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The title compound, catena-poly[[tetrakis(μ-decanoato-κ2O:O′)diruthenium(II,III)(RuRu)]-μ-octanesulfonato-κ2O:O′], [Ru2(C10H19O2)4(C8H17O3S)], is an octane­sulfonate derivative of the mixed-valence complex diruthenium tetradecanoate. The equatorial carboxyl­ate ligands are bidentate, bridging two Ru atoms to form a dinuclear structure. Each of the two independent dinuclear metal complexes in the asymmetric unit is located at an inversion centre. The octane­sulfonate anion bridges the two dinuclear units through axial coordination. The alkyl chains of the carboxyl­ate and sulfonate ligands are arranged in a parallel manner. The global structure can be seen as infinite chains of polar moieties separated by a double layer of non-polar alkyl groups, without interdigitation of the alkyl chains.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101021540/da1217sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101021540/da1217Isup2.hkl
Contains datablock I

CCDC reference: 182967

Comment top

Mixed-valence diruthenium(II,III) tetracarboxylates, [Ru2(O2CR)4X] (X- is an anion), have been extensively studied in recent years because they exhibit interesting electronic structures, spectroscopic features, magnetic behaviour and liquid crystalline (LC) properties (Aquino, 1998). In particular, LC phases (mesophases) have been obtained with long-chain carboxylates, provided that an appropriate combination of the equatorial carboxylate (RC2-) and axial anion (X-) is used (Cukiernik, Ibn-Elhaj et al., 1998; Chaia et al., 1999; Caplan et al., 1999). For example, aliphatic equatorial carboxylates combined with long-chain axial anions, such as dodecylsulfate or an aliphatic carboxylate, induce mesomorphic behaviour (Cukiernik, Ibn-Elhaj et al., 1998). In some of these cases, a model describing the structural changes taking place through the phase transition has been proposed. As is usual in LC work, these models were based on the structural parameters of the LC phase (obtained from powder X-ray diffraction experiments), on information provided by local spectroscopic probes and on the crystalline structure of short chain (non-mesogenic) analogues.

Of the more than 30 structures of mixed-valence diruthenium carboxylates that are known, the great majority deal with short chain analogues (Bennett et al., 1969; Bino et al., 1979, Togano et al., 1980, Cotton et al., 1988, Barral et al., 1997). The longest chain [Ru2(O2CR)4X] compound for which the molecular structure is known is the non-mesogenic pentanoate derivative [Ru2(O2C(CH2)3CH3)4Cl] (Cukiernik, Luneau et al., 1998). We have now determined the structure of the title ruthenium decanoate derivative with octanesulfonate as the axial anion, [Ru2{O2C(CH2)8CH3}4{O3S(CH2)7CH3}], (I). This compound is particularly interesting, as it undergoes a transition to a thermotropic hexagonal columnar LC phase at 458 K. We are confident that the crystal structure information we report here will be useful when interpreting the structure of the mesophase of the whole [Ru2{O2C(CH2)n-2CH3}4{O3S(CH2)7CH3}] series of compounds with n = ?-? Please supply range for n. Is the -2 necessary?. \sch

In compound (I), a Ru25+ metallic centre is bridged by four carboxylate equatorial ligands; the axial positions are occupied by the octanesulfonate anion. The unit cell contains two independent dinuclear complexes, each one located at a crystallographic inversion centre. The Ru atoms are in an environment of approximately C4v symmetry, while the dinuclear structure exhibits approximate D4 h symmetry.

The Ru—O equatorial bond distances are in the range 2.019–2.034 Å. The average O—C—O bond angle of the carboxylate ligands is 123.1 (3)°, and the Oi—Ruj—Ruj' angles (i = 11, 12, 13, 14, 21, 22, 23 or 24 and j = 1 or 2) are nearly 90°. Thus, the pseudo-octahedral environment of the Ru atoms is not significantly distorted, indicating that the dinuclear structure is achieved with little stress around the metal centres.

The Ru—Ru' distance is 2.271 (3) Å (averaged for the two independent dinuclear units), a typical value for mixed-valence diruthenium carboxylates axially coordinated by O atoms (Aquino, 1998). Four alkyl chains from carboxylate ligands are oriented towards the periphery of the polar centre in a zigzag conformation. Two of them are completely extended, while the others rotate around the β-C atom (C12 and C32) in order to align with the former chains. The alkyl chain of the sulfonate ligand also aligns in an extended conformation parallel to the carboxylic alkyl chains.

The alkylsulfonate moiety acts as a bidentate ligand bridging two independent dinuclear units (Fig. 1). The three S—O distances are consistent with double bonds, although the S—O3 bond is significantly shorter than the other two. This can be ascribed to a slight softening of the S—O bonds involved in coordination to the Ru centres (S—O1 and S—O2), arising from p back-donation.

Due to the bridging nature of the octanesulfonate axial anion, the bimetallic centres polymerize in an infinite chain nearly parallel to the b axis. An intermolecular distance along the polymeric structure of 6.755 Å can be calculated, being the distance between two neighbouring dinuclear centres. The corresponding Ru—Ru axes are nearly perpendicular one to each other (91.94°). However, all the aliphatic chains (both carboxylic and sulfonic) of each such polymeric structure are parallel, without interdigitation.

In the global structure, polar chains composed of dinuclear centres and sulfonate axial ligands are separated by non-polar double layers of alkyl chains. An interlayer separation of 26.6 Å can be inferred from the distance between adjacent ab faces. There is no interdigitation between adjacent layers.

Experimental top

[Ru2{O2C(CH2)8CH3}4Cl] was synthesized following a method already reported for other homologues of this series (Cukiernik. Luneau et al., 1998). Compound (I) was obtained by a metathesis reaction. A methanol suspension of [Ag{O3S(CH2)7CH3}] (150 mg) was slowly added to [Ru2{O2(CH2)8CH3}4Cl] (418 mg) dissolved in methanol. The reaction was protected from light and refluxed for 3 h under nitrogen. The AgCl by-product was filtered off while still hot and the solvent was evaporated under vacuum. The pale-brown solid obtained was dissolved in CH2Cl2, the solution was filtered on a 0.2 mm porous membrane and, after addition of heptane, the CH2Cl2 was evaporated under vacuum. After a couple of hours, a pale-brown solid was filtered, and then washed by suspension on ethylic ether and on distilled water. Brown crystals of (I) were obtained by slow evaporation of a methanolic solution. Characterization was performed by IR spectroscopy (KBr pellets) on an FT—IR Nicolet 150P and by elemental analysis on a Carlo Erba EA1108 analyzer. IR spectroscopic analysis (ν, cm1-): 1249 (m) (nS—O SO3), 1115 (s) (nS—O SO3); analysis calculated for Ru2C48H95SO11: C 53.36, S 2.97, H 8.68%; found: C 53.50, S 2.26, H 8.63%; calculated for Ru2C40H76ClO8: C 52.07, H 8.30%; found: C 51.31, H 8.39%.

Refinement top

The carboxylate chain labelled C11—C19 is disordered. During the refinement, the corresponding occupancies were allowed to vary so as to add up to 1.0 and the C—C bond distances were restrained to a target value of 1.51 (1) Å. Several H atoms were located in a Fourier difference map. However, they were positioned stereochemically and refined with the riding model. The methyl H atoms were treated in the refinement as rigid bodies and allowed to rotate around the corresponding C—C bond so as to maximize the sum of the observed electron density at the three calculated H-atom positions. As expected, all methyl groups converged to staggered conformations.

Computing details top

Data collection: DENZO and SCALEPACK (Otwinowski & Minor, 1997); cell refinement: SCALEPACK; 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: PLATON (Spek, 1998); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. The crystal packing of (I) viewed down a, showing the non-H atom labelling. Only the most populated (61% occupancy) of the two conformations of the C1n chain is shown for clarity.
catena-poly[[tetrakis(decanoato-κ2O:O')diruthenium(II,III)(Ru—Ru)]- µ-octanesulfonato-κ2-O:O'] top
Crystal data top
[Ru2(C10H19O2)4(C8H17O3S)]Z = 2
Mr = 1080.43F(000) = 1146
Triclinic, P1Dx = 1.321 Mg m3
a = 8.0020 (1) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.3040 (4) ÅCell parameters from 8725 reflections
c = 26.7230 (6) Åθ = 1.0–27.5°
α = 83.427 (2)°µ = 0.65 mm1
β = 85.045 (1)°T = 120 K
γ = 74.051 (1)°Thin plate, red
V = 2712.9 (1) Å30.40 × 0.18 × 0.06 mm
Data collection top
Nonius KappaCCD area-detector
diffractometer
11539 independent reflections
Radiation source: fine-focus sealed tube8728 reflections with I > 2σ(I)
Horizontally mounted graphite crystal monochromatorRint = 0.084
Detector resolution: 9 pixels mm-1θmax = 27.5°, θmin = 1.5°
CCD scansh = 1010
Absorption correction: numerical
(Spek, 1990)
k = 1717
Tmin = 0.782, Tmax = 0.965l = 3430
31736 measured reflections
Refinement top
Refinement on F2Primary atom site location: Patterson
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.155H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.0748P)2 + 2.5168P]
where P = (Fo2 + 2Fc2)/3
11539 reflections(Δ/σ)max = 0.124
647 parametersΔρmax = 1.04 e Å3
18 restraintsΔρmin = 1.67 e Å3
Crystal data top
[Ru2(C10H19O2)4(C8H17O3S)]γ = 74.051 (1)°
Mr = 1080.43V = 2712.9 (1) Å3
Triclinic, P1Z = 2
a = 8.0020 (1) ÅMo Kα radiation
b = 13.3040 (4) ŵ = 0.65 mm1
c = 26.7230 (6) ÅT = 120 K
α = 83.427 (2)°0.40 × 0.18 × 0.06 mm
β = 85.045 (1)°
Data collection top
Nonius KappaCCD area-detector
diffractometer
11539 independent reflections
Absorption correction: numerical
(Spek, 1990)
8728 reflections with I > 2σ(I)
Tmin = 0.782, Tmax = 0.965Rint = 0.084
31736 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04918 restraints
wR(F2) = 0.155H-atom parameters constrained
S = 1.11(Δ/σ)max = 0.124
11539 reflectionsΔρmax = 1.04 e Å3
647 parametersΔρmin = 1.67 e Å3
Special details top

Experimental. The crystals grow in the form of thin plates parallel to (001), that can be easily bent without breaking the crystal.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ru10.54718 (4)0.56896 (2)0.481342 (11)0.02727 (10)
O110.7762 (3)0.5099 (2)0.51494 (11)0.0358 (7)
C100.7978 (5)0.4231 (4)0.54323 (16)0.0354 (10)
C110.9650 (13)0.3702 (12)0.5682 (4)0.031 (3)0.610 (6)
H11A1.06300.36280.54240.038*0.610 (6)
H11B0.96160.29870.58260.038*0.610 (6)
C120.9986 (9)0.4295 (6)0.6099 (2)0.0351 (17)0.610 (6)
H12A1.12290.40270.61740.042*0.610 (6)
H12B0.97820.50450.59710.042*0.610 (6)
C130.8889 (13)0.4225 (8)0.6589 (3)0.043 (2)0.610 (6)
H13A0.76410.45060.65210.052*0.610 (6)
H13B0.90850.34790.67230.052*0.610 (6)
C140.9331 (17)0.4832 (9)0.6980 (3)0.047 (3)0.610 (6)
H14A0.89800.55890.68630.057*0.610 (6)
H14B1.06090.46220.70070.057*0.610 (6)
C150.8477 (11)0.4672 (7)0.7497 (3)0.049 (2)0.610 (6)
H15A0.87920.39120.76100.059*0.610 (6)
H15B0.71980.49060.74740.059*0.610 (6)
C160.898 (3)0.5251 (14)0.7891 (4)0.061 (5)0.610 (6)
H16A0.85840.60140.77890.073*0.610 (6)
H16B1.02630.50570.78940.073*0.610 (6)
C170.8251 (13)0.5048 (8)0.8420 (3)0.070 (3)0.610 (6)
H17A0.85870.42810.85150.083*0.610 (6)
H17B0.69640.52800.84210.083*0.610 (6)
C180.883 (2)0.5580 (9)0.8820 (4)0.070 (6)0.610 (6)
H18A1.01180.53560.88170.084*0.610 (6)
H18B0.84780.63490.87290.084*0.610 (6)
C190.8103 (19)0.5350 (10)0.9348 (4)0.109 (5)0.610 (6)
H19A0.68360.54830.93470.163*0.610 (6)
H19B0.83820.58050.95740.163*0.610 (6)
H19C0.86170.46130.94670.163*0.610 (6)
C11'0.9790 (15)0.389 (2)0.5618 (5)0.046 (8)0.390 (6)
H11C1.03870.44560.55240.056*0.390 (6)
H11D1.04780.32520.54660.056*0.390 (6)
C12'0.9605 (15)0.3684 (9)0.6185 (4)0.037 (3)0.390 (6)
H12C0.86940.33090.62720.045*0.390 (6)
H12D1.07160.32180.63060.045*0.390 (6)
C13'0.914 (2)0.4671 (10)0.6458 (4)0.041 (4)0.390 (6)
H13C0.99790.50850.63440.049*0.390 (6)
H13D0.79670.51040.63650.049*0.390 (6)
C14'0.914 (3)0.4445 (11)0.7027 (5)0.047 (5)0.390 (6)
H14C1.02510.39270.71100.056*0.390 (6)
H14D0.81940.41050.71380.056*0.390 (6)
C15'0.8910 (18)0.5362 (10)0.7336 (5)0.051 (4)0.390 (6)
H15C0.77630.58650.72730.061*0.390 (6)
H15D0.98180.57270.72190.061*0.390 (6)
C16'0.902 (5)0.5052 (17)0.7897 (5)0.067 (10)0.390 (6)
H16C1.01530.45330.79570.080*0.390 (6)
H16D0.80940.47000.80130.080*0.390 (6)
C17'0.884 (2)0.5948 (12)0.8214 (5)0.063 (4)0.390 (6)
H17C0.97350.63200.80930.076*0.390 (6)
H17D0.76830.64520.81710.076*0.390 (6)
C18'0.904 (7)0.558 (2)0.8766 (6)0.143 (19)0.390 (6)
H18C0.81400.52100.88850.172*0.390 (6)
H18D1.01910.50720.88070.172*0.390 (6)
C19'0.887 (3)0.6458 (19)0.9092 (7)0.115 (8)0.390 (6)
H19D0.97380.68420.89720.172*0.390 (6)
H19E0.90730.61650.94420.172*0.390 (6)
H19F0.77020.69390.90740.172*0.390 (6)
O120.4468 (3)0.6485 (2)0.54201 (10)0.0304 (6)
C200.3667 (5)0.6064 (3)0.57747 (15)0.0291 (9)
C210.2839 (6)0.6692 (3)0.62074 (15)0.0343 (9)
H21A0.15640.67910.62180.041*
H21B0.30550.73940.61450.041*
C220.3498 (6)0.6192 (3)0.67198 (15)0.0354 (9)
H22A0.31940.55160.68010.042*
H22B0.47820.60460.67080.042*
C230.2702 (7)0.6911 (4)0.71269 (16)0.0476 (12)
H23A0.14240.70260.71420.057*
H23B0.29440.75990.70270.057*
C240.3337 (7)0.6522 (4)0.76535 (16)0.0494 (13)
H24A0.29720.58790.77750.059*
H24B0.46250.63360.76370.059*
C250.2623 (9)0.7344 (4)0.80275 (18)0.0670 (18)
H25A0.29600.79920.78970.080*
H25B0.13360.75160.80450.080*
C260.3244 (9)0.7012 (4)0.85593 (18)0.0680 (18)
H26A0.45310.67690.85410.082*
H26B0.27950.64130.87070.082*
C270.2657 (11)0.7895 (5)0.8907 (2)0.088 (2)
H27A0.30780.85010.87550.105*
H27B0.13680.81250.89320.105*
C280.3314 (11)0.7577 (5)0.9436 (2)0.089 (2)
H28A0.45870.72590.94100.106*
H28B0.27620.70390.96070.106*
C290.2913 (12)0.8519 (6)0.9757 (2)0.109 (3)
H29A0.34250.90630.95840.163*
H29B0.34090.82861.00860.163*
H29C0.16490.88050.98040.163*
O130.3190 (4)0.6253 (2)0.44773 (10)0.0349 (7)
O140.6494 (4)0.4866 (2)0.42149 (10)0.0339 (7)
Ru20.12772 (4)0.94178 (2)0.489274 (12)0.02826 (10)
O210.2279 (4)1.0638 (2)0.46494 (10)0.0296 (6)
O220.0445 (4)0.9479 (2)0.41892 (10)0.0319 (6)
O230.0241 (4)0.8202 (2)0.51409 (10)0.0296 (6)
C300.1327 (6)0.8421 (3)0.53318 (14)0.0303 (9)
C310.2082 (6)0.7551 (3)0.55553 (15)0.0328 (9)
H31A0.11240.69150.56340.039*
H31B0.27860.73900.53040.039*
C320.3221 (6)0.7817 (3)0.60336 (15)0.0359 (10)
H32A0.36340.71990.61710.043*
H32B0.42560.83980.59450.043*
C330.2308 (6)0.8135 (4)0.64418 (16)0.0398 (10)
H33A0.12160.75800.65050.048*
H33B0.19840.87870.63110.048*
C340.3335 (7)0.8316 (4)0.69354 (18)0.0523 (13)
H34A0.35230.76400.70900.063*
H34B0.44920.88020.68690.063*
C350.2485 (7)0.8764 (4)0.73094 (16)0.0496 (13)
H35A0.23820.94640.71630.060*
H35B0.12900.83070.73520.060*
C360.3418 (9)0.8878 (6)0.7826 (2)0.078 (2)
H36A0.46460.92780.77830.094*
H36B0.34160.81700.79880.094*
C370.2641 (8)0.9419 (5)0.81750 (19)0.0681 (18)
H37A0.26921.01380.80190.082*
H37B0.13980.90380.82050.082*
C380.3520 (11)0.9496 (7)0.8704 (2)0.111 (3)
H38A0.47800.98330.86770.133*
H38B0.33880.87780.88730.133*
C390.2775 (11)1.0119 (6)0.9028 (2)0.106 (3)
H39A0.15710.97380.90970.159*
H39B0.34751.02130.93480.159*
H39C0.28001.08080.88490.159*
O240.2043 (4)0.9355 (2)0.55986 (10)0.0321 (6)
C400.1036 (6)0.9907 (3)0.59170 (15)0.0315 (9)
C410.1579 (6)0.9777 (3)0.64436 (15)0.0387 (10)
H41A0.28580.96580.64320.046*
H41B0.13120.91360.66170.046*
C420.0754 (7)1.0681 (3)0.67596 (15)0.0408 (11)
H42A0.09941.13320.65900.049*
H42B0.05241.07880.67910.049*
C430.1462 (8)1.0462 (4)0.72793 (18)0.0584 (15)
H43A0.27381.03590.72420.070*
H43B0.12490.97960.74390.070*
C440.0690 (8)1.1315 (4)0.76321 (17)0.0609 (16)
H44A0.09121.19820.74780.073*
H44B0.05871.14220.76720.073*
C450.1444 (9)1.1048 (5)0.81501 (19)0.078 (2)
H45A0.27191.09460.81070.094*
H45B0.12361.03740.83000.094*
C460.0688 (9)1.1879 (5)0.85182 (18)0.084 (2)
H46A0.09111.25520.83740.101*
H46B0.05891.19870.85620.101*
C470.1473 (10)1.1566 (6)0.9034 (2)0.096 (3)
H47A0.27471.14680.89890.115*
H47B0.12701.08840.91730.115*
C480.0718 (12)1.2373 (7)0.9411 (2)0.117 (4)
H48A0.05541.24680.94630.141*
H48B0.09181.30570.92760.141*
C490.1573 (13)1.2014 (8)0.9919 (2)0.149 (5)
H49A0.14031.13271.00490.223*
H49B0.10391.25261.01620.223*
H49C0.28221.19580.98710.223*
S0.52875 (17)0.81235 (9)0.42757 (4)0.0417 (3)
O10.6311 (4)0.7040 (2)0.44037 (11)0.0327 (6)
O20.3906 (4)0.8406 (2)0.46754 (11)0.0409 (7)
O30.6357 (6)0.8829 (3)0.41500 (14)0.0628 (11)
C500.4225 (7)0.8121 (4)0.37157 (18)0.0496 (12)
H50A0.32730.77760.38020.060*
H50B0.36920.88560.35840.060*
C510.5419 (7)0.7568 (5)0.33057 (17)0.0543 (14)
H51A0.58820.68190.34270.065*
H51B0.64160.78780.32350.065*
C520.4525 (8)0.7641 (5)0.28188 (18)0.0607 (16)
H52A0.34200.74430.29010.073*
H52B0.42260.83820.26720.073*
C530.5556 (9)0.6972 (4)0.24270 (18)0.0677 (18)
H53A0.57670.62270.25630.081*
H53B0.67030.71260.23660.081*
C540.4730 (9)0.7112 (5)0.19292 (19)0.076 (2)
H54A0.35440.70180.19970.091*
H54B0.46000.78470.17850.091*
C550.5641 (11)0.6408 (5)0.1535 (2)0.090 (3)
H55A0.57270.56730.16720.108*
H55B0.68430.64800.14750.108*
C560.4825 (13)0.6593 (6)0.1039 (2)0.112 (3)
H56A0.36210.65240.11000.134*
H56B0.47440.73270.09010.134*
C570.5743 (14)0.5878 (6)0.0643 (2)0.136 (4)
H57A0.69830.58540.06130.204*
H57B0.52310.61460.03180.204*
H57C0.56130.51690.07400.204*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.01993 (18)0.03526 (19)0.02970 (18)0.00955 (13)0.00094 (13)0.01225 (13)
O110.0189 (15)0.0479 (18)0.0449 (17)0.0099 (13)0.0035 (13)0.0183 (14)
C100.020 (2)0.053 (3)0.033 (2)0.0045 (19)0.0011 (18)0.018 (2)
C110.020 (5)0.041 (5)0.036 (5)0.011 (4)0.006 (4)0.015 (5)
C120.024 (4)0.041 (4)0.040 (4)0.009 (3)0.004 (3)0.002 (3)
C130.032 (5)0.057 (6)0.034 (5)0.001 (5)0.004 (4)0.003 (4)
C140.047 (6)0.051 (7)0.044 (5)0.012 (6)0.005 (4)0.006 (5)
C150.042 (5)0.053 (5)0.046 (5)0.001 (4)0.005 (4)0.010 (4)
C160.064 (11)0.051 (7)0.067 (12)0.003 (7)0.024 (8)0.016 (6)
C170.068 (7)0.081 (7)0.044 (5)0.017 (5)0.019 (5)0.022 (5)
C180.084 (11)0.068 (10)0.046 (8)0.010 (8)0.021 (8)0.026 (7)
C190.140 (13)0.099 (10)0.063 (7)0.026 (9)0.028 (8)0.035 (7)
C11'0.022 (10)0.073 (17)0.038 (10)0.005 (9)0.004 (8)0.002 (8)
C12'0.026 (6)0.045 (7)0.042 (7)0.012 (5)0.013 (5)0.006 (5)
C13'0.040 (9)0.049 (9)0.026 (7)0.000 (7)0.008 (6)0.002 (6)
C14'0.074 (12)0.027 (8)0.043 (8)0.022 (8)0.006 (7)0.007 (6)
C15'0.048 (8)0.058 (9)0.048 (8)0.012 (7)0.003 (6)0.018 (7)
C16'0.10 (2)0.064 (16)0.028 (12)0.014 (13)0.009 (12)0.006 (8)
C17'0.066 (10)0.078 (11)0.045 (8)0.017 (8)0.001 (7)0.011 (7)
C18'0.23 (5)0.15 (4)0.07 (2)0.08 (3)0.00 (3)0.01 (2)
C19'0.120 (19)0.17 (2)0.069 (12)0.042 (17)0.007 (12)0.048 (14)
O120.0258 (15)0.0345 (15)0.0327 (15)0.0076 (12)0.0019 (12)0.0124 (12)
C200.019 (2)0.036 (2)0.033 (2)0.0066 (16)0.0004 (17)0.0111 (17)
C210.030 (2)0.039 (2)0.033 (2)0.0038 (18)0.0006 (18)0.0124 (17)
C220.038 (3)0.036 (2)0.031 (2)0.0069 (18)0.0028 (19)0.0092 (17)
C230.052 (3)0.051 (3)0.033 (2)0.003 (2)0.010 (2)0.013 (2)
C240.065 (4)0.041 (3)0.035 (2)0.002 (2)0.009 (2)0.008 (2)
C250.090 (5)0.057 (3)0.037 (3)0.018 (3)0.021 (3)0.017 (2)
C260.094 (5)0.058 (3)0.036 (3)0.011 (3)0.014 (3)0.013 (2)
C270.137 (7)0.067 (4)0.037 (3)0.024 (4)0.034 (4)0.018 (3)
C280.127 (6)0.082 (5)0.038 (3)0.015 (4)0.029 (4)0.018 (3)
C290.180 (9)0.090 (5)0.041 (3)0.004 (5)0.032 (4)0.023 (3)
O130.0240 (16)0.0473 (18)0.0327 (15)0.0050 (13)0.0035 (13)0.0107 (13)
O140.0256 (16)0.0435 (17)0.0364 (15)0.0123 (13)0.0045 (13)0.0167 (13)
Ru20.0346 (2)0.02031 (16)0.02742 (17)0.00524 (13)0.00640 (14)0.00361 (12)
O210.0337 (16)0.0229 (13)0.0312 (14)0.0075 (11)0.0045 (12)0.0036 (11)
O220.0388 (17)0.0249 (14)0.0286 (14)0.0047 (12)0.0029 (13)0.0021 (11)
O230.0342 (16)0.0211 (13)0.0321 (14)0.0072 (11)0.0101 (13)0.0058 (11)
C300.040 (3)0.025 (2)0.0271 (19)0.0115 (17)0.0020 (18)0.0046 (15)
C310.038 (2)0.030 (2)0.032 (2)0.0118 (18)0.0004 (19)0.0034 (17)
C320.038 (3)0.037 (2)0.033 (2)0.0119 (19)0.0014 (19)0.0001 (17)
C330.045 (3)0.043 (3)0.033 (2)0.014 (2)0.000 (2)0.0043 (18)
C340.048 (3)0.065 (3)0.038 (3)0.004 (2)0.003 (2)0.014 (2)
C350.054 (3)0.053 (3)0.032 (2)0.002 (2)0.001 (2)0.006 (2)
C360.069 (4)0.116 (6)0.040 (3)0.001 (4)0.006 (3)0.034 (3)
C370.080 (4)0.071 (4)0.036 (3)0.012 (3)0.005 (3)0.014 (3)
C380.097 (6)0.168 (8)0.051 (4)0.008 (5)0.002 (4)0.051 (5)
C390.147 (8)0.103 (6)0.044 (3)0.021 (5)0.023 (4)0.029 (4)
O240.0374 (17)0.0237 (14)0.0309 (14)0.0030 (12)0.0053 (13)0.0030 (11)
C400.042 (3)0.0216 (19)0.029 (2)0.0090 (17)0.0086 (18)0.0002 (15)
C410.051 (3)0.028 (2)0.031 (2)0.0009 (19)0.000 (2)0.0010 (17)
C420.051 (3)0.034 (2)0.030 (2)0.000 (2)0.002 (2)0.0031 (17)
C430.080 (4)0.045 (3)0.035 (2)0.012 (3)0.009 (3)0.007 (2)
C440.072 (4)0.061 (3)0.032 (2)0.015 (3)0.003 (3)0.011 (2)
C450.100 (5)0.074 (4)0.030 (3)0.028 (4)0.006 (3)0.011 (3)
C460.100 (5)0.092 (5)0.029 (3)0.037 (4)0.014 (3)0.021 (3)
C470.113 (6)0.104 (5)0.035 (3)0.038 (4)0.014 (3)0.016 (3)
C480.145 (8)0.133 (7)0.030 (3)0.048 (6)0.013 (4)0.030 (4)
C490.174 (10)0.194 (10)0.029 (3)0.045 (7)0.020 (5)0.027 (5)
S0.0465 (7)0.0398 (6)0.0407 (6)0.0133 (5)0.0043 (5)0.0119 (5)
O10.0269 (16)0.0337 (15)0.0384 (16)0.0082 (12)0.0002 (13)0.0080 (12)
O20.0450 (19)0.0381 (17)0.0324 (15)0.0007 (14)0.0065 (14)0.0100 (13)
O30.088 (3)0.056 (2)0.055 (2)0.041 (2)0.026 (2)0.0176 (17)
C500.052 (3)0.048 (3)0.041 (3)0.000 (2)0.000 (2)0.008 (2)
C510.048 (3)0.074 (4)0.035 (2)0.000 (3)0.002 (2)0.022 (2)
C520.062 (4)0.073 (4)0.035 (2)0.009 (3)0.009 (3)0.016 (2)
C530.092 (5)0.062 (4)0.036 (3)0.009 (3)0.013 (3)0.015 (2)
C540.101 (5)0.074 (4)0.034 (3)0.012 (3)0.015 (3)0.011 (3)
C550.134 (7)0.071 (4)0.039 (3)0.027 (4)0.023 (4)0.020 (3)
C560.175 (9)0.094 (5)0.039 (3)0.024 (5)0.033 (4)0.026 (3)
C570.240 (11)0.080 (5)0.047 (4)0.046 (6)0.047 (5)0.027 (3)
Geometric parameters (Å, º) top
Ru1—O122.023 (3)Ru2—O242.019 (3)
Ru1—O142.028 (3)Ru2—O212.021 (3)
Ru1—O132.020 (3)Ru2—O232.035 (3)
Ru1—O112.029 (3)Ru2—O222.034 (3)
Ru1—O12.228 (3)Ru2—O22.233 (3)
Ru1—Ru1i2.2680 (6)Ru2—Ru2ii2.2732 (6)
O11—C101.284 (5)O21—C30ii1.278 (5)
C10—O13i1.265 (5)O22—C40ii1.275 (5)
C10—C111.504 (8)O23—C301.282 (5)
C10—C11'1.505 (9)C30—O21ii1.278 (5)
C11—C121.518 (9)C30—C311.491 (6)
C11—H11A0.9900C31—C321.521 (6)
C11—H11B0.9900C31—H31A0.9900
C12—C131.522 (8)C31—H31B0.9900
C12—H12A0.9900C32—C331.522 (6)
C12—H12B0.9900C32—H32A0.9900
C13—C141.510 (8)C32—H32B0.9900
C13—H13A0.9900C33—C341.500 (6)
C13—H13B0.9900C33—H33A0.9900
C14—C151.507 (8)C33—H33B0.9900
C14—H14A0.9900C34—C351.515 (7)
C14—H14B0.9900C34—H34A0.9900
C15—C161.514 (9)C34—H34B0.9900
C15—H15A0.9900C35—C361.515 (7)
C15—H15B0.9900C35—H35A0.9900
C16—C171.504 (9)C35—H35B0.9900
C16—H16A0.9900C36—C371.508 (8)
C16—H16B0.9900C36—H36A0.9900
C17—C181.516 (8)C36—H36B0.9900
C17—H17A0.9900C37—C381.524 (8)
C17—H17B0.9900C37—H37A0.9900
C18—C191.512 (9)C37—H37B0.9900
C18—H18A0.9900C38—C391.52 (1)
C18—H18B0.9900C38—H38A0.9900
C19—H19A0.9800C38—H38B0.9900
C19—H19B0.9800C39—H39A0.9800
C19—H19C0.9800C39—H39B0.9800
C11'—C12'1.51 (1)C39—H39C0.9800
C11'—H11C0.9900O24—C401.270 (5)
C11'—H11D0.9900C40—O22ii1.275 (5)
C12'—C13'1.516 (9)C40—C411.486 (5)
C12'—H12C0.9900C41—C421.515 (6)
C12'—H12D0.9900C41—H41A0.9900
C13'—C14'1.516 (9)C41—H41B0.9900
C13'—H13C0.9900C42—C431.512 (6)
C13'—H13D0.9900C42—H42A0.9900
C14'—C15'1.512 (9)C42—H42B0.9900
C14'—H14C0.9900C43—C441.522 (6)
C14'—H14D0.9900C43—H43A0.9900
C15'—C16'1.51 (1)C43—H43B0.9900
C15'—H15C0.9900C44—C451.523 (7)
C15'—H15D0.9900C44—H44A0.9900
C16'—C17'1.51 (1)C44—H44B0.9900
C16'—H16C0.9900C45—C461.528 (7)
C16'—H16D0.9900C45—H45A0.9900
C17'—C18'1.51 (1)C45—H45B0.9900
C17'—H17C0.9900C46—C471.530 (7)
C17'—H17D0.9900C46—H46A0.9900
C18'—C19'1.51 (1)C46—H46B0.9900
C18'—H18C0.9900C47—C481.525 (8)
C18'—H18D0.9900C47—H47A0.9900
C19'—H19D0.9800C47—H47B0.9900
C19'—H19E0.9800C48—C491.540 (8)
C19'—H19F0.9800C48—H48A0.9900
O12—C201.262 (5)C48—H48B0.9900
C20—O14i1.275 (5)C49—H49A0.9800
C20—C211.502 (5)C49—H49B0.9800
C21—C221.523 (5)C49—H49C0.9800
C21—H21A0.9900S—O31.430 (4)
C21—H21B0.9900S—O11.467 (3)
C22—C231.513 (6)S—O21.471 (3)
C22—H22A0.9900S—C501.785 (5)
C22—H22B0.9900C50—C511.507 (6)
C23—C241.523 (6)C50—H50A0.9900
C23—H23A0.9900C50—H50B0.9900
C23—H23B0.9900C51—C521.519 (6)
C24—C251.526 (6)C51—H51A0.9900
C24—H24A0.9900C51—H51B0.9900
C24—H24B0.9900C52—C531.493 (7)
C25—C261.523 (6)C52—H52A0.9900
C25—H25A0.9900C52—H52B0.9900
C25—H25B0.9900C53—C541.506 (7)
C26—C271.528 (7)C53—H53A0.9900
C26—H26A0.9900C53—H53B0.9900
C26—H26B0.9900C54—C551.495 (7)
C27—C281.524 (7)C54—H54A0.9900
C27—H27A0.9900C54—H54B0.9900
C27—H27B0.9900C55—C561.494 (8)
C28—C291.545 (8)C55—H55A0.9900
C28—H28A0.9900C55—H55B0.9900
C28—H28B0.9900C56—C571.510 (9)
C29—H29A0.9800C56—H56A0.9900
C29—H29B0.9800C56—H56B0.9900
C29—H29C0.9800C57—H57A0.9800
O13—C10i1.265 (5)C57—H57B0.9800
O14—C20i1.275 (5)C57—H57C0.9800
O12—Ru1—O14178.8 (1)O24—Ru2—O22178.6 (1)
O12—Ru1—O1390.8 (1)O21—Ru2—O2288.7 (1)
O14—Ru1—O1389.9 (1)O23—Ru2—O2291.4 (1)
O12—Ru1—O1189.8 (1)O24—Ru2—O289.3 (1)
O14—Ru1—O1189.5 (1)O21—Ru2—O285.5 (1)
O13—Ru1—O11179.0 (1)O23—Ru2—O295.2 (1)
O12—Ru1—O193.1 (1)O22—Ru2—O291.9 (1)
O14—Ru1—O187.8 (1)O24—Ru2—Ru2ii89.59 (8)
O13—Ru1—O187.7 (1)O21—Ru2—Ru2ii89.01 (8)
O11—Ru1—O193.1 (1)O23—Ru2—Ru2ii90.28 (8)
O12—Ru1—Ru1i89.10 (8)O22—Ru2—Ru2ii89.36 (8)
O14—Ru1—Ru1i90.00 (8)O2—Ru2—Ru2ii174.33 (9)
O13—Ru1—Ru1i89.38 (9)C30ii—O21—Ru2119.9 (3)
O11—Ru1—Ru1i89.83 (9)C40ii—O22—Ru2118.7 (3)
O1—Ru1—Ru1i176.36 (7)C30—O23—Ru2117.9 (2)
C10—O11—Ru1118.2 (2)O21ii—C30—O23122.9 (4)
O13i—C10—O11123.0 (3)O21ii—C30—C31117.7 (4)
O13i—C10—C11114.4 (8)O23—C30—C31119.4 (3)
O11—C10—C11122.5 (8)C30—C31—C32112.8 (3)
O13i—C10—C11'127 (1)C30—C31—H31A109.0
O11—C10—C11'110 (1)C32—C31—H31A109.0
C10—C11—C12113.2 (8)C30—C31—H31B109.0
C10—C11—H11A108.9C32—C31—H31B109.0
C12—C11—H11A108.9H31A—C31—H31B107.8
C10—C11—H11B108.9C31—C32—C33114.1 (4)
C12—C11—H11B108.9C31—C32—H32A108.7
H11A—C11—H11B107.7C33—C32—H32A108.7
C13—C12—C11115.8 (9)C31—C32—H32B108.7
C13—C12—H12A108.3C33—C32—H32B108.7
C11—C12—H12A108.3H32A—C32—H32B107.6
C13—C12—H12B108.3C34—C33—C32115.8 (4)
C11—C12—H12B108.3C34—C33—H33A108.3
H12A—C12—H12B107.4C32—C33—H33A108.3
C14—C13—C12111.7 (7)C34—C33—H33B108.3
C14—C13—H13A109.3C32—C33—H33B108.3
C12—C13—H13A109.3H33A—C33—H33B107.4
C14—C13—H13B109.3C33—C34—C35114.4 (4)
C12—C13—H13B109.3C33—C34—H34A108.7
H13A—C13—H13B107.9C35—C34—H34A108.7
C13—C14—C15114.4 (8)C33—C34—H34B108.7
C13—C14—H14A108.7C35—C34—H34B108.7
C15—C14—H14A108.7H34A—C34—H34B107.6
C13—C14—H14B108.7C34—C35—C36115.8 (5)
C15—C14—H14B108.7C34—C35—H35A108.3
H14A—C14—H14B107.6C36—C35—H35A108.3
C14—C15—C16114.1 (9)C34—C35—H35B108.3
C14—C15—H15A108.7C36—C35—H35B108.3
C16—C15—H15A108.7H35A—C35—H35B107.4
C14—C15—H15B108.7C37—C36—C35114.7 (6)
C16—C15—H15B108.7C37—C36—H36A108.6
H15A—C15—H15B107.6C35—C36—H36A108.6
C15—C16—C17116 (1)C37—C36—H36B108.6
C15—C16—H16A108.4C35—C36—H36B108.6
C17—C16—H16A108.4H36A—C36—H36B107.6
C15—C16—H16B108.4C36—C37—C38115.2 (6)
C17—C16—H16B108.4C36—C37—H37A108.5
H16A—C16—H16B107.5C38—C37—H37A108.5
C16—C17—C18116 (1)C36—C37—H37B108.5
C16—C17—H17A108.4C38—C37—H37B108.5
C18—C17—H17A108.4H37A—C37—H37B107.5
C16—C17—H17B108.4C39—C38—C37113.1 (7)
C18—C17—H17B108.4C39—C38—H38A109.0
H17A—C17—H17B107.5C37—C38—H38A109.0
C19—C18—C17114 (1)C39—C38—H38B109.0
C19—C18—H18A108.7C37—C38—H38B109.0
C17—C18—H18A108.7H38A—C38—H38B107.8
C19—C18—H18B108.6C38—C39—H39A109.5
C17—C18—H18B108.6C38—C39—H39B109.5
H18A—C18—H18B107.6H39A—C39—H39B109.5
C10—C11'—C12'106.8 (9)C38—C39—H39C109.5
C10—C11'—H11C110.4H39A—C39—H39C109.5
C12'—C11'—H11C110.4H39B—C39—H39C109.5
C10—C11'—H11D110.4C40—O24—Ru2119.3 (3)
C12'—C11'—H11D110.4O22ii—C40—O24123.0 (4)
H11C—C11'—H11D108.6O22ii—C40—C41119.0 (4)
C13'—C12'—C11'114 (2)O24—C40—C41117.9 (4)
C13'—C12'—H12C108.9C40—C41—C42116.3 (3)
C11'—C12'—H12C108.9C40—C41—H41A108.2
C13'—C12'—H12D108.9C42—C41—H41A108.2
C11'—C12'—H12D108.9C40—C41—H41B108.2
H12C—C12'—H12D107.7C42—C41—H41B108.2
C14'—C13'—C12'113 (1)H41A—C41—H41B107.4
C14'—C13'—H13C109.0C43—C42—C41110.8 (4)
C12'—C13'—H13C109.0C43—C42—H42A109.5
C14'—C13'—H13D109.0C41—C42—H42A109.5
C12'—C13'—H13D109.0C43—C42—H42B109.5
H13C—C13'—H13D107.8C41—C42—H42B109.5
C13'—C14'—C15'118 (1)H42A—C42—H42B108.1
C13'—C14'—H14C107.9C42—C43—C44115.1 (4)
C15'—C14'—H14C107.9C42—C43—H43A108.5
C13'—C14'—H14D107.9C44—C43—H43A108.5
C15'—C14'—H14D107.9C42—C43—H43B108.5
H14C—C14'—H14D107.2C44—C43—H43B108.5
C14'—C15'—C16'114 (1)H43A—C43—H43B107.5
C14'—C15'—H15C108.8C45—C44—C43112.7 (4)
C16'—C15'—H15C108.9C45—C44—H44A109.1
C14'—C15'—H15D108.8C43—C44—H44A109.1
C16'—C15'—H15D108.7C45—C44—H44B109.1
H15C—C15'—H15D107.7C43—C44—H44B109.1
C15'—C16'—C17'115 (1)H44A—C44—H44B107.8
C15'—C16'—H16C108.6C44—C45—C46114.4 (4)
C17'—C16'—H16C108.6C44—C45—H45A108.7
C15'—C16'—H16D108.5C46—C45—H45A108.7
C17'—C16'—H16D108.5C44—C45—H45B108.7
H16C—C16'—H16D107.5C46—C45—H45B108.7
C18'—C17'—C16'112 (1)H45A—C45—H45B107.6
C18'—C17'—H17C109.1C47—C46—C45112.2 (5)
C16'—C17'—H17C109.1C47—C46—H46A109.2
C18'—C17'—H17D109.1C45—C46—H46A109.2
C16'—C17'—H17D109.2C47—C46—H46B109.2
H17C—C17'—H17D107.9C45—C46—H46B109.2
C19'—C18'—C17'114 (2)H46A—C46—H46B107.9
C19'—C18'—H18C108.8C46—C47—C48113.3 (5)
C17'—C18'—H18C108.8C46—C47—H47A108.9
C19'—C18'—H18D108.9C48—C47—H47A108.9
C17'—C18'—H18D108.9C46—C47—H47B108.9
H18C—C18'—H18D107.7C48—C47—H47B108.9
C18'—C19'—H19D109.4H47A—C47—H47B107.7
C18'—C19'—H19E109.5C47—C48—C49110.6 (6)
H19D—C19'—H19E109.5C47—C48—H48A109.5
C18'—C19'—H19F109.5C49—C48—H48A109.5
H19D—C19'—H19F109.5C47—C48—H48B109.5
H19E—C19'—H19F109.5C49—C48—H48B109.5
C20—O12—Ru1119.3 (2)H48A—C48—H48B108.1
O12—C20—O14i123.6 (4)C48—C49—H49A109.5
O12—C20—C21118.6 (4)C48—C49—H49B109.5
O14i—C20—C21117.8 (4)H49A—C49—H49B109.5
C20—C21—C22114.2 (3)C48—C49—H49C109.5
C20—C21—H21A108.7H49A—C49—H49C109.5
C22—C21—H21A108.7H49B—C49—H49C109.5
C20—C21—H21B108.7O3—S—O1112.5 (2)
C22—C21—H21B108.7O3—S—O2116.4 (2)
H21A—C21—H21B107.6O1—S—O2108.32 (18)
C23—C22—C21110.7 (3)O3—S—C50105.8 (3)
C23—C22—H22A109.5O1—S—C50106.7 (2)
C21—C22—H22A109.5O2—S—C50106.5 (2)
C23—C22—H22B109.5S—O1—Ru1129.6 (2)
C21—C22—H22B109.5S—O2—Ru2147.4 (2)
H22A—C22—H22B108.1C51—C50—S113.8 (4)
C22—C23—C24115.6 (4)C51—C50—H50A108.8
C22—C23—H23A108.4S—C50—H50A108.8
C24—C23—H23A108.4C51—C50—H50B108.8
C22—C23—H23B108.4S—C50—H50B108.8
C24—C23—H23B108.4H50A—C50—H50B107.7
H23A—C23—H23B107.4C50—C51—C52113.1 (4)
C25—C24—C23112.1 (4)C50—C51—H51A109.0
C25—C24—H24A109.2C52—C51—H51A109.0
C23—C24—H24A109.2C50—C51—H51B109.0
C25—C24—H24B109.2C52—C51—H51B109.0
C23—C24—H24B109.2H51A—C51—H51B107.8
H24A—C24—H24B107.9C53—C52—C51115.5 (4)
C26—C25—C24114.7 (4)C53—C52—H52A108.4
C26—C25—H25A108.6C51—C52—H52A108.4
C24—C25—H25A108.6C53—C52—H52B108.4
C26—C25—H25B108.6C51—C52—H52B108.4
C24—C25—H25B108.6H52A—C52—H52B107.5
H25A—C25—H25B107.6C52—C53—C54115.4 (5)
C25—C26—C27113.1 (4)C52—C53—H53A108.4
C25—C26—H26A109.0C54—C53—H53A108.4
C27—C26—H26A109.0C52—C53—H53B108.4
C25—C26—H26B109.0C54—C53—H53B108.4
C27—C26—H26B109.0H53A—C53—H53B107.5
H26A—C26—H26B107.8C55—C54—C53117.7 (5)
C28—C27—C26113.3 (5)C55—C54—H54A107.9
C28—C27—H27A108.9C53—C54—H54A107.9
C26—C27—H27A108.9C55—C54—H54B107.9
C28—C27—H27B108.9C53—C54—H54B107.9
C26—C27—H27B108.9H54A—C54—H54B107.2
H27A—C27—H27B107.7C54—C55—C56116.4 (5)
C27—C28—C29112.3 (5)C54—C55—H55A108.2
C27—C28—H28A109.2C56—C55—H55A108.2
C29—C28—H28A109.2C54—C55—H55B108.2
C27—C28—H28B109.2C56—C55—H55B108.2
C29—C28—H28B109.2H55A—C55—H55B107.3
H28A—C28—H28B107.9C57—C56—C55116.3 (6)
C28—C29—H29A109.5C57—C56—H56A108.2
C28—C29—H29B109.5C55—C56—H56A108.2
H29A—C29—H29B109.5C57—C56—H56B108.2
C28—C29—H29C109.5C55—C56—H56B108.2
H29A—C29—H29C109.5H56A—C56—H56B107.4
H29B—C29—H29C109.5C56—C57—H57A109.5
C10i—O13—Ru1119.5 (3)C56—C57—H57B109.5
C20i—O14—Ru1117.9 (3)H57A—C57—H57B109.5
O24—Ru2—O2192.3 (1)C56—C57—H57C109.5
O24—Ru2—O2387.6 (1)H57A—C57—H57C109.5
O21—Ru2—O23179.3 (1)H57B—C57—H57C109.5
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+2, z+1.

Experimental details

Crystal data
Chemical formula[Ru2(C10H19O2)4(C8H17O3S)]
Mr1080.43
Crystal system, space groupTriclinic, P1
Temperature (K)120
a, b, c (Å)8.0020 (1), 13.3040 (4), 26.7230 (6)
α, β, γ (°)83.427 (2), 85.045 (1), 74.051 (1)
V3)2712.9 (1)
Z2
Radiation typeMo Kα
µ (mm1)0.65
Crystal size (mm)0.40 × 0.18 × 0.06
Data collection
DiffractometerNonius KappaCCD area-detector
diffractometer
Absorption correctionNumerical
(Spek, 1990)
Tmin, Tmax0.782, 0.965
No. of measured, independent and
observed [I > 2σ(I)] reflections
31736, 11539, 8728
Rint0.084
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.049, 0.155, 1.11
No. of reflections11539
No. of parameters647
No. of restraints18
H-atom treatmentH-atom parameters constrained
(Δ/σ)max0.124
Δρmax, Δρmin (e Å3)1.04, 1.67

Computer programs: DENZO and SCALEPACK (Otwinowski & Minor, 1997), DENZO and SCALEPACK, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 1998), WinGX (Farrugia, 1999).

Selected geometric parameters (Å, º) top
Ru1—O122.023 (3)Ru2—O232.035 (3)
Ru1—O142.028 (3)Ru2—O222.034 (3)
Ru1—O132.020 (3)Ru2—O22.233 (3)
Ru1—O112.029 (3)Ru2—Ru2ii2.2732 (6)
Ru1—O12.228 (3)O21—C30ii1.278 (5)
Ru1—Ru1i2.2680 (6)O22—C40ii1.275 (5)
O11—C101.284 (5)O23—C301.282 (5)
C10—O13i1.265 (5)C30—O21ii1.278 (5)
C10—C111.504 (8)C30—C311.491 (6)
C10—C11'1.505 (9)C40—O22ii1.275 (5)
O12—C201.262 (5)C40—C411.486 (5)
C20—O14i1.275 (5)S—O31.430 (4)
C20—C211.502 (5)S—O11.467 (3)
O13—C10i1.265 (5)S—O21.471 (3)
O14—C20i1.275 (5)S—C501.785 (5)
Ru2—O242.019 (3)C50—C511.507 (6)
Ru2—O212.021 (3)C51—C521.519 (6)
O12—Ru1—O14178.8 (1)O24—Ru2—O22178.6 (1)
O12—Ru1—O1390.8 (1)O21—Ru2—O2288.7 (1)
O14—Ru1—O1389.9 (1)O23—Ru2—O2291.4 (1)
O12—Ru1—O1189.8 (1)O24—Ru2—O289.3 (1)
O14—Ru1—O1189.5 (1)O21—Ru2—O285.5 (1)
O13—Ru1—O11179.0 (1)O23—Ru2—O295.2 (1)
O12—Ru1—O193.1 (1)O22—Ru2—O291.9 (1)
O14—Ru1—O187.8 (1)O24—Ru2—Ru2ii89.59 (8)
O13—Ru1—O187.7 (1)O21—Ru2—Ru2ii89.01 (8)
O11—Ru1—O193.1 (1)O23—Ru2—Ru2ii90.28 (8)
O12—Ru1—Ru1i89.10 (8)O22—Ru2—Ru2ii89.36 (8)
O14—Ru1—Ru1i90.00 (8)O2—Ru2—Ru2ii174.33 (9)
O13—Ru1—Ru1i89.38 (9)C30ii—O21—Ru2119.9 (3)
O11—Ru1—Ru1i89.83 (9)C40ii—O22—Ru2118.7 (3)
O1—Ru1—Ru1i176.36 (7)C30—O23—Ru2117.9 (2)
C10—O11—Ru1118.2 (2)O21ii—C30—O23122.9 (4)
O13i—C10—O11123.0 (3)O21ii—C30—C31117.7 (4)
O13i—C10—C11114.4 (8)C40—O24—Ru2119.3 (3)
O11—C10—C11122.5 (8)O22ii—C40—O24123.0 (4)
O13i—C10—C11'127 (1)O22ii—C40—C41119.0 (4)
O11—C10—C11'110 (1)O24—C40—C41117.9 (4)
C20—O12—Ru1119.3 (2)O3—S—O1112.5 (2)
O12—C20—O14i123.6 (4)O3—S—O2116.4 (2)
O12—C20—C21118.6 (4)O1—S—O2108.32 (18)
O14i—C20—C21117.8 (4)O3—S—C50105.8 (3)
C10i—O13—Ru1119.5 (3)O1—S—C50106.7 (2)
C20i—O14—Ru1117.9 (3)O2—S—C50106.5 (2)
O24—Ru2—O2192.3 (1)S—O1—Ru1129.6 (2)
O24—Ru2—O2387.6 (1)S—O2—Ru2147.4 (2)
O21—Ru2—O23179.3 (1)C51—C50—S113.8 (4)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+2, z+1.
 

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