9)
F220.0271 (10)0.0330 (10)0.0401 (11)0.0065 (8)0.0068 (8)0.0110 (8)
F230.0580 (13)0.0266 (9)0.0224 (10)0.0003 (8)0.0026 (8)0.0000 (8)
F240.0884 (16)0.0392 (11)0.0228 (11)0.0087 (10)0.0123 (10)0.0050 (9)
F250.0771 (16)0.0371 (11)0.0430 (12)0.0063 (11)0.0095 (11)0.0173 (9)
F260.0668 (15)0.0494 (12)0.0444 (12)0.0251 (11)0.0024 (10)0.0217 (10)
O10.0143 (10)0.0163 (10)0.0186 (10)0.0017 (7)0.0017 (7)0.0057 (8)
O20.0129 (9)0.0143 (9)0.0158 (10)0.0000 (7)0.0015 (7)0.0017 (7)
O30.0136 (9)0.0136 (9)0.0175 (10)0.0005 (7)0.0009 (7)0.0032 (7)
O40.0170 (10)0.0124 (9)0.0181 (10)0.0014 (7)0.0012 (8)0.0002 (8)
O50.0245 (12)0.0362 (12)0.0295 (12)0.0016 (9)0.0101 (10)0.0104 (10)
O60.0227 (11)0.0376 (12)0.0205 (11)0.0052 (9)0.0061 (9)0.0056 (9)
O70.0206 (11)0.0333 (12)0.0183 (11)0.0070 (9)0.0027 (9)0.0029 (9)
O80.0204 (11)0.0354 (12)0.0246 (12)0.0072 (9)0.0066 (9)0.0078 (9)
O90.0166 (10)0.0228 (11)0.0417 (13)0.0057 (8)0.0010 (9)0.0050 (9)
O100.0158 (10)0.0226 (10)0.0363 (12)0.0048 (8)0.0006 (9)0.0032 (9)
C10.0075 (13)0.0171 (14)0.0171 (15)0.0042 (11)0.0019 (10)0.0008 (11)
C5_a0.016 (3)0.031 (3)0.014 (3)0.005 (2)0.005 (2)0.006 (2)
C20.0154 (14)0.0179 (14)0.0229 (16)0.0013 (11)0.0036 (11)0.0064 (12)
C6_a0.038 (5)0.023 (4)0.032 (4)0.014 (3)0.005 (4)0.007 (3)
C30.0164 (15)0.0191 (14)0.0189 (15)0.0046 (11)0.0022 (11)0.0044 (12)
C40.032 (2)0.0235 (16)0.0233 (17)0.0035 (14)0.0083 (14)0.0078 (13)
C70.061 (3)0.032 (2)0.033 (2)0.0103 (18)0.007 (2)0.0011 (16)
C80.0089 (13)0.0196 (15)0.0153 (15)0.0021 (11)0.0045 (10)0.0058 (12)
C90.0127 (14)0.0149 (14)0.0218 (15)0.0015 (10)0.0016 (11)0.0002 (11)
C100.0129 (14)0.0163 (14)0.0206 (15)0.0036 (11)0.0002 (11)0.0019 (11)
C110.0147 (15)0.0259 (16)0.0226 (16)0.0029 (12)0.0017 (12)0.0012 (12)
C120.0250 (17)0.0363 (18)0.0187 (17)0.0087 (13)0.0043 (13)0.0031 (14)
C130.0348 (18)0.0224 (16)0.0220 (17)0.0070 (13)0.0011 (13)0.0027 (13)
C140.056 (2)0.0303 (19)0.027 (2)0.0086 (17)0.0054 (16)0.0041 (15)
C150.0193 (15)0.0176 (14)0.0209 (16)0.0005 (11)0.0047 (13)0.0043 (12)
C160.0166 (15)0.0149 (14)0.0204 (16)0.0007 (11)0.0057 (12)0.0032 (12)
C170.0172 (15)0.0183 (14)0.0159 (15)0.0048 (11)0.0051 (12)0.0041 (11)
C180.0175 (15)0.0161 (14)0.0169 (15)0.0001 (11)0.0036 (12)0.0040 (11)
C190.046 (2)0.0220 (17)0.069 (3)0.0037 (15)0.0260 (18)0.0206 (17)
C200.0377 (19)0.0177 (16)0.045 (2)0.0035 (13)0.0173 (16)0.0048 (14)
C210.0300 (18)0.0144 (15)0.052 (2)0.0036 (13)0.0126 (15)0.0013 (14)
C220.0357 (19)0.0280 (17)0.0344 (19)0.0136 (14)0.0147 (14)0.0183 (14)
F8A_b0.025 (4)0.042 (5)0.041 (4)0.014 (3)0.003 (3)0.008 (4)
F9A_b0.024 (3)0.048 (5)0.049 (5)0.007 (3)0.005 (3)0.002 (4)
F10A_b0.039 (7)0.046 (11)0.027 (6)0.019 (7)0.010 (5)0.000 (7)
F11A_b0.123 (11)0.043 (4)0.023 (5)0.021 (7)0.011 (6)0.003 (3)
F12A_b0.057 (5)0.059 (6)0.084 (6)0.020 (4)0.023 (4)0.043 (5)
F13A_b0.075 (6)0.037 (5)0.084 (6)0.025 (4)0.019 (4)0.003 (5)
C5A_b0.036 (8)0.040 (6)0.021 (5)0.007 (4)0.010 (4)0.003 (4)
C6A_b0.047 (9)0.025 (7)0.029 (7)0.007 (6)0.017 (7)0.001 (5)
F7A_b0.065 (6)0.052 (4)0.018 (3)0.004 (4)0.020 (4)0.003 (3)
F5A_b0.022 (3)0.034 (5)0.033 (5)0.014 (3)0.009 (3)0.004 (4)
F6A_b0.041 (4)0.014 (5)0.026 (4)0.008 (3)0.001 (3)0.015 (6)
Ru30.0113 (1)0.0113 (1)0.0126 (1)0.0001 (1)0.0002 (1)0.0016 (1)
Ru40.0124 (1)0.0105 (1)0.0131 (1)0.0003 (1)0.0001 (1)0.0003 (1)
S30.0136 (3)0.0123 (3)0.0181 (4)0.0004 (2)0.0001 (3)0.0023 (3)
S40.0143 (3)0.0126 (3)0.0192 (4)0.0011 (3)0.0008 (3)0.0023 (3)
F270.0119 (8)0.0340 (9)0.0343 (10)0.0055 (7)0.0049 (7)0.0121 (8)
F280.0353 (10)0.0144 (8)0.0286 (10)0.0029 (7)0.0138 (7)0.0021 (7)
F290.0291 (9)0.0180 (8)0.0222 (9)0.0076 (7)0.0010 (7)0.0023 (7)
F300.0166 (8)0.0304 (9)0.0225 (9)0.0002 (7)0.0014 (7)0.0053 (7)
F310.0612 (13)0.0273 (10)0.0247 (10)0.0093 (9)0.0052 (9)0.0077 (8)
F320.0376 (11)0.0528 (12)0.0377 (11)0.0213 (9)0.0206 (9)0.0115 (9)
F330.0340 (11)0.0575 (12)0.0373 (11)0.0171 (9)0.0037 (8)0.0168 (9)
F340.0621 (14)0.0553 (13)0.0261 (11)0.0059 (10)0.0226 (9)0.0030 (9)
F350.0558 (13)0.0412 (11)0.0230 (10)0.0112 (9)0.0057 (8)0.0069 (8)
F360.0375 (11)0.0566 (12)0.0446 (12)0.0149 (9)0.0073 (9)0.0209 (10)
F370.0862 (19)0.0841 (17)0.0560 (15)0.0182 (14)0.0058 (13)0.0451 (13)
F380.0788 (16)0.0475 (12)0.0445 (13)0.0292 (11)0.0036 (11)0.0185 (10)
F390.116 (2)0.0506 (13)0.0222 (11)0.0265 (13)0.0074 (11)0.0068 (10)
F400.0353 (10)0.0160 (8)0.0203 (9)0.0023 (7)0.0091 (7)0.0074 (7)
F410.0128 (8)0.0247 (9)0.0302 (9)0.0031 (6)0.0037 (7)0.0010 (7)
F420.0295 (9)0.0163 (8)0.0202 (9)0.0045 (7)0.0044 (7)0.0032 (6)
F430.0145 (8)0.0266 (9)0.0224 (9)0.0024 (6)0.0025 (6)0.0005 (7)
F440.0421 (11)0.0258 (9)0.0216 (9)0.0094 (8)0.0019 (8)0.0088 (7)
F450.0278 (10)0.0328 (10)0.0279 (10)0.0113 (7)0.0119 (7)0.0038 (8)
F460.0345 (10)0.0274 (9)0.0229 (9)0.0114 (7)0.0044 (7)0.0025 (7)
F470.0316 (10)0.0292 (9)0.0290 (10)0.0119 (8)0.0049 (8)0.0036 (7)
F480.0425 (12)0.0474 (12)0.0318 (11)0.0074 (9)0.0136 (9)0.0035 (9)
F490.0672 (14)0.0367 (11)0.0240 (10)0.0147 (9)0.0127 (9)0.0035 (8)
F500.0759 (15)0.0440 (12)0.0220 (11)0.0100 (10)0.0086 (10)0.0041 (9)
F510.0980 (18)0.0309 (11)0.0327 (11)0.0181 (11)0.0006 (11)0.0005 (9)
F520.0569 (15)0.0575 (14)0.0507 (14)0.0202 (11)0.0028 (11)0.0256 (10)
O110.0124 (9)0.0147 (9)0.0153 (10)0.0023 (7)0.0003 (7)0.0034 (7)
O120.0142 (10)0.0144 (10)0.0192 (10)0.0005 (7)0.0028 (8)0.0004 (8)
O130.0141 (10)0.0162 (9)0.0182 (10)0.0001 (7)0.0010 (7)0.0051 (8)
O140.0138 (9)0.0119 (9)0.0153 (10)0.0005 (7)0.0018 (7)0.0008 (7)
O150.0221 (11)0.0356 (12)0.0198 (11)0.0009 (9)0.0071 (9)0.0011 (9)
O160.0245 (12)0.0299 (12)0.0289 (12)0.0063 (9)0.0111 (10)0.0001 (9)
O170.0175 (11)0.0276 (11)0.0216 (11)0.0026 (8)0.0036 (9)0.0004 (9)
O180.0298 (12)0.0316 (12)0.0230 (12)0.0077 (9)0.0071 (10)0.0045 (9)
O190.0140 (10)0.0225 (10)0.0319 (12)0.0046 (8)0.0000 (8)0.0051 (9)
O200.0156 (10)0.0245 (11)0.0349 (12)0.0054 (8)0.0006 (8)0.0096 (9)
C230.0103 (13)0.0144 (14)0.0176 (15)0.0037 (10)0.0036 (11)0.0033 (11)
C240.0143 (14)0.0143 (14)0.0252 (16)0.0008 (11)0.0036 (11)0.0008 (12)
C250.0118 (14)0.0181 (14)0.0231 (16)0.0014 (11)0.0018 (11)0.0009 (12)
C260.0290 (17)0.0267 (16)0.0230 (17)0.0016 (13)0.0090 (13)0.0005 (13)
C270.0347 (19)0.0356 (18)0.0225 (18)0.0053 (15)0.0099 (14)0.0005 (14)
C280.042 (2)0.0347 (18)0.0229 (18)0.0067 (15)0.0010 (14)0.0057 (14)
C290.060 (3)0.043 (2)0.024 (2)0.0093 (19)0.0005 (17)0.0075 (16)
C300.0097 (13)0.0152 (14)0.0157 (15)0.0048 (10)0.0022 (10)0.0001 (11)
C310.0125 (14)0.0153 (14)0.0234 (16)0.0010 (10)0.0022 (11)0.0060 (12)
C320.0129 (14)0.0167 (14)0.0217 (16)0.0022 (11)0.0016 (11)0.0058 (11)
C330.0185 (15)0.0206 (15)0.0225 (16)0.0002 (12)0.0026 (12)0.0060 (12)
C340.0222 (16)0.0211 (15)0.0206 (16)0.0001 (12)0.0006 (12)0.0032 (12)
C350.0280 (18)0.0299 (17)0.0228 (17)0.0030 (13)0.0016 (13)0.0060 (13)
C360.049 (2)0.0351 (19)0.0208 (19)0.0044 (16)0.0032 (15)0.0044 (15)
C370.0166 (15)0.0121 (13)0.0193 (16)0.0010 (11)0.0067 (12)0.0026 (11)
C380.0206 (15)0.0126 (13)0.0197 (16)0.0017 (11)0.0034 (12)0.0020 (11)
C390.0163 (15)0.0133 (13)0.0151 (15)0.0017 (11)0.0036 (12)0.0004 (11)
C400.0170 (14)0.0151 (14)0.0179 (16)0.0014 (11)0.0035 (12)0.0044 (11)
C410.0339 (18)0.0175 (15)0.0322 (18)0.0000 (13)0.0136 (14)0.0076 (13)
C420.0219 (16)0.0167 (14)0.0265 (17)0.0016 (11)0.0066 (12)0.0039 (12)
C430.0351 (18)0.0165 (15)0.0370 (19)0.0058 (13)0.0130 (14)0.0025 (13)
C440.0274 (17)0.0212 (15)0.0255 (17)0.0047 (12)0.0063 (13)0.0087 (13)
Geometric parameters (Å, º) top
Ru1—Ru22.6907 (4)F39—C291.304 (4)
Ru1—S12.4164 (8)F40—C311.347 (3)
Ru1—O12.1476 (17)F41—C311.353 (3)
Ru1—O32.1256 (18)F42—C321.345 (3)
Ru1—C151.864 (3)F43—C321.350 (3)
Ru1—C171.850 (3)F44—C331.346 (3)
Ru2—S22.4095 (7)F45—C331.345 (3)
Ru2—O22.1364 (18)F46—C341.342 (3)
Ru2—O42.1515 (17)F47—C341.346 (3)
Ru2—C161.852 (3)F48—C351.341 (4)
Ru2—C181.856 (3)F49—C351.341 (4)
Ru3—O112.1370 (18)F50—C361.328 (3)
Ru3—O132.1558 (17)F51—C361.322 (4)
Ru3—C371.854 (3)F52—C361.314 (4)
Ru3—C391.853 (3)O1—C11.253 (3)
Ru3—S32.4242 (7)O2—C11.242 (3)
Ru3—Ru42.6908 (4)O3—C81.247 (3)
Ru4—O122.1484 (17)O4—C81.250 (3)
Ru4—S42.4239 (7)O5—C151.142 (4)
Ru4—C401.843 (3)O6—C161.148 (4)
Ru4—O142.1290 (18)O7—C171.145 (3)
Ru4—C381.852 (3)O8—C181.146 (4)
S1—C191.773 (3)O11—C231.248 (3)
S1—O91.4761 (19)O12—C231.248 (3)
S1—C201.771 (3)O13—C301.255 (3)
S2—O101.4789 (19)O14—C301.247 (3)
S2—C211.779 (3)O15—C371.150 (3)
S2—C221.767 (3)O16—C381.151 (4)
S3—O191.4801 (19)O17—C391.143 (3)
S3—C421.773 (3)O18—C401.150 (4)
S3—C411.775 (3)C1—C21.549 (4)
S4—O201.4780 (19)C2—C31.550 (4)
S4—C431.777 (3)C3—C41.541 (4)
S4—C441.775 (3)C4—C5i1.610 (5)
F1—C21.354 (3)C4—C5Aii1.588 (8)
F2—C21.344 (3)C5i—C6i1.553 (10)
F3—C31.348 (3)C5Aii—C6Aii1.467 (16)
F4—C31.351 (3)C6i—C71.507 (9)
F5i—C41.239 (6)C6Aii—C71.634 (13)
F5Aii—C41.506 (9)C8—C91.546 (3)
F6i—C41.427 (7)C9—C101.553 (4)
F6Aii—C41.182 (12)C10—C111.542 (4)
F7i—C5i1.348 (6)C11—C121.561 (4)
F7Aii—C5Aii1.345 (11)C12—C131.536 (4)
F8i—C5i1.345 (7)C13—C141.545 (4)
F8Aii—C5Aii1.364 (13)C19—H19C0.9800
F9i—C6i1.345 (19)C19—H19A0.9800
F9Aii—C6Aii1.380 (16)C19—H19B0.9800
F10i—C6i1.334 (10)C20—H20B0.9800
F10Aii—C6Aii1.32 (3)C20—H20A0.9800
F11i—C71.363 (8)C20—H20C0.9800
F11Aii—C71.287 (11)C21—H21A0.9800
F12i—C71.272 (6)C21—H21B0.9800
F12Aii—C71.378 (9)C21—H21C0.9800
F13i—C71.330 (6)C22—H22B0.9800
F13Aii—C71.243 (10)C22—H22C0.9800
F14—C91.359 (3)C22—H22A0.9800
F15—C91.347 (3)C23—C241.539 (3)
F16—C101.352 (3)C24—C251.550 (4)
F17—C101.347 (3)C25—C261.544 (4)
F18—C111.340 (3)C26—C271.558 (4)
F19—C111.350 (3)C27—C281.541 (4)
F20—C121.340 (3)C28—C291.552 (5)
F21—C121.356 (3)C30—C311.548 (4)
F22—C131.344 (3)C31—C321.553 (4)
F23—C131.341 (3)C32—C331.547 (4)
F24—C141.324 (4)C33—C341.555 (4)
F25—C141.326 (4)C34—C351.539 (4)
F26—C141.324 (4)C35—C361.539 (4)
F27—C241.360 (3)C41—H41A0.9800
F28—C241.347 (3)C41—H41B0.9800
F29—C251.346 (3)C41—H41C0.9800
F30—C251.351 (3)C42—H42A0.9800
F31—C261.343 (3)C42—H42B0.9800
F32—C261.345 (4)C42—H42C0.9800
F33—C271.344 (4)C43—H43A0.9800
F34—C271.349 (3)C43—H43B0.9800
F35—C281.342 (3)C43—H43C0.9800
F36—C281.343 (4)C44—H44A0.9800
F37—C291.325 (5)C44—H44B0.9800
F38—C291.315 (5)C44—H44C0.9800
Ru2—Ru1—S1165.14 (3)F16—C10—C11108.3 (2)
Ru2—Ru1—O185.57 (5)F17—C10—C9108.61 (19)
Ru2—Ru1—O381.03 (5)C9—C10—C11115.0 (2)
Ru2—Ru1—C1591.69 (9)F16—C10—F17107.67 (19)
Ru2—Ru1—C1797.51 (8)F16—C10—C9108.21 (18)
S1—Ru1—O184.66 (5)F17—C10—C11108.8 (2)
S1—Ru1—O386.48 (5)F18—C11—C10108.8 (2)
S1—Ru1—C1597.79 (9)F18—C11—C12108.2 (2)
S1—Ru1—C1793.93 (8)F18—C11—F19108.2 (2)
O1—Ru1—O381.58 (7)C10—C11—C12117.7 (2)
O1—Ru1—C15176.98 (10)F19—C11—C10107.9 (2)
O1—Ru1—C1791.58 (10)F19—C11—C12105.8 (2)
O3—Ru1—C1596.76 (10)F21—C12—C11105.7 (2)
O3—Ru1—C17173.08 (10)F20—C12—F21107.9 (2)
C15—Ru1—C1790.03 (13)C11—C12—C13117.8 (2)
Ru1—Ru2—S2164.70 (3)F20—C12—C11108.2 (2)
Ru1—Ru2—O280.73 (5)F21—C12—C13108.1 (2)
Ru1—Ru2—O485.21 (5)F20—C12—C13108.8 (2)
Ru1—Ru2—C1698.04 (8)F23—C13—C14107.7 (2)
Ru1—Ru2—C1892.40 (8)C12—C13—C14114.9 (3)
S2—Ru2—O286.55 (5)F23—C13—C12108.9 (2)
S2—Ru2—O484.54 (5)F22—C13—C12109.4 (2)
S2—Ru2—C1693.78 (8)F22—C13—C14107.5 (3)
S2—Ru2—C1897.63 (8)F22—C13—F23108.3 (2)
O2—Ru2—O481.56 (7)F24—C14—F25108.3 (3)
O2—Ru2—C16174.25 (10)F24—C14—F26108.7 (3)
O2—Ru2—C1897.19 (10)F26—C14—C13110.8 (3)
O4—Ru2—C1692.75 (10)F24—C14—C13111.1 (2)
O4—Ru2—C18177.44 (10)F25—C14—F26108.4 (2)
C16—Ru2—C1888.47 (13)F25—C14—C13109.5 (3)
O13—Ru3—C3794.49 (10)Ru1—C15—O5178.8 (3)
O13—Ru3—C39174.63 (10)Ru2—C16—O6177.2 (3)
C37—Ru3—C3989.47 (13)Ru1—C17—O7176.1 (3)
S3—Ru3—O1384.05 (5)Ru2—C18—O8177.1 (3)
Ru4—Ru3—S3164.05 (3)H19B—C19—H19C109.00
Ru4—Ru3—O1180.94 (5)S1—C19—H19B110.00
Ru4—Ru3—O1384.70 (5)S1—C19—H19A110.00
Ru4—Ru3—C3798.17 (8)H19A—C19—H19C110.00
Ru4—Ru3—C3991.15 (8)S1—C19—H19C109.00
S3—Ru3—O1186.41 (5)H19A—C19—H19B109.00
O11—Ru3—O1382.52 (7)S1—C20—H20C109.00
S3—Ru3—C3793.95 (8)S1—C20—H20B110.00
S3—Ru3—C3999.33 (8)S1—C20—H20A110.00
O11—Ru3—C37176.94 (10)H20A—C20—H20B110.00
O11—Ru3—C3993.48 (10)H20A—C20—H20C109.00
Ru3—Ru4—S4163.46 (3)H20B—C20—H20C109.00
O14—Ru4—C40174.39 (10)S2—C21—H21A109.00
C38—Ru4—C4088.68 (13)S2—C21—H21B109.00
S4—Ru4—C3899.90 (8)S2—C21—H21C109.00
Ru3—Ru4—O1284.99 (5)H21A—C21—H21B109.00
Ru3—Ru4—O1480.98 (5)H21A—C21—H21C110.00
Ru3—Ru4—C3891.68 (8)H21B—C21—H21C110.00
Ru3—Ru4—C4098.23 (8)S2—C22—H22A110.00
S4—Ru4—O1283.07 (5)S2—C22—H22B110.00
S4—Ru4—O1485.90 (5)S2—C22—H22C110.00
O12—Ru4—C38176.35 (10)H22A—C22—H22B109.00
S4—Ru4—C4093.84 (8)H22A—C22—H22C109.00
O12—Ru4—O1481.15 (7)H22B—C22—H22C109.00
O12—Ru4—C4093.25 (10)O11—C23—O12128.9 (2)
O14—Ru4—C3896.89 (10)O11—C23—C24116.6 (2)
Ru1—S1—C20110.65 (10)O12—C23—C24114.5 (2)
Ru1—S1—O9117.00 (8)F27—C24—F28107.77 (19)
Ru1—S1—C19111.89 (11)F27—C24—C23108.1 (2)
C19—S1—C2099.36 (15)F27—C24—C25107.93 (19)
O9—S1—C19108.31 (13)F28—C24—C23111.1 (2)
O9—S1—C20108.12 (13)F28—C24—C25108.5 (2)
O10—S2—C21108.32 (13)C23—C24—C25113.2 (2)
Ru2—S2—O10116.95 (8)F29—C25—F30107.61 (19)
Ru2—S2—C21112.04 (10)F29—C25—C24108.5 (2)
Ru2—S2—C22109.90 (10)F29—C25—C26108.6 (2)
O10—S2—C22108.79 (13)F30—C25—C24108.05 (19)
C21—S2—C2299.37 (14)F30—C25—C26108.1 (2)
Ru3—S3—O19116.29 (8)C24—C25—C26115.7 (2)
Ru3—S3—C41112.73 (10)F31—C26—F32108.3 (2)
Ru3—S3—C42110.79 (10)F31—C26—C25108.8 (2)
O19—S3—C41108.12 (13)F31—C26—C27108.4 (2)
O19—S3—C42108.35 (13)F32—C26—C25108.0 (2)
C41—S3—C4299.13 (14)F32—C26—C27105.4 (2)
Ru4—S4—O20116.02 (8)C25—C26—C27117.6 (2)
Ru4—S4—C43112.90 (10)F33—C27—F34108.1 (2)
O20—S4—C43108.41 (13)F33—C27—C26108.4 (2)
O20—S4—C44108.89 (13)F33—C27—C28108.3 (2)
C43—S4—C4499.25 (14)F34—C27—C26105.9 (2)
Ru4—S4—C44110.03 (10)F34—C27—C28107.7 (2)
Ru1—O1—C1115.61 (15)C26—C27—C28118.1 (3)
Ru2—O2—C1123.30 (16)F35—C28—F36108.2 (2)
Ru1—O3—C8123.30 (16)F35—C28—C27109.0 (2)
Ru2—O4—C8116.06 (15)F35—C28—C29107.6 (2)
Ru3—O11—C23122.72 (16)F36—C28—C27109.3 (2)
Ru4—O12—C23116.39 (15)F36—C28—C29107.6 (3)
Ru3—O13—C30114.98 (14)C27—C28—C29114.9 (3)
Ru4—O14—C30122.65 (16)F37—C29—F38107.7 (3)
O1—C1—O2129.3 (2)F37—C29—F39108.7 (3)
O1—C1—C2114.2 (2)F37—C29—C28109.0 (3)
O2—C1—C2116.5 (2)F38—C29—F39109.1 (3)
C1—C2—C3111.83 (19)F38—C29—C28110.5 (3)
F1—C2—C3107.89 (18)F39—C29—C28111.8 (3)
F1—C2—F2107.79 (19)O13—C30—O14129.0 (2)
F1—C2—C1109.0 (2)O13—C30—C31114.8 (2)
F2—C2—C1110.82 (19)O14—C30—C31116.1 (2)
F2—C2—C3109.3 (2)F40—C31—F41107.77 (19)
F4—C3—C2108.09 (19)F40—C31—C30111.0 (2)
F3—C3—C4108.2 (2)F40—C31—C32108.5 (2)
C2—C3—C4116.5 (2)F41—C31—C30109.9 (2)
F3—C3—F4107.8 (2)F41—C31—C32108.81 (19)
F4—C3—C4107.8 (2)C30—C31—C32110.81 (19)
F3—C3—C2108.1 (2)F42—C32—F43108.2 (2)
C3—C4—C5i115.9 (3)F42—C32—C31109.0 (2)
F5Aii—C4—C3103.7 (5)F42—C32—C33107.8 (2)
F6i—C4—C3107.9 (5)F43—C32—C31107.43 (19)
F6Aii—C4—C5Aii115.2 (9)F43—C32—C33107.4 (2)
F5i—C4—F6i109.6 (4)C31—C32—C33116.7 (2)
F6Aii—C4—C3111.6 (9)F44—C33—F45108.3 (2)
C3—C4—C5Aii117.5 (3)F44—C33—C32108.6 (2)
F6i—C4—C5i101.1 (5)F44—C33—C34108.9 (2)
F5Aii—C4—F6Aii107.9 (6)F45—C33—C32108.8 (2)
F5Aii—C4—C5Aii98.7 (6)F45—C33—C34108.8 (2)
F5i—C4—C3111.4 (4)C32—C33—C34113.4 (2)
F5i—C4—C5i110.3 (4)F46—C34—F47108.1 (2)
F8i—C5i—C6i108.7 (5)F46—C34—C33108.9 (2)
C4—C5i—C6i118.2 (4)F46—C34—C35108.2 (2)
F7i—C5i—F8i107.5 (4)F47—C34—C33108.4 (2)
F8i—C5i—C4109.7 (4)F47—C34—C35108.8 (2)
F7i—C5i—C4104.1 (3)C33—C34—C35114.3 (2)
F7i—C5i—C6i108.0 (4)F48—C35—F49109.1 (2)
C4—C5Aii—C6Aii113.8 (9)F48—C35—C34108.7 (2)
F7Aii—C5Aii—C4104.0 (5)F48—C35—C36107.3 (2)
F8Aii—C5Aii—C4112.3 (7)F49—C35—C34109.1 (2)
F7Aii—C5Aii—F8Aii108.7 (9)F49—C35—C36108.0 (2)
F7Aii—C5Aii—C6Aii109.8 (8)C34—C35—C36114.5 (2)
F8Aii—C5Aii—C6Aii108.2 (8)F50—C36—F51108.7 (2)
F10i—C6i—C7111.7 (6)F50—C36—F52108.1 (2)
C5i—C6i—C7113.8 (5)F50—C36—C35109.3 (2)
F10i—C6i—C5i109.2 (6)F51—C36—F52108.8 (2)
F9i—C6i—C7106.0 (9)F51—C36—C35110.5 (2)
F9i—C6i—C5i107.8 (8)F52—C36—C35111.5 (2)
F9i—C6i—F10i108.1 (9)Ru3—C37—O15178.5 (2)
F9Aii—C6Aii—F10Aii106.4 (14)Ru4—C38—O16177.3 (2)
F9Aii—C6Aii—C5Aii108.7 (10)Ru3—C39—O17178.5 (2)
F10Aii—C6Aii—C5Aii113.3 (14)Ru4—C40—O18177.6 (3)
C5Aii—C6Aii—C7112.3 (9)S3—C41—H41A110.00
F9Aii—C6Aii—C7107.6 (9)S3—C41—H41B109.00
F10Aii—C6Aii—C7108.3 (13)S3—C41—H41C109.00
F12i—C7—F13i111.6 (4)H41A—C41—H41B109.00
F11i—C7—F12i108.6 (4)H41A—C41—H41C109.00
F12i—C7—C6i115.1 (4)H41B—C41—H41C109.00
F13i—C7—C6i109.6 (4)S3—C42—H42A110.00
F11Aii—C7—F12Aii109.0 (7)S3—C42—H42B109.00
F12Aii—C7—C6Aii103.0 (7)S3—C42—H42C110.00
F13Aii—C7—C6Aii109.2 (7)H42A—C42—H42B109.00
F12Aii—C7—F13Aii106.5 (6)H42A—C42—H42C109.00
F11Aii—C7—C6Aii111.3 (7)H42B—C42—H42C109.00
F11i—C7—F13i102.8 (5)S4—C43—H43A109.00
F11i—C7—C6i108.3 (5)S4—C43—H43B110.00
F11Aii—C7—F13Aii116.8 (8)S4—C43—H43C110.00
O3—C8—C9116.0 (2)H43A—C43—H43B109.00
O3—C8—O4129.0 (2)H43A—C43—H43C109.00
O4—C8—C9115.0 (2)H43B—C43—H43C109.00
F14—C9—C8108.6 (2)S4—C44—H44A109.00
C8—C9—C10113.15 (19)S4—C44—H44B109.00
F14—C9—F15107.75 (19)S4—C44—H44C110.00
F15—C9—C8110.72 (19)H44A—C44—H44B110.00
F15—C9—C10108.7 (2)H44A—C44—H44C110.00
F14—C9—C10107.78 (18)H44B—C44—H44C109.00
O1—Ru1—Ru2—O215.43 (7)C4—C5i—C6i—C7162.5 (4)
O1—Ru1—Ru2—O497.64 (7)C4—C5i—C6i—F9i80.3 (10)
O1—Ru1—Ru2—C16170.26 (10)C4—C5i—C6i—F10i36.9 (7)
O1—Ru1—Ru2—C1881.47 (10)F8i—C5i—C6i—F10i162.8 (5)
O3—Ru1—Ru2—O266.73 (7)F9i—C6i—C7—F13i55.4 (10)
O3—Ru1—Ru2—O415.48 (7)F10i—C6i—C7—F11i49.3 (7)
O3—Ru1—Ru2—C16107.59 (10)F10i—C6i—C7—F12i171.1 (5)
O3—Ru1—Ru2—C18163.62 (10)C5i—C6i—C7—F11i74.9 (7)
C15—Ru1—Ru2—O2163.31 (10)C5i—C6i—C7—F12i46.9 (7)
C15—Ru1—Ru2—O481.10 (10)C5i—C6i—C7—F13i173.7 (6)
C15—Ru1—Ru2—C1611.01 (13)F9i—C6i—C7—F11i166.9 (9)
C15—Ru1—Ru2—C1899.80 (13)F9i—C6i—C7—F12i71.4 (9)
C17—Ru1—Ru2—O2106.44 (10)F10i—C6i—C7—F13i62.1 (7)
C17—Ru1—Ru2—O4171.35 (10)O3—C8—C9—F14118.2 (2)
C17—Ru1—Ru2—C1679.24 (13)O3—C8—C9—F150.1 (3)
C17—Ru1—Ru2—C189.55 (13)O4—C8—C9—F1462.4 (3)
O1—Ru1—S1—O948.27 (11)O4—C8—C9—F15179.51 (19)
O1—Ru1—S1—C19174.06 (13)O3—C8—C9—C10122.2 (2)
O1—Ru1—S1—C2076.14 (12)O4—C8—C9—C1057.2 (3)
O3—Ru1—S1—O9130.13 (11)F14—C9—C10—F1740.9 (2)
O3—Ru1—S1—C19104.09 (13)F14—C9—C10—C1181.4 (3)
O3—Ru1—S1—C205.72 (12)F15—C9—C10—F1686.0 (2)
C15—Ru1—S1—O9133.52 (13)F15—C9—C10—F17157.35 (17)
C15—Ru1—S1—C197.73 (15)F15—C9—C10—C1135.1 (3)
C15—Ru1—S1—C20102.08 (14)C8—C9—C10—F1637.4 (3)
C17—Ru1—S1—O942.95 (13)F14—C9—C10—F16157.45 (19)
C17—Ru1—S1—C1982.84 (15)C8—C9—C10—C11158.6 (2)
C17—Ru1—S1—C20167.36 (14)C8—C9—C10—F1779.2 (2)
Ru2—Ru1—O1—C122.27 (16)F16—C10—C11—F1845.6 (3)
S1—Ru1—O1—C1146.52 (17)F16—C10—C11—F19162.7 (2)
O3—Ru1—O1—C159.30 (17)F17—C10—C11—F18162.4 (2)
C17—Ru1—O1—C1119.68 (18)F17—C10—C11—F1980.5 (3)
Ru2—Ru1—O3—C816.49 (17)F16—C10—C11—C1277.8 (3)
S1—Ru1—O3—C8171.59 (18)C9—C10—C11—F1875.5 (3)
O1—Ru1—O3—C8103.30 (18)C9—C10—C11—F1941.6 (3)
C15—Ru1—O3—C874.2 (2)C9—C10—C11—C12161.0 (2)
O2—Ru2—S2—O10127.14 (11)F17—C10—C11—C1238.9 (3)
O2—Ru2—S2—C21106.97 (12)F18—C11—C12—F20167.5 (2)
O2—Ru2—S2—C222.50 (12)F18—C11—C12—F2152.1 (3)
O4—Ru2—S2—O1045.30 (11)F19—C11—C12—F2051.8 (3)
O4—Ru2—S2—C21171.19 (12)F19—C11—C12—F2163.5 (3)
O4—Ru2—S2—C2279.34 (12)F18—C11—C12—C1368.7 (3)
C16—Ru2—S2—O1047.11 (13)C10—C11—C12—F2068.7 (3)
C16—Ru2—S2—C2178.78 (15)C10—C11—C12—F21175.9 (2)
C16—Ru2—S2—C22171.74 (14)C10—C11—C12—C1355.1 (3)
C18—Ru2—S2—O10136.06 (13)F19—C11—C12—C13175.6 (2)
C18—Ru2—S2—C2110.17 (15)F20—C12—C13—F2349.3 (3)
C18—Ru2—S2—C2299.30 (14)F20—C12—C13—C1471.5 (3)
Ru1—Ru2—O2—C115.60 (17)F20—C12—C13—F22167.5 (2)
S2—Ru2—O2—C1172.93 (18)F21—C12—C13—F23166.3 (2)
O4—Ru2—O2—C1102.09 (18)F21—C12—C13—C1445.4 (3)
C18—Ru2—O2—C175.67 (19)C11—C12—C13—F2244.0 (3)
Ru1—Ru2—O4—C821.65 (16)C11—C12—C13—F2374.2 (3)
S2—Ru2—O4—C8146.97 (17)C11—C12—C13—C14165.0 (2)
O2—Ru2—O4—C859.66 (17)F21—C12—C13—F2275.6 (3)
C16—Ru2—O4—C8119.50 (18)F22—C13—C14—F2450.5 (4)
O11—Ru3—S3—C41111.80 (12)F22—C13—C14—F2569.1 (3)
O11—Ru3—S3—C421.74 (12)F23—C13—C14—F24167.0 (3)
O13—Ru3—S3—O1939.70 (10)F23—C13—C14—F2547.4 (3)
O13—Ru3—S3—C41165.35 (12)F23—C13—C14—F2672.1 (3)
O13—Ru3—S3—C4284.59 (12)C12—C13—C14—F2471.5 (4)
C37—Ru3—S3—O1954.41 (13)C12—C13—C14—F25169.0 (3)
C37—Ru3—S3—C4171.25 (14)C12—C13—C14—F2649.4 (3)
C37—Ru3—S3—C42178.69 (14)F22—C13—C14—F26171.4 (2)
C39—Ru3—S3—O19144.52 (12)O11—C23—C24—F27116.5 (2)
C39—Ru3—S3—C4118.86 (14)O11—C23—C24—F281.6 (3)
C39—Ru3—S3—C4291.20 (14)O11—C23—C24—C25124.1 (2)
Ru4—Ru3—O11—C2317.91 (17)O12—C23—C24—F2764.1 (3)
S3—Ru3—O11—C23171.85 (18)O12—C23—C24—F28177.85 (19)
O13—Ru3—O11—C23103.69 (18)O12—C23—C24—C2555.4 (3)
C39—Ru3—O11—C2372.70 (19)F27—C24—C25—F2946.0 (2)
Ru4—Ru3—O13—C3026.38 (16)F27—C24—C25—F30162.36 (19)
S3—Ru3—O13—C30142.30 (17)F27—C24—C25—C2676.3 (3)
O11—Ru3—O13—C3055.15 (17)F28—C24—C25—F29162.52 (17)
C37—Ru3—O13—C30124.19 (18)F28—C24—C25—F3081.1 (2)
O11—Ru3—Ru4—C40109.10 (10)F28—C24—C25—C2640.2 (3)
O13—Ru3—Ru4—O1299.77 (7)C23—C24—C25—F2973.6 (2)
O13—Ru3—Ru4—O1417.96 (7)C23—C24—C25—F3042.8 (3)
O13—Ru3—Ru4—C3878.75 (10)C23—C24—C25—C26164.1 (2)
O13—Ru3—Ru4—C40167.66 (10)F29—C25—C26—F31160.5 (2)
C37—Ru3—Ru4—O12166.44 (10)F29—C25—C26—F3282.1 (2)
C37—Ru3—Ru4—O14111.75 (10)F29—C25—C26—C2736.9 (3)
C37—Ru3—Ru4—C3815.04 (13)F30—C25—C26—F3144.0 (3)
C37—Ru3—Ru4—C4073.87 (13)F30—C25—C26—F32161.4 (2)
C39—Ru3—Ru4—O1276.81 (10)F30—C25—C26—C2779.6 (3)
C39—Ru3—Ru4—O14158.63 (10)C24—C25—C26—F3177.2 (3)
C39—Ru3—Ru4—C38104.66 (12)C24—C25—C26—F3240.1 (3)
C39—Ru3—Ru4—C4015.76 (13)C24—C25—C26—C27159.1 (2)
O11—Ru3—S3—O19122.54 (10)F31—C26—C27—F33168.6 (2)
O11—Ru3—Ru4—O1465.29 (7)F31—C26—C27—F3452.8 (3)
O11—Ru3—Ru4—C38162.00 (10)F31—C26—C27—C2867.9 (3)
O11—Ru3—Ru4—O1216.53 (7)F32—C26—C27—F3352.7 (3)
Ru3—Ru4—O14—C3017.46 (17)F32—C26—C27—F3463.0 (3)
S4—Ru4—O14—C30172.65 (17)F32—C26—C27—C28176.3 (2)
C38—Ru4—O14—C3073.15 (19)C25—C26—C27—F3367.6 (3)
O14—Ru4—S4—C43105.01 (12)C25—C26—C27—F34176.6 (2)
O12—Ru4—O14—C30103.74 (18)C25—C26—C27—C2855.9 (3)
C38—Ru4—S4—O20134.70 (13)F33—C27—C28—F3552.3 (3)
C38—Ru4—S4—C438.72 (14)F33—C27—C28—F36170.3 (2)
C38—Ru4—S4—C44101.15 (14)F33—C27—C28—C2968.6 (3)
C40—Ru4—S4—O2045.38 (13)F34—C27—C28—F35168.9 (2)
C40—Ru4—S4—C4380.61 (14)F34—C27—C28—F3673.0 (3)
C40—Ru4—S4—C44169.53 (14)F34—C27—C28—C2948.1 (3)
O14—Ru4—S4—C444.85 (12)C26—C27—C28—F3571.3 (3)
O14—Ru4—O12—C2358.69 (17)C26—C27—C28—F3646.8 (3)
C40—Ru4—O12—C23120.92 (18)C26—C27—C28—C29167.8 (3)
O12—Ru4—S4—O2047.43 (10)F35—C28—C29—F3748.6 (4)
O12—Ru4—S4—C43173.42 (12)F35—C28—C29—F3869.6 (4)
O12—Ru4—S4—C4476.72 (12)F35—C28—C29—F39168.8 (3)
O14—Ru4—S4—O20129.00 (10)F36—C28—C29—F3767.8 (3)
Ru3—Ru4—O12—C2322.94 (16)F36—C28—C29—F38174.1 (3)
S4—Ru4—O12—C23145.60 (17)F36—C28—C29—F3952.4 (4)
Ru1—O1—C1—O218.7 (3)C27—C28—C29—F37170.2 (3)
Ru1—O1—C1—C2159.62 (14)C27—C28—C29—F3852.1 (4)
Ru2—O2—C1—C2179.83 (14)C27—C28—C29—F3969.6 (4)
Ru2—O2—C1—O11.9 (3)O13—C30—C31—F40178.07 (19)
Ru1—O3—C8—C9176.96 (14)O13—C30—C31—F4162.8 (3)
Ru1—O3—C8—O43.8 (3)O13—C30—C31—C3257.5 (3)
Ru2—O4—C8—C9162.21 (15)O14—C30—C31—F400.1 (3)
Ru2—O4—C8—O317.1 (3)O14—C30—C31—F41119.0 (2)
Ru3—O11—C23—O124.8 (3)O14—C30—C31—C32120.7 (2)
Ru3—O11—C23—C24175.85 (14)F40—C31—C32—F42160.26 (18)
Ru4—O12—C23—O1117.5 (3)F40—C31—C32—F4382.7 (2)
Ru4—O12—C23—C24161.86 (14)F40—C31—C32—C3337.8 (3)
Ru3—O13—C30—O1423.1 (3)F41—C31—C32—F4243.3 (3)
Ru3—O13—C30—C31154.81 (15)F41—C31—C32—F43160.26 (19)
Ru4—O14—C30—O130.6 (3)F41—C31—C32—C3379.2 (3)
Ru4—O14—C30—C31178.51 (14)C30—C31—C32—F4277.7 (2)
O1—C1—C2—F163.3 (3)C30—C31—C32—F4339.3 (3)
O1—C1—C2—F2178.20 (19)C30—C31—C32—C33159.9 (2)
O1—C1—C2—C355.9 (3)F42—C32—C33—F44162.30 (19)
O2—C1—C2—F1118.2 (2)F42—C32—C33—F4580.1 (2)
O2—C1—C2—F20.3 (3)F42—C32—C33—C3441.1 (3)
O2—C1—C2—C3122.6 (2)F43—C32—C33—F4445.9 (3)
F2—C2—C3—F482.8 (2)F43—C32—C33—F45163.6 (2)
F2—C2—C3—C438.7 (3)F43—C32—C33—C3475.3 (3)
C1—C2—C3—F376.1 (2)C31—C32—C33—F4474.7 (3)
F1—C2—C3—F343.8 (3)C31—C32—C33—F4543.0 (3)
F1—C2—C3—F4160.2 (2)C31—C32—C33—C34164.2 (2)
F1—C2—C3—C478.3 (3)F44—C33—C34—F4683.8 (3)
F2—C2—C3—F3160.76 (18)F44—C33—C34—F47158.8 (2)
C1—C2—C3—F440.3 (3)F44—C33—C34—C3537.3 (3)
C1—C2—C3—C4161.8 (2)F45—C33—C34—F46158.4 (2)
F4—C3—C4—F6i59.0 (4)F45—C33—C34—F4741.0 (3)
F3—C3—C4—C5i62.9 (3)F45—C33—C34—C3580.6 (3)
F4—C3—C4—F5i179.4 (4)C32—C33—C34—F4637.2 (3)
C2—C3—C4—C5i175.1 (3)C32—C33—C34—F4780.2 (3)
F3—C3—C4—F6i175.3 (3)C32—C33—C34—C35158.3 (2)
F4—C3—C4—C5i53.4 (3)F46—C34—C35—F4847.8 (3)
C2—C3—C4—F5i57.7 (4)F46—C34—C35—F49166.6 (2)
F3—C3—C4—F5i64.3 (4)F46—C34—C35—C3672.2 (3)
C2—C3—C4—F6i62.7 (4)F47—C34—C35—F48165.0 (2)
F6i—C4—C5i—C6i176.6 (6)F47—C34—C35—F4976.2 (3)
C3—C4—C5i—C6i60.3 (5)F47—C34—C35—C3645.0 (3)
F5i—C4—C5i—C6i67.4 (6)C33—C34—C35—F4873.7 (3)
C3—C4—C5i—F8i65.1 (4)C33—C34—C35—F4945.1 (3)
F5i—C4—C5i—F8i167.2 (5)C33—C34—C35—C36166.3 (3)
F6i—C4—C5i—F8i51.3 (5)F48—C35—C36—F5049.6 (3)
C3—C4—C5i—F7i179.9 (3)F48—C35—C36—F5170.0 (3)
F6i—C4—C5i—F7i63.6 (5)F48—C35—C36—F52169.0 (2)
F5i—C4—C5i—F7i52.4 (5)F49—C35—C36—F5067.9 (3)
F7i—C5i—C6i—F10i80.8 (6)F49—C35—C36—F51172.5 (2)
F7i—C5i—C6i—F9i161.9 (9)F49—C35—C36—F5251.5 (3)
F8i—C5i—C6i—C771.6 (6)C34—C35—C36—F50170.3 (2)
F7i—C5i—C6i—C744.7 (7)C34—C35—C36—F5150.8 (3)
F8i—C5i—C6i—F9i45.6 (10)C34—C35—C36—F5270.3 (3)
Symmetry codes: (i) x, y+1, z; (ii) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C20—H20A···F29i0.982.472.977 (3)112
C20—H20A···O30.982.592.953 (3)102
C22—H22A···F42ii0.982.422.997 (3)117
C22—H22A···O20.982.572.922 (3)101
C22—H22C···F270.982.483.363 (3)150
C41—H41A···O18iii0.982.553.299 (4)133
C42—H42A···F1iv0.982.523.371 (3)145
C42—H42C···O100.982.443.344 (4)153
C43—H43C···O9v0.982.563.424 (4)147
C44—H44A···F14vi0.982.433.313 (3)150
C44—H44C···O140.982.582.920 (3)100
Symmetry codes: (i) x, y+1, z; (ii) x1, y, z; (iii) x+2, y, z; (iv) x+1, y, z; (v) x+1, y1, z; (vi) x, y1, z.

Experimental details

Crystal data
Chemical formula[Ru2(C7F13O2)2(C2H6OS)2(CO)4]
Mr1196.60
Crystal system, space groupTriclinic, P1
Temperature (K)123
a, b, c (Å)10.3430 (5), 14.1199 (8), 25.3010 (13)
α, β, γ (°)101.243 (3), 90.478 (2), 90.830 (2)
V3)3623.5 (3)
Z4
Radiation typeMo Kα
µ (mm1)1.13
Crystal size (mm)0.34 × 0.29 × 0.09
Data collection
DiffractometerBruker APEXII CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2008)
Tmin, Tmax0.703, 0.901
No. of measured, independent and
observed [I > 2σ(I)] reflections
86914, 13225, 11061
Rint0.038
(sin θ/λ)max1)0.605
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.053, 1.04
No. of reflections13225
No. of parameters1225
No. of restraints24
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.73, 0.48

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008) and SHELXLE (Hübschle et al., 2011), PLATON (Spek, 2009) and enCIFer (Allen et al., 2004).

Selected geometric parameters (Å, º) top
Ru1—Ru22.6907 (4)Ru2—C161.852 (3)
Ru1—S12.4164 (8)Ru2—C181.856 (3)
Ru1—O12.1476 (17)S1—O91.4761 (19)
Ru1—O32.1256 (18)S2—O101.4789 (19)
Ru1—C151.864 (3)O5—C151.142 (4)
Ru1—C171.850 (3)O6—C161.148 (4)
Ru2—S22.4095 (7)O7—C171.145 (3)
Ru2—O22.1364 (18)O8—C181.146 (4)
Ru2—O42.1515 (17)
Ru2—Ru1—S1165.14 (3)Ru1—Ru2—S2164.70 (3)
Ru2—Ru1—O381.03 (5)Ru1—Ru2—O485.21 (5)
O1—Ru1—O381.58 (7)O2—Ru2—O481.56 (7)
O1—Ru1—C1791.58 (10)O2—Ru2—C1897.19 (10)
O3—Ru1—C1596.76 (10)O4—Ru2—C1692.75 (10)
C15—Ru1—C1790.03 (13)C16—Ru2—C1888.47 (13)
O1—Ru1—Ru2—O215.43 (7)O3—Ru1—Ru2—O415.48 (7)
 

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