Abstract
The molecular geometry of the complex cation in the title structure, [(μ-Cl)3{RuII(η6-C6Me6)}2][FeIIICl4], compares very well with that reported earlier for the corresponding PF6 − salt [Pandey et al. (1999 ▶). J. Organomet. Chem. 592, 278–282]. The [FeCl4]− counter ion has a rather regular tetrahedral geometry with Fe—Cl distances and Cl—Fe—Cl angles in the range 2.1891 (7)–2.2018 (8) Å and 107.10 (3)–110.56 (3)°, respectively. There are no significant intermolecular interactions in the crystal except for some weak C—H⋯Cl contacts, which in turn indicates that the crystal packing is determined predominantly by electrostatic interactions between the ionic constituents.
Related literature
Crystals of the title compound were isolated during attempted recrystallization of [(η6-C6Me6)RuCl2{Ph2PfcCON(CH2CH2OH)2}] [fc = ferrocene-1,1′-diyl; for the preparation of this ligand, see Schulz et al. (2009 ▶)] from chloroform–diethyl ether. It is likely a decomposition product as the result of photolytic cleavage of the ferrocene moiety in the halogenated solvent (Brand & Snedden, 1957 ▶). For the crystal structure of [(μ-Cl)3{Ru(η6-C6Me6)}2][PF6], see: Pandey et al. (1999 ▶); Redwine et al. (2000 ▶). For the first structurally characterized compound of this type, [(μ-Cl)3{Ru(η6-C6Me6)}2][BPh4]·CH3OH, see: Tocher & Walkinshaw (1982 ▶). For the structures of simple tetrachloridoferrate(III) salts, see: Wyrzykowski et al. (2006 ▶); Jin et al. (2005 ▶).
Experimental
Crystal data
[Ru2Cl3(C12H18)2][FeCl4]
M r = 830.67
Triclinic,
a = 8.4490 (2) Å
b = 12.8352 (2) Å
c = 14.6752 (4) Å
α = 106.5767 (12)°
β = 90.4341 (9)°
γ = 99.7915 (12)°
V = 1500.43 (6) Å3
Z = 2
Mo Kα radiation
μ = 2.11 mm−1
T = 150 K
0.30 × 0.20 × 0.08 mm
Data collection
Nonius KappaCCD diffractometer
Absorption correction: Gaussian using the diffractometer software T min = 0.529, T max = 0.855
27082 measured reflections
6900 independent reflections
6172 reflections with I > 2σ(I)
R int = 0.036
Refinement
R[F 2 > 2σ(F 2)] = 0.026
wR(F 2) = 0.061
S = 1.08
6900 reflections
319 parameters
H-atom parameters constrained
Δρmax = 0.47 e Å−3
Δρmin = −0.68 e Å−3
Data collection: COLLECT (Nonius, 2000 ▶); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997 ▶); data reduction: HKL (Otwinowski & Minor, 1997 ▶) DENZO and SCALEPACK; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXL97 and PLATON.
Supplementary Material
Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S160053681103621X/su2311sup1.cif
Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681103621X/su2311Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report
Table 1. Hydrogen-bond geometry (Å, °).
| D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A |
|---|---|---|---|---|
| C9—H9A⋯Cl3i | 0.96 | 2.80 | 3.629 (3) | 145 |
| C11—H11B⋯Cl6ii | 0.96 | 2.71 | 3.588 (3) | 153 |
Symmetry codes: (i)
; (ii)
.
Acknowledgments
This work was supported financially by the Grant Agency of Charles University in Prague (project No. 69309), and is a part of a long-term research plan supported by the Ministry of Education, Youth and Sports of the Czech Republic (project No. MSM0021620857).
supplementary crystallographic information
Comment
A view of the molecular structure of the title compound is given in Fig. 1. The geometry of the complex cation in the structure is very similar to that reported for [(µ–Cl)3{Ru(η6-C6Me6)}2][PF6] (Pandey et al., 1999). The Ru—Cl and Ru—C distances range 2.4354 (6) - 2.4615 (6) Å and 2.170 (2) - 2.192 (3) Å, respectively. The distance between the ruthenium atoms is 3.2723 (3) Å and they are symmetrically bridged by the three chloride ligands with Ru—Cl—Ru angles in the range 83.56 (2)–84.18 (2) °. The π-coordinated arene rings are practically coplanar (dihedral angle of their mean planes is 2.31 (12) °) and assume an almost perfect staggered conformation (Fig. 2).
The [FeCl4]- counter ion has a regular tetrahedral geometry with Fe—Cl distances in the range of 2.1890 (8)–2.2018 (10) Å, and interligand angles of 107.10 (3)–110.57 (3) °. These structural data compare well with those observed for simple tetrachloridoferrate(III) salts that have been recently structurally characterized (e.g., quinolinium tetrachloroferrate(III) [Wyrzykowski et al., 2006], and matrinium tetrachloroferrate(III) [Jin et al., 2005]).
In the crystal of the title compound the cations and anions form separate layers that are perpendicular to the crystallographic a-axis direction and regularly alternate at distances determined by their van der Waals envelope. No significant hydrogen-bonding interactions (except for some weak C—H···Cl contacts, Table 1) or π···π stacking interactions were detected in the structure, which suggests that the crystal packing is governed predominantly by electrostatic interactions of the ionic constituents.
Experimental
Burgundy red crystals of the title compound were obtained serendipitously during an attempted crystallization of [(η6-C6Me6)RuCl2{Ph2PfcCON(CH2CH2OH)2-κP}] (fc = ferrocene-1,1-diyl), which had been prepared by a conventional bridge-cleavage reaction of [(η6-C6Me6)RuCl2]2 with Ph2PfcCON(CH2CH2OH)2 (Schulz et al., 2009), from chloroform–diethyl ether over an extended period (several weeks). The complex is very likely a decomposition product as the result of photolytic cleavage of the ferrocene moiety in the halogenated solvent (Brand & Snedden, 1957). This has produced FeCl3 and chloride ions required for the formation of both the complex cation and complex anion that constitute the title compound.
A few crystals of the product were analysed by electrospray ionization (ESI) mass spectroscopy, which clearly showed signals due to ions [(C6Me6)2Ru2Cl3]+ (m/z 633) and [FeCl4]- (m/z 196) with correct isotopic distribution patterns. High-resolution mass spectra further confirmed the formulation: calculated for [(C6Me6)2102Ru235Cl3]+ 632.9970, found 632.9993; calculated for [56Fe35Cl4]- 195.8109, found 195.8108.
Refinement
All H-atoms were included in their calculated positions and refined as riding atoms: C—H = 0.96 Å, with Uiso(H) = 1.2Ueq(C).
Figures
Fig. 1.
View of the molecular structure of the title compound, showing the atom numbering scheme and displacement ellipsoids drawn at the 30% probability level.
Fig. 2.
View along the Ru1···Ru2 line of the complex cation in the title compound.
Crystal data
| [Ru2Cl3(C12H18)2][Cl4Fe] | Z = 2 |
| Mr = 830.67 | F(000) = 826 |
| Triclinic, P1 | Dx = 1.839 Mg m−3 |
| a = 8.4490 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
| b = 12.8352 (2) Å | Cell parameters from 15369 reflections |
| c = 14.6752 (4) Å | θ = 1.0–27.5° |
| α = 106.5767 (12)° | µ = 2.11 mm−1 |
| β = 90.4341 (9)° | T = 150 K |
| γ = 99.7915 (12)° | Plate, red |
| V = 1500.43 (6) Å3 | 0.30 × 0.20 × 0.08 mm |
Data collection
| Nonius KappaCCD diffractometer | 6900 independent reflections |
| Radiation source: fine-focus sealed tube | 6172 reflections with I > 2σ(I) |
| horizontally mounted graphite crystal | Rint = 0.036 |
| Detector resolution: 9.091 pixels mm-1 | θmax = 27.5°, θmin = 1.5° |
| ω and π scans to fill the Ewald sphere | h = −10→10 |
| Absorption correction: gaussian (Reference? year?) | k = −16→16 |
| Tmin = 0.529, Tmax = 0.855 | l = −19→19 |
| 27082 measured reflections |
Refinement
| Refinement on F2 | Primary atom site location: structure-invariant direct methods |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| R[F2 > 2σ(F2)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.061 | H-atom parameters constrained |
| S = 1.08 | w = 1/[σ2(Fo2) + (0.0211P)2 + 1.9353P] where P = (Fo2 + 2Fc2)/3 |
| 6900 reflections | (Δ/σ)max = 0.001 |
| 319 parameters | Δρmax = 0.47 e Å−3 |
| 0 restraints | Δρmin = −0.68 e Å−3 |
Special details
| 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 on 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 > 2 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)
| x | y | z | Uiso*/Ueq | ||
| Ru1 | 0.02214 (2) | 0.229351 (15) | 0.359389 (13) | 0.01330 (5) | |
| Ru2 | −0.10556 (2) | 0.289505 (14) | 0.172745 (13) | 0.01278 (5) | |
| Cl1 | 0.01161 (7) | 0.13405 (5) | 0.18933 (4) | 0.02091 (12) | |
| Cl3 | −0.23873 (7) | 0.26089 (5) | 0.31265 (4) | 0.02071 (12) | |
| Cl2 | 0.11067 (7) | 0.38573 (5) | 0.29639 (4) | 0.01942 (12) | |
| C1 | −0.0309 (3) | 0.2545 (2) | 0.50855 (17) | 0.0179 (5) | |
| C2 | 0.1257 (3) | 0.3123 (2) | 0.50368 (17) | 0.0179 (5) | |
| C3 | 0.2415 (3) | 0.2553 (2) | 0.44795 (17) | 0.0175 (5) | |
| C4 | 0.1993 (3) | 0.1418 (2) | 0.39726 (18) | 0.0186 (5) | |
| C5 | 0.0393 (3) | 0.08221 (19) | 0.40182 (18) | 0.0185 (5) | |
| C6 | −0.0745 (3) | 0.1384 (2) | 0.45724 (17) | 0.0175 (5) | |
| C7 | −0.1569 (3) | 0.3129 (2) | 0.5627 (2) | 0.0252 (6) | |
| H7A | −0.1180 | 0.3911 | 0.5822 | 0.030* | |
| H7B | −0.1795 | 0.2881 | 0.6179 | 0.030* | |
| H7C | −0.2535 | 0.2965 | 0.5225 | 0.030* | |
| C8 | 0.1739 (3) | 0.4348 (2) | 0.5527 (2) | 0.0272 (6) | |
| H8A | 0.0814 | 0.4640 | 0.5790 | 0.033* | |
| H8B | 0.2166 | 0.4717 | 0.5074 | 0.033* | |
| H8C | 0.2544 | 0.4466 | 0.6029 | 0.033* | |
| C9 | 0.4059 (3) | 0.3199 (2) | 0.4407 (2) | 0.0280 (6) | |
| H9A | 0.4670 | 0.2723 | 0.3982 | 0.034* | |
| H9B | 0.4611 | 0.3479 | 0.5026 | 0.034* | |
| H9C | 0.3940 | 0.3804 | 0.4166 | 0.034* | |
| C10 | 0.3173 (3) | 0.0828 (2) | 0.3344 (2) | 0.0282 (6) | |
| H10A | 0.3854 | 0.1340 | 0.3087 | 0.034* | |
| H10B | 0.2593 | 0.0238 | 0.2832 | 0.034* | |
| H10C | 0.3819 | 0.0531 | 0.3713 | 0.034* | |
| C11 | −0.0095 (3) | −0.0368 (2) | 0.3438 (2) | 0.0270 (6) | |
| H11A | −0.0604 | −0.0791 | 0.3834 | 0.032* | |
| H11B | 0.0843 | −0.0655 | 0.3190 | 0.032* | |
| H11C | −0.0832 | −0.0418 | 0.2920 | 0.032* | |
| C12 | −0.2441 (3) | 0.0774 (2) | 0.4589 (2) | 0.0266 (6) | |
| H12A | −0.2956 | 0.0551 | 0.3961 | 0.032* | |
| H12B | −0.3039 | 0.1252 | 0.5020 | 0.032* | |
| H12C | −0.2402 | 0.0133 | 0.4795 | 0.032* | |
| C21 | −0.2956 (3) | 0.3670 (2) | 0.13151 (18) | 0.0178 (5) | |
| C22 | −0.1436 (3) | 0.43297 (19) | 0.12874 (17) | 0.0167 (5) | |
| C23 | −0.0186 (3) | 0.38344 (19) | 0.07579 (17) | 0.0161 (5) | |
| C24 | −0.0481 (3) | 0.2687 (2) | 0.02469 (17) | 0.0179 (5) | |
| C25 | −0.2022 (3) | 0.2026 (2) | 0.02849 (17) | 0.0186 (5) | |
| C26 | −0.3243 (3) | 0.2508 (2) | 0.08142 (18) | 0.0183 (5) | |
| C27 | −0.4253 (3) | 0.4163 (2) | 0.1900 (2) | 0.0247 (6) | |
| H27A | −0.3818 | 0.4901 | 0.2281 | 0.030* | |
| H27B | −0.4642 | 0.3720 | 0.2308 | 0.030* | |
| H27C | −0.5123 | 0.4180 | 0.1483 | 0.030* | |
| C28 | −0.1085 (3) | 0.5541 (2) | 0.1839 (2) | 0.0255 (6) | |
| H28A | −0.1997 | 0.5734 | 0.2192 | 0.031* | |
| H28B | −0.0872 | 0.5976 | 0.1405 | 0.031* | |
| H28C | −0.0162 | 0.5683 | 0.2271 | 0.031* | |
| C29 | 0.1449 (3) | 0.4543 (2) | 0.07921 (19) | 0.0234 (5) | |
| H29A | 0.2174 | 0.4095 | 0.0445 | 0.028* | |
| H29B | 0.1857 | 0.4862 | 0.1443 | 0.028* | |
| H29C | 0.1356 | 0.5120 | 0.0511 | 0.028* | |
| C30 | 0.0826 (3) | 0.2148 (2) | −0.0284 (2) | 0.0266 (6) | |
| H30A | 0.1836 | 0.2649 | −0.0119 | 0.032* | |
| H30B | 0.0580 | 0.1964 | −0.0957 | 0.032* | |
| H30C | 0.0895 | 0.1487 | −0.0115 | 0.032* | |
| C31 | −0.2325 (3) | 0.0799 (2) | −0.0213 (2) | 0.0283 (6) | |
| H31A | −0.2678 | 0.0403 | 0.0235 | 0.034* | |
| H31B | −0.1349 | 0.0585 | −0.0472 | 0.034* | |
| H31C | −0.3141 | 0.0629 | −0.0718 | 0.034* | |
| C32 | −0.4824 (3) | 0.1789 (2) | 0.0883 (2) | 0.0275 (6) | |
| H32A | −0.5410 | 0.1538 | 0.0274 | 0.033* | |
| H32B | −0.5445 | 0.2209 | 0.1347 | 0.033* | |
| H32C | −0.4623 | 0.1163 | 0.1070 | 0.033* | |
| Fe1 | 0.49209 (4) | 0.77416 (3) | 0.20266 (3) | 0.01901 (8) | |
| Cl4 | 0.52218 (8) | 0.63784 (5) | 0.07833 (5) | 0.02709 (14) | |
| Cl5 | 0.58902 (10) | 0.75020 (7) | 0.33345 (6) | 0.03875 (18) | |
| Cl6 | 0.23261 (7) | 0.77493 (5) | 0.21100 (5) | 0.02774 (14) | |
| Cl7 | 0.61347 (8) | 0.93196 (5) | 0.18546 (5) | 0.02927 (15) |
Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Ru1 | 0.01313 (9) | 0.01651 (10) | 0.01132 (10) | 0.00389 (7) | 0.00058 (7) | 0.00500 (7) |
| Ru2 | 0.01294 (9) | 0.01399 (9) | 0.01185 (10) | 0.00173 (7) | −0.00050 (7) | 0.00489 (7) |
| Cl1 | 0.0317 (3) | 0.0190 (3) | 0.0137 (3) | 0.0112 (2) | 0.0000 (2) | 0.0036 (2) |
| Cl3 | 0.0141 (3) | 0.0338 (3) | 0.0193 (3) | 0.0068 (2) | 0.0028 (2) | 0.0143 (3) |
| Cl2 | 0.0202 (3) | 0.0195 (3) | 0.0176 (3) | −0.0020 (2) | −0.0041 (2) | 0.0072 (2) |
| C1 | 0.0208 (12) | 0.0257 (12) | 0.0089 (11) | 0.0062 (9) | 0.0010 (9) | 0.0065 (9) |
| C2 | 0.0189 (11) | 0.0252 (12) | 0.0102 (11) | 0.0042 (9) | −0.0023 (9) | 0.0061 (9) |
| C3 | 0.0134 (11) | 0.0278 (13) | 0.0139 (12) | 0.0045 (9) | −0.0019 (9) | 0.0096 (10) |
| C4 | 0.0175 (11) | 0.0239 (12) | 0.0186 (13) | 0.0086 (9) | −0.0015 (9) | 0.0099 (10) |
| C5 | 0.0216 (12) | 0.0192 (12) | 0.0183 (13) | 0.0055 (9) | −0.0022 (10) | 0.0104 (10) |
| C6 | 0.0179 (11) | 0.0237 (12) | 0.0143 (12) | 0.0032 (9) | 0.0007 (9) | 0.0115 (10) |
| C7 | 0.0253 (13) | 0.0303 (14) | 0.0210 (14) | 0.0077 (11) | 0.0063 (11) | 0.0074 (11) |
| C8 | 0.0288 (14) | 0.0265 (13) | 0.0211 (14) | −0.0001 (11) | −0.0018 (11) | 0.0016 (11) |
| C9 | 0.0179 (12) | 0.0354 (15) | 0.0296 (16) | 0.0017 (11) | 0.0012 (11) | 0.0097 (12) |
| C10 | 0.0257 (13) | 0.0318 (15) | 0.0306 (16) | 0.0131 (11) | 0.0054 (12) | 0.0098 (12) |
| C11 | 0.0291 (14) | 0.0227 (13) | 0.0293 (15) | 0.0066 (10) | −0.0017 (11) | 0.0069 (11) |
| C12 | 0.0212 (13) | 0.0326 (14) | 0.0279 (15) | 0.0016 (11) | 0.0035 (11) | 0.0137 (12) |
| C21 | 0.0163 (11) | 0.0231 (12) | 0.0179 (13) | 0.0059 (9) | −0.0031 (9) | 0.0111 (10) |
| C22 | 0.0211 (11) | 0.0167 (11) | 0.0161 (12) | 0.0047 (9) | −0.0025 (9) | 0.0099 (9) |
| C23 | 0.0183 (11) | 0.0203 (11) | 0.0127 (12) | 0.0023 (9) | −0.0007 (9) | 0.0102 (9) |
| C24 | 0.0217 (12) | 0.0219 (12) | 0.0112 (12) | 0.0042 (9) | 0.0002 (9) | 0.0062 (9) |
| C25 | 0.0227 (12) | 0.0196 (12) | 0.0125 (12) | 0.0014 (9) | −0.0037 (9) | 0.0044 (9) |
| C26 | 0.0159 (11) | 0.0231 (12) | 0.0163 (12) | 0.0002 (9) | −0.0063 (9) | 0.0084 (10) |
| C27 | 0.0201 (12) | 0.0295 (14) | 0.0279 (15) | 0.0090 (10) | 0.0028 (11) | 0.0107 (11) |
| C28 | 0.0290 (14) | 0.0189 (12) | 0.0282 (15) | 0.0042 (10) | 0.0005 (11) | 0.0063 (11) |
| C29 | 0.0211 (12) | 0.0256 (13) | 0.0226 (14) | −0.0012 (10) | 0.0017 (10) | 0.0085 (11) |
| C30 | 0.0292 (14) | 0.0290 (14) | 0.0218 (14) | 0.0088 (11) | 0.0056 (11) | 0.0054 (11) |
| C31 | 0.0340 (15) | 0.0187 (12) | 0.0270 (15) | −0.0003 (11) | −0.0047 (12) | 0.0018 (11) |
| C32 | 0.0206 (12) | 0.0299 (14) | 0.0307 (16) | −0.0043 (10) | −0.0035 (11) | 0.0121 (12) |
| Fe1 | 0.02005 (17) | 0.01886 (17) | 0.01832 (19) | 0.00242 (13) | 0.00093 (14) | 0.00633 (14) |
| Cl4 | 0.0285 (3) | 0.0239 (3) | 0.0266 (4) | 0.0058 (2) | 0.0066 (3) | 0.0030 (3) |
| Cl5 | 0.0465 (4) | 0.0444 (4) | 0.0288 (4) | 0.0040 (3) | −0.0083 (3) | 0.0188 (3) |
| Cl6 | 0.0224 (3) | 0.0257 (3) | 0.0344 (4) | 0.0054 (2) | 0.0061 (3) | 0.0068 (3) |
| Cl7 | 0.0307 (3) | 0.0235 (3) | 0.0331 (4) | −0.0034 (3) | −0.0018 (3) | 0.0121 (3) |
Geometric parameters (Å, °)
| Ru1—C4 | 2.175 (2) | C10—H10C | 0.9600 |
| Ru1—C5 | 2.177 (2) | C11—H11A | 0.9600 |
| Ru1—C6 | 2.177 (2) | C11—H11B | 0.9600 |
| Ru1—C3 | 2.178 (2) | C11—H11C | 0.9600 |
| Ru1—C2 | 2.180 (2) | C12—H12A | 0.9600 |
| Ru1—C1 | 2.181 (2) | C12—H12B | 0.9600 |
| Ru1—Cl3 | 2.4354 (6) | C12—H12C | 0.9600 |
| Ru1—Cl1 | 2.4393 (6) | C21—C22 | 1.420 (3) |
| Ru1—Cl2 | 2.4498 (6) | C21—C26 | 1.440 (3) |
| Ru2—C25 | 2.170 (2) | C21—C27 | 1.509 (3) |
| Ru2—C23 | 2.171 (2) | C22—C23 | 1.443 (3) |
| Ru2—C26 | 2.175 (2) | C22—C28 | 1.511 (3) |
| Ru2—C24 | 2.181 (2) | C23—C24 | 1.427 (3) |
| Ru2—C22 | 2.188 (2) | C23—C29 | 1.511 (3) |
| Ru2—C21 | 2.192 (2) | C24—C25 | 1.439 (3) |
| Ru2—Cl3 | 2.4374 (6) | C24—C30 | 1.507 (3) |
| Ru2—Cl1 | 2.4425 (6) | C25—C26 | 1.416 (4) |
| Ru2—Cl2 | 2.4616 (6) | C25—C31 | 1.512 (3) |
| C1—C2 | 1.416 (3) | C26—C32 | 1.511 (3) |
| C1—C6 | 1.446 (3) | C27—H27A | 0.9600 |
| C1—C7 | 1.507 (3) | C27—H27B | 0.9600 |
| C2—C3 | 1.441 (3) | C27—H27C | 0.9600 |
| C2—C8 | 1.513 (3) | C28—H28A | 0.9600 |
| C3—C4 | 1.415 (3) | C28—H28B | 0.9600 |
| C3—C9 | 1.513 (3) | C28—H28C | 0.9600 |
| C4—C5 | 1.448 (3) | C29—H29A | 0.9600 |
| C4—C10 | 1.513 (4) | C29—H29B | 0.9600 |
| C5—C6 | 1.421 (3) | C29—H29C | 0.9600 |
| C5—C11 | 1.506 (3) | C30—H30A | 0.9600 |
| C6—C12 | 1.515 (3) | C30—H30B | 0.9600 |
| C7—H7A | 0.9600 | C30—H30C | 0.9600 |
| C7—H7B | 0.9600 | C31—H31A | 0.9600 |
| C7—H7C | 0.9600 | C31—H31B | 0.9600 |
| C8—H8A | 0.9600 | C31—H31C | 0.9600 |
| C8—H8B | 0.9600 | C32—H32A | 0.9600 |
| C8—H8C | 0.9600 | C32—H32B | 0.9600 |
| C9—H9A | 0.9600 | C32—H32C | 0.9600 |
| C9—H9B | 0.9600 | Fe1—Cl4 | 2.1891 (7) |
| C9—H9C | 0.9600 | Fe1—Cl7 | 2.1925 (7) |
| C10—H10A | 0.9600 | Fe1—Cl6 | 2.1982 (7) |
| C10—H10B | 0.9600 | Fe1—Cl5 | 2.2018 (8) |
| C4—Ru1—C5 | 38.86 (9) | H7A—C7—H7B | 109.5 |
| C4—Ru1—C6 | 69.45 (9) | C1—C7—H7C | 109.5 |
| C5—Ru1—C6 | 38.09 (9) | H7A—C7—H7C | 109.5 |
| C4—Ru1—C3 | 37.96 (9) | H7B—C7—H7C | 109.5 |
| C5—Ru1—C3 | 69.40 (9) | C2—C8—H8A | 109.5 |
| C6—Ru1—C3 | 81.96 (9) | C2—C8—H8B | 109.5 |
| C4—Ru1—C2 | 69.41 (9) | H8A—C8—H8B | 109.5 |
| C5—Ru1—C2 | 82.33 (9) | C2—C8—H8C | 109.5 |
| C6—Ru1—C2 | 69.31 (9) | H8A—C8—H8C | 109.5 |
| C3—Ru1—C2 | 38.63 (9) | H8B—C8—H8C | 109.5 |
| C4—Ru1—C1 | 82.20 (9) | C3—C9—H9A | 109.5 |
| C5—Ru1—C1 | 69.55 (9) | C3—C9—H9B | 109.5 |
| C6—Ru1—C1 | 38.75 (9) | H9A—C9—H9B | 109.5 |
| C3—Ru1—C1 | 69.14 (9) | C3—C9—H9C | 109.5 |
| C2—Ru1—C1 | 37.89 (9) | H9A—C9—H9C | 109.5 |
| C4—Ru1—Cl3 | 158.47 (7) | H9B—C9—H9C | 109.5 |
| C5—Ru1—Cl3 | 120.10 (7) | C4—C10—H10A | 109.5 |
| C6—Ru1—Cl3 | 94.48 (6) | C4—C10—H10B | 109.5 |
| C3—Ru1—Cl3 | 157.47 (7) | H10A—C10—H10B | 109.5 |
| C2—Ru1—Cl3 | 119.41 (7) | C4—C10—H10C | 109.5 |
| C1—Ru1—Cl3 | 94.18 (6) | H10A—C10—H10C | 109.5 |
| C4—Ru1—Cl1 | 94.63 (7) | H10B—C10—H10C | 109.5 |
| C5—Ru1—Cl1 | 94.10 (7) | C5—C11—H11A | 109.5 |
| C6—Ru1—Cl1 | 119.50 (7) | C5—C11—H11B | 109.5 |
| C3—Ru1—Cl1 | 120.52 (7) | H11A—C11—H11B | 109.5 |
| C2—Ru1—Cl1 | 158.63 (7) | C5—C11—H11C | 109.5 |
| C1—Ru1—Cl1 | 157.61 (7) | H11A—C11—H11C | 109.5 |
| Cl3—Ru1—Cl1 | 80.63 (2) | H11B—C11—H11C | 109.5 |
| C4—Ru1—Cl2 | 119.53 (7) | C6—C12—H12A | 109.5 |
| C5—Ru1—Cl2 | 157.44 (7) | C6—C12—H12B | 109.5 |
| C6—Ru1—Cl2 | 159.55 (7) | H12A—C12—H12B | 109.5 |
| C3—Ru1—Cl2 | 95.09 (6) | C6—C12—H12C | 109.5 |
| C2—Ru1—Cl2 | 95.77 (7) | H12A—C12—H12C | 109.5 |
| C1—Ru1—Cl2 | 121.39 (7) | H12B—C12—H12C | 109.5 |
| Cl3—Ru1—Cl2 | 80.48 (2) | C22—C21—C26 | 119.8 (2) |
| Cl1—Ru1—Cl2 | 79.48 (2) | C22—C21—C27 | 120.8 (2) |
| C25—Ru2—C23 | 69.46 (9) | C26—C21—C27 | 119.4 (2) |
| C25—Ru2—C26 | 38.05 (9) | C22—C21—Ru2 | 70.92 (13) |
| C23—Ru2—C26 | 82.24 (9) | C26—C21—Ru2 | 70.08 (13) |
| C25—Ru2—C24 | 38.62 (9) | C27—C21—Ru2 | 129.35 (17) |
| C23—Ru2—C24 | 38.27 (9) | C21—C22—C23 | 120.0 (2) |
| C26—Ru2—C24 | 69.40 (9) | C21—C22—C28 | 120.7 (2) |
| C25—Ru2—C22 | 81.91 (9) | C23—C22—C28 | 119.2 (2) |
| C23—Ru2—C22 | 38.67 (9) | C21—C22—Ru2 | 71.24 (13) |
| C26—Ru2—C22 | 69.11 (9) | C23—C22—Ru2 | 70.00 (12) |
| C24—Ru2—C22 | 69.42 (9) | C28—C22—Ru2 | 129.46 (17) |
| C25—Ru2—C21 | 69.14 (9) | C24—C23—C22 | 120.2 (2) |
| C23—Ru2—C21 | 69.28 (9) | C24—C23—C29 | 121.1 (2) |
| C26—Ru2—C21 | 38.50 (9) | C22—C23—C29 | 118.7 (2) |
| C24—Ru2—C21 | 82.06 (9) | C24—C23—Ru2 | 71.26 (13) |
| C22—Ru2—C21 | 37.84 (9) | C22—C23—Ru2 | 71.32 (13) |
| C25—Ru2—Cl3 | 122.69 (7) | C29—C23—Ru2 | 127.77 (17) |
| C23—Ru2—Cl3 | 154.96 (7) | C23—C24—C25 | 119.3 (2) |
| C26—Ru2—Cl3 | 95.76 (7) | C23—C24—C30 | 120.9 (2) |
| C24—Ru2—Cl3 | 161.03 (6) | C25—C24—C30 | 119.7 (2) |
| C22—Ru2—Cl3 | 117.41 (7) | C23—C24—Ru2 | 70.46 (13) |
| C21—Ru2—Cl3 | 93.62 (7) | C25—C24—Ru2 | 70.27 (14) |
| C25—Ru2—Cl1 | 93.22 (7) | C30—C24—Ru2 | 128.70 (18) |
| C23—Ru2—Cl1 | 122.67 (7) | C26—C25—C24 | 120.6 (2) |
| C26—Ru2—Cl1 | 117.14 (7) | C26—C25—C31 | 119.5 (2) |
| C24—Ru2—Cl1 | 95.47 (6) | C24—C25—C31 | 119.9 (2) |
| C22—Ru2—Cl1 | 161.18 (7) | C26—C25—Ru2 | 71.15 (13) |
| C21—Ru2—Cl1 | 154.69 (7) | C24—C25—Ru2 | 71.11 (13) |
| Cl3—Ru2—Cl1 | 80.53 (2) | C31—C25—Ru2 | 128.74 (18) |
| C25—Ru2—Cl2 | 154.68 (7) | C25—C26—C21 | 120.1 (2) |
| C23—Ru2—Cl2 | 94.21 (6) | C25—C26—C32 | 119.7 (2) |
| C26—Ru2—Cl2 | 162.53 (7) | C21—C26—C32 | 120.1 (2) |
| C24—Ru2—Cl2 | 117.47 (6) | C25—C26—Ru2 | 70.80 (13) |
| C22—Ru2—Cl2 | 97.49 (6) | C21—C26—Ru2 | 71.42 (13) |
| C21—Ru2—Cl2 | 124.36 (7) | C32—C26—Ru2 | 128.38 (18) |
| Cl3—Ru2—Cl2 | 80.21 (2) | C21—C27—H27A | 109.5 |
| Cl1—Ru2—Cl2 | 79.19 (2) | C21—C27—H27B | 109.5 |
| Ru1—Cl1—Ru2 | 84.181 (19) | H27A—C27—H27B | 109.5 |
| Ru1—Cl3—Ru2 | 84.372 (19) | C21—C27—H27C | 109.5 |
| Ru1—Cl2—Ru2 | 83.559 (18) | H27A—C27—H27C | 109.5 |
| C2—C1—C6 | 119.9 (2) | H27B—C27—H27C | 109.5 |
| C2—C1—C7 | 121.2 (2) | C22—C28—H28A | 109.5 |
| C6—C1—C7 | 118.8 (2) | C22—C28—H28B | 109.5 |
| C2—C1—Ru1 | 71.00 (14) | H28A—C28—H28B | 109.5 |
| C6—C1—Ru1 | 70.48 (13) | C22—C28—H28C | 109.5 |
| C7—C1—Ru1 | 128.64 (17) | H28A—C28—H28C | 109.5 |
| C1—C2—C3 | 119.9 (2) | H28B—C28—H28C | 109.5 |
| C1—C2—C8 | 121.6 (2) | C23—C29—H29A | 109.5 |
| C3—C2—C8 | 118.4 (2) | C23—C29—H29B | 109.5 |
| C1—C2—Ru1 | 71.11 (13) | H29A—C29—H29B | 109.5 |
| C3—C2—Ru1 | 70.61 (13) | C23—C29—H29C | 109.5 |
| C8—C2—Ru1 | 128.84 (17) | H29A—C29—H29C | 109.5 |
| C4—C3—C2 | 120.4 (2) | H29B—C29—H29C | 109.5 |
| C4—C3—C9 | 120.6 (2) | C24—C30—H30A | 109.5 |
| C2—C3—C9 | 118.9 (2) | C24—C30—H30B | 109.5 |
| C4—C3—Ru1 | 70.90 (13) | H30A—C30—H30B | 109.5 |
| C2—C3—Ru1 | 70.76 (13) | C24—C30—H30C | 109.5 |
| C9—C3—Ru1 | 128.73 (18) | H30A—C30—H30C | 109.5 |
| C3—C4—C5 | 120.0 (2) | H30B—C30—H30C | 109.5 |
| C3—C4—C10 | 120.7 (2) | C25—C31—H31A | 109.5 |
| C5—C4—C10 | 119.3 (2) | C25—C31—H31B | 109.5 |
| C3—C4—Ru1 | 71.15 (13) | H31A—C31—H31B | 109.5 |
| C5—C4—Ru1 | 70.65 (13) | C25—C31—H31C | 109.5 |
| C10—C4—Ru1 | 128.39 (18) | H31A—C31—H31C | 109.5 |
| C6—C5—C4 | 119.6 (2) | H31B—C31—H31C | 109.5 |
| C6—C5—C11 | 120.1 (2) | C26—C32—H32A | 109.5 |
| C4—C5—C11 | 120.2 (2) | C26—C32—H32B | 109.5 |
| C6—C5—Ru1 | 70.98 (13) | H32A—C32—H32B | 109.5 |
| C4—C5—Ru1 | 70.49 (13) | C26—C32—H32C | 109.5 |
| C11—C5—Ru1 | 127.97 (18) | H32A—C32—H32C | 109.5 |
| C5—C6—C1 | 120.2 (2) | H32B—C32—H32C | 109.5 |
| C5—C6—C12 | 119.7 (2) | Cl4—Fe1—Cl7 | 110.26 (3) |
| C1—C6—C12 | 120.1 (2) | Cl4—Fe1—Cl6 | 107.10 (3) |
| C5—C6—Ru1 | 70.93 (13) | Cl7—Fe1—Cl6 | 109.15 (3) |
| C1—C6—Ru1 | 70.77 (13) | Cl4—Fe1—Cl5 | 110.56 (3) |
| C12—C6—Ru1 | 128.84 (17) | Cl7—Fe1—Cl5 | 109.87 (3) |
| C1—C7—H7A | 109.5 | Cl6—Fe1—Cl5 | 109.85 (3) |
| C1—C7—H7B | 109.5 | ||
| C4—Ru1—Cl1—Ru2 | −161.28 (7) | C2—C1—C6—Ru1 | −52.9 (2) |
| C5—Ru1—Cl1—Ru2 | 159.74 (7) | C7—C1—C6—Ru1 | 124.1 (2) |
| C6—Ru1—Cl1—Ru2 | 129.75 (7) | C4—Ru1—C6—C5 | −29.58 (14) |
| C3—Ru1—Cl1—Ru2 | −131.80 (7) | C3—Ru1—C6—C5 | −66.69 (14) |
| C2—Ru1—Cl1—Ru2 | −120.87 (18) | C2—Ru1—C6—C5 | −104.51 (15) |
| C1—Ru1—Cl1—Ru2 | 117.96 (17) | C1—Ru1—C6—C5 | −133.2 (2) |
| Cl3—Ru1—Cl1—Ru2 | 39.886 (19) | Cl3—Ru1—C6—C5 | 135.69 (13) |
| Cl2—Ru1—Cl1—Ru2 | −42.073 (19) | Cl1—Ru1—C6—C5 | 53.93 (15) |
| C25—Ru2—Cl1—Ru1 | −162.48 (7) | Cl2—Ru1—C6—C5 | −149.66 (15) |
| C23—Ru2—Cl1—Ru1 | 129.94 (7) | C4—Ru1—C6—C1 | 103.63 (15) |
| C26—Ru2—Cl1—Ru1 | −131.52 (8) | C5—Ru1—C6—C1 | 133.2 (2) |
| C24—Ru2—Cl1—Ru1 | 158.85 (6) | C3—Ru1—C6—C1 | 66.51 (14) |
| C22—Ru2—Cl1—Ru1 | 123.3 (2) | C2—Ru1—C6—C1 | 28.70 (13) |
| C21—Ru2—Cl1—Ru1 | −118.16 (16) | Cl3—Ru1—C6—C1 | −91.10 (13) |
| Cl3—Ru2—Cl1—Ru1 | −39.863 (19) | Cl1—Ru1—C6—C1 | −172.86 (11) |
| Cl2—Ru2—Cl1—Ru1 | 41.875 (19) | Cl2—Ru1—C6—C1 | −16.5 (3) |
| C4—Ru1—Cl3—Ru2 | −118.72 (19) | C4—Ru1—C6—C12 | −142.8 (3) |
| C5—Ru1—Cl3—Ru2 | −129.29 (8) | C5—Ru1—C6—C12 | −113.2 (3) |
| C6—Ru1—Cl3—Ru2 | −159.16 (7) | C3—Ru1—C6—C12 | −179.9 (2) |
| C3—Ru1—Cl3—Ru2 | 121.07 (17) | C2—Ru1—C6—C12 | 142.3 (2) |
| C2—Ru1—Cl3—Ru2 | 132.10 (7) | C1—Ru1—C6—C12 | 113.6 (3) |
| C1—Ru1—Cl3—Ru2 | 161.98 (7) | Cl3—Ru1—C6—C12 | 22.5 (2) |
| Cl1—Ru1—Cl3—Ru2 | −39.971 (19) | Cl1—Ru1—C6—C12 | −59.3 (2) |
| Cl2—Ru1—Cl3—Ru2 | 40.820 (19) | Cl2—Ru1—C6—C12 | 97.1 (3) |
| C25—Ru2—Cl3—Ru1 | 127.66 (8) | C25—Ru2—C21—C22 | −104.19 (16) |
| C23—Ru2—Cl3—Ru1 | −119.47 (15) | C23—Ru2—C21—C22 | −29.11 (14) |
| C26—Ru2—Cl3—Ru1 | 156.54 (7) | C26—Ru2—C21—C22 | −133.2 (2) |
| C24—Ru2—Cl3—Ru1 | 119.1 (2) | C24—Ru2—C21—C22 | −66.48 (15) |
| C22—Ru2—Cl3—Ru1 | −134.03 (7) | Cl3—Ru2—C21—C22 | 132.09 (14) |
| C21—Ru2—Cl3—Ru1 | −164.88 (7) | Cl1—Ru2—C21—C22 | −152.49 (13) |
| Cl1—Ru2—Cl3—Ru1 | 39.923 (19) | Cl2—Ru2—C21—C22 | 51.49 (16) |
| Cl2—Ru2—Cl3—Ru1 | −40.624 (19) | C25—Ru2—C21—C26 | 29.01 (14) |
| C4—Ru1—Cl2—Ru2 | 131.11 (8) | C23—Ru2—C21—C26 | 104.09 (16) |
| C5—Ru1—Cl2—Ru2 | 116.80 (17) | C24—Ru2—C21—C26 | 66.72 (15) |
| C6—Ru1—Cl2—Ru2 | −117.51 (18) | C22—Ru2—C21—C26 | 133.2 (2) |
| C3—Ru1—Cl2—Ru2 | 161.87 (7) | Cl3—Ru2—C21—C26 | −94.71 (13) |
| C2—Ru1—Cl2—Ru2 | −159.32 (6) | Cl1—Ru2—C21—C26 | −19.3 (2) |
| C1—Ru1—Cl2—Ru2 | −129.50 (7) | Cl2—Ru2—C21—C26 | −175.31 (11) |
| Cl3—Ru1—Cl2—Ru2 | −40.409 (19) | C25—Ru2—C21—C27 | 141.2 (2) |
| Cl1—Ru1—Cl2—Ru2 | 41.733 (19) | C23—Ru2—C21—C27 | −143.7 (2) |
| C25—Ru2—Cl2—Ru1 | −116.04 (15) | C26—Ru2—C21—C27 | 112.2 (3) |
| C23—Ru2—Cl2—Ru1 | −164.20 (7) | C24—Ru2—C21—C27 | 178.9 (2) |
| C26—Ru2—Cl2—Ru1 | 118.3 (2) | C22—Ru2—C21—C27 | −114.6 (3) |
| C24—Ru2—Cl2—Ru1 | −132.30 (7) | Cl3—Ru2—C21—C27 | 17.5 (2) |
| C22—Ru2—Cl2—Ru1 | 157.05 (7) | Cl1—Ru2—C21—C27 | 92.9 (3) |
| C21—Ru2—Cl2—Ru1 | 128.10 (8) | Cl2—Ru2—C21—C27 | −63.1 (2) |
| Cl3—Ru2—Cl2—Ru1 | 40.409 (19) | C26—C21—C22—C23 | 0.0 (3) |
| Cl1—Ru2—Cl2—Ru1 | −41.716 (19) | C27—C21—C22—C23 | 177.3 (2) |
| C4—Ru1—C1—C2 | 66.29 (14) | Ru2—C21—C22—C23 | 52.19 (19) |
| C5—Ru1—C1—C2 | 104.32 (15) | C26—C21—C22—C28 | −177.5 (2) |
| C6—Ru1—C1—C2 | 133.0 (2) | C27—C21—C22—C28 | −0.3 (3) |
| C3—Ru1—C1—C2 | 29.37 (14) | Ru2—C21—C22—C28 | −125.4 (2) |
| Cl3—Ru1—C1—C2 | −135.05 (13) | C26—C21—C22—Ru2 | −52.16 (19) |
| Cl1—Ru1—C1—C2 | 149.49 (14) | C27—C21—C22—Ru2 | 125.1 (2) |
| Cl2—Ru1—C1—C2 | −53.67 (15) | C25—Ru2—C22—C21 | 66.21 (15) |
| C4—Ru1—C1—C6 | −66.71 (14) | C23—Ru2—C22—C21 | 133.3 (2) |
| C5—Ru1—C1—C6 | −28.68 (13) | C26—Ru2—C22—C21 | 29.06 (14) |
| C3—Ru1—C1—C6 | −103.63 (15) | C24—Ru2—C22—C21 | 104.06 (16) |
| C2—Ru1—C1—C6 | −133.0 (2) | Cl3—Ru2—C22—C21 | −56.53 (15) |
| Cl3—Ru1—C1—C6 | 91.95 (13) | Cl1—Ru2—C22—C21 | 142.25 (17) |
| Cl1—Ru1—C1—C6 | 16.5 (2) | Cl2—Ru2—C22—C21 | −139.35 (13) |
| Cl2—Ru1—C1—C6 | 173.34 (11) | C25—Ru2—C22—C23 | −67.07 (14) |
| C4—Ru1—C1—C7 | −178.5 (2) | C26—Ru2—C22—C23 | −104.21 (15) |
| C5—Ru1—C1—C7 | −140.5 (2) | C24—Ru2—C22—C23 | −29.21 (13) |
| C6—Ru1—C1—C7 | −111.8 (3) | C21—Ru2—C22—C23 | −133.3 (2) |
| C3—Ru1—C1—C7 | 144.6 (2) | Cl3—Ru2—C22—C23 | 170.19 (11) |
| C2—Ru1—C1—C7 | 115.2 (3) | Cl1—Ru2—C22—C23 | 9.0 (3) |
| Cl3—Ru1—C1—C7 | −19.9 (2) | Cl2—Ru2—C22—C23 | 87.38 (13) |
| Cl1—Ru1—C1—C7 | −95.3 (3) | C25—Ru2—C22—C28 | −179.0 (2) |
| Cl2—Ru1—C1—C7 | 61.5 (2) | C23—Ru2—C22—C28 | −111.9 (3) |
| C6—C1—C2—C3 | −0.3 (3) | C26—Ru2—C22—C28 | 143.9 (2) |
| C7—C1—C2—C3 | −177.3 (2) | C24—Ru2—C22—C28 | −141.1 (2) |
| Ru1—C1—C2—C3 | −53.0 (2) | C21—Ru2—C22—C28 | 114.8 (3) |
| C6—C1—C2—C8 | 177.3 (2) | Cl3—Ru2—C22—C28 | 58.3 (2) |
| C7—C1—C2—C8 | 0.3 (4) | Cl1—Ru2—C22—C28 | −103.0 (3) |
| Ru1—C1—C2—C8 | 124.6 (2) | Cl2—Ru2—C22—C28 | −24.5 (2) |
| C6—C1—C2—Ru1 | 52.7 (2) | C21—C22—C23—C24 | 1.2 (3) |
| C7—C1—C2—Ru1 | −124.3 (2) | C28—C22—C23—C24 | 178.8 (2) |
| C4—Ru1—C2—C1 | −104.29 (15) | Ru2—C22—C23—C24 | 53.92 (19) |
| C5—Ru1—C2—C1 | −66.36 (15) | C21—C22—C23—C29 | −176.3 (2) |
| C6—Ru1—C2—C1 | −29.30 (14) | C28—C22—C23—C29 | 1.3 (3) |
| C3—Ru1—C2—C1 | −132.8 (2) | Ru2—C22—C23—C29 | −123.5 (2) |
| Cl3—Ru1—C2—C1 | 53.98 (15) | C21—C22—C23—Ru2 | −52.75 (19) |
| Cl1—Ru1—C2—C1 | −147.94 (15) | C28—C22—C23—Ru2 | 124.8 (2) |
| Cl2—Ru1—C2—C1 | 136.28 (13) | C25—Ru2—C23—C24 | −29.30 (14) |
| C4—Ru1—C2—C3 | 28.48 (14) | C26—Ru2—C23—C24 | −66.40 (14) |
| C5—Ru1—C2—C3 | 66.42 (14) | C22—Ru2—C23—C24 | −132.5 (2) |
| C6—Ru1—C2—C3 | 103.47 (15) | C21—Ru2—C23—C24 | −103.94 (15) |
| C1—Ru1—C2—C3 | 132.8 (2) | Cl3—Ru2—C23—C24 | −153.40 (13) |
| Cl3—Ru1—C2—C3 | −173.25 (11) | Cl1—Ru2—C23—C24 | 50.96 (15) |
| Cl1—Ru1—C2—C3 | −15.2 (3) | Cl2—Ru2—C23—C24 | 130.80 (13) |
| Cl2—Ru1—C2—C3 | −90.95 (13) | C25—Ru2—C23—C22 | 103.17 (15) |
| C4—Ru1—C2—C8 | 139.9 (2) | C26—Ru2—C23—C22 | 66.07 (14) |
| C5—Ru1—C2—C8 | 177.8 (2) | C24—Ru2—C23—C22 | 132.5 (2) |
| C6—Ru1—C2—C8 | −145.1 (2) | C21—Ru2—C23—C22 | 28.52 (13) |
| C3—Ru1—C2—C8 | 111.4 (3) | Cl3—Ru2—C23—C22 | −20.9 (2) |
| C1—Ru1—C2—C8 | −115.8 (3) | Cl1—Ru2—C23—C22 | −176.57 (11) |
| Cl3—Ru1—C2—C8 | −61.9 (2) | Cl2—Ru2—C23—C22 | −96.73 (13) |
| Cl1—Ru1—C2—C8 | 96.2 (3) | C25—Ru2—C23—C29 | −144.6 (2) |
| Cl2—Ru1—C2—C8 | 20.4 (2) | C26—Ru2—C23—C29 | 178.4 (2) |
| C1—C2—C3—C4 | 0.6 (3) | C24—Ru2—C23—C29 | −115.2 (3) |
| C8—C2—C3—C4 | −177.1 (2) | C22—Ru2—C23—C29 | 112.3 (3) |
| Ru1—C2—C3—C4 | −52.7 (2) | C21—Ru2—C23—C29 | 140.8 (2) |
| C1—C2—C3—C9 | 177.6 (2) | Cl3—Ru2—C23—C29 | 91.4 (2) |
| C8—C2—C3—C9 | −0.1 (3) | Cl1—Ru2—C23—C29 | −64.3 (2) |
| Ru1—C2—C3—C9 | 124.3 (2) | Cl2—Ru2—C23—C29 | 15.6 (2) |
| C1—C2—C3—Ru1 | 53.2 (2) | C22—C23—C24—C25 | −1.5 (3) |
| C8—C2—C3—Ru1 | −124.4 (2) | C29—C23—C24—C25 | 175.8 (2) |
| C5—Ru1—C3—C4 | 29.47 (14) | Ru2—C23—C24—C25 | 52.4 (2) |
| C6—Ru1—C3—C4 | 66.72 (15) | C22—C23—C24—C30 | −178.1 (2) |
| C2—Ru1—C3—C4 | 133.5 (2) | C29—C23—C24—C30 | −0.7 (4) |
| C1—Ru1—C3—C4 | 104.62 (16) | Ru2—C23—C24—C30 | −124.1 (2) |
| Cl3—Ru1—C3—C4 | 148.97 (15) | C22—C23—C24—Ru2 | −53.94 (19) |
| Cl1—Ru1—C3—C4 | −52.89 (15) | C29—C23—C24—Ru2 | 123.4 (2) |
| Cl2—Ru1—C3—C4 | −133.66 (13) | C25—Ru2—C24—C23 | 132.8 (2) |
| C4—Ru1—C3—C2 | −133.5 (2) | C26—Ru2—C24—C23 | 104.08 (15) |
| C5—Ru1—C3—C2 | −104.00 (15) | C22—Ru2—C24—C23 | 29.50 (13) |
| C6—Ru1—C3—C2 | −66.75 (14) | C21—Ru2—C24—C23 | 66.43 (14) |
| C1—Ru1—C3—C2 | −28.85 (14) | Cl3—Ru2—C24—C23 | 144.33 (17) |
| Cl3—Ru1—C3—C2 | 15.5 (3) | Cl1—Ru2—C24—C23 | −138.95 (12) |
| Cl1—Ru1—C3—C2 | 173.64 (11) | Cl2—Ru2—C24—C23 | −58.30 (14) |
| Cl2—Ru1—C3—C2 | 92.87 (13) | C23—Ru2—C24—C25 | −132.8 (2) |
| C4—Ru1—C3—C9 | 114.4 (3) | C26—Ru2—C24—C25 | −28.67 (14) |
| C5—Ru1—C3—C9 | 143.9 (3) | C22—Ru2—C24—C25 | −103.26 (15) |
| C6—Ru1—C3—C9 | −178.9 (2) | C21—Ru2—C24—C25 | −66.33 (14) |
| C2—Ru1—C3—C9 | −112.1 (3) | Cl3—Ru2—C24—C25 | 11.6 (3) |
| C1—Ru1—C3—C9 | −141.0 (3) | Cl1—Ru2—C24—C25 | 88.30 (13) |
| Cl3—Ru1—C3—C9 | −96.6 (3) | Cl2—Ru2—C24—C25 | 168.94 (11) |
| Cl1—Ru1—C3—C9 | 61.5 (2) | C25—Ru2—C24—C30 | −112.8 (3) |
| Cl2—Ru1—C3—C9 | −19.2 (2) | C23—Ru2—C24—C30 | 114.5 (3) |
| C2—C3—C4—C5 | −0.5 (3) | C26—Ru2—C24—C30 | −141.4 (2) |
| C9—C3—C4—C5 | −177.4 (2) | C22—Ru2—C24—C30 | 144.0 (2) |
| Ru1—C3—C4—C5 | −53.1 (2) | C21—Ru2—C24—C30 | −179.1 (2) |
| C2—C3—C4—C10 | 176.7 (2) | Cl3—Ru2—C24—C30 | −101.2 (3) |
| C9—C3—C4—C10 | −0.3 (4) | Cl1—Ru2—C24—C30 | −24.5 (2) |
| Ru1—C3—C4—C10 | 124.1 (2) | Cl2—Ru2—C24—C30 | 56.2 (2) |
| C2—C3—C4—Ru1 | 52.6 (2) | C23—C24—C25—C26 | 0.7 (3) |
| C9—C3—C4—Ru1 | −124.4 (2) | C30—C24—C25—C26 | 177.3 (2) |
| C5—Ru1—C4—C3 | −132.8 (2) | Ru2—C24—C25—C26 | 53.2 (2) |
| C6—Ru1—C4—C3 | −103.75 (16) | C23—C24—C25—C31 | −177.0 (2) |
| C2—Ru1—C4—C3 | −28.95 (14) | C30—C24—C25—C31 | −0.4 (4) |
| C1—Ru1—C4—C3 | −65.87 (15) | Ru2—C24—C25—C31 | −124.5 (2) |
| Cl3—Ru1—C4—C3 | −147.43 (16) | C23—C24—C25—Ru2 | −52.5 (2) |
| Cl1—Ru1—C4—C3 | 136.43 (13) | C30—C24—C25—Ru2 | 124.1 (2) |
| Cl2—Ru1—C4—C3 | 55.91 (15) | C23—Ru2—C25—C26 | −104.17 (15) |
| C6—Ru1—C4—C5 | 29.03 (14) | C24—Ru2—C25—C26 | −133.2 (2) |
| C3—Ru1—C4—C5 | 132.8 (2) | C22—Ru2—C25—C26 | −66.25 (14) |
| C2—Ru1—C4—C5 | 103.83 (16) | C21—Ru2—C25—C26 | −29.33 (14) |
| C1—Ru1—C4—C5 | 66.91 (15) | Cl3—Ru2—C25—C26 | 51.22 (15) |
| Cl3—Ru1—C4—C5 | −14.7 (3) | Cl1—Ru2—C25—C26 | 132.03 (13) |
| Cl1—Ru1—C4—C5 | −90.79 (14) | Cl2—Ru2—C25—C26 | −156.68 (13) |
| Cl2—Ru1—C4—C5 | −171.31 (12) | C23—Ru2—C25—C24 | 29.06 (13) |
| C5—Ru1—C4—C10 | 112.5 (3) | C26—Ru2—C25—C24 | 133.2 (2) |
| C6—Ru1—C4—C10 | 141.6 (2) | C22—Ru2—C25—C24 | 66.98 (14) |
| C3—Ru1—C4—C10 | −114.7 (3) | C21—Ru2—C25—C24 | 103.90 (15) |
| C2—Ru1—C4—C10 | −143.6 (2) | Cl3—Ru2—C25—C24 | −175.55 (11) |
| C1—Ru1—C4—C10 | 179.5 (2) | Cl1—Ru2—C25—C24 | −94.75 (13) |
| Cl3—Ru1—C4—C10 | 97.9 (3) | Cl2—Ru2—C25—C24 | −23.4 (2) |
| Cl1—Ru1—C4—C10 | 21.8 (2) | C23—Ru2—C25—C31 | 142.7 (2) |
| Cl2—Ru1—C4—C10 | −58.8 (2) | C26—Ru2—C25—C31 | −113.1 (3) |
| C3—C4—C5—C6 | 0.1 (3) | C24—Ru2—C25—C31 | 113.7 (3) |
| C10—C4—C5—C6 | −177.1 (2) | C22—Ru2—C25—C31 | −179.4 (2) |
| Ru1—C4—C5—C6 | −53.21 (19) | C21—Ru2—C25—C31 | −142.4 (2) |
| C3—C4—C5—C11 | 176.6 (2) | Cl3—Ru2—C25—C31 | −61.9 (2) |
| C10—C4—C5—C11 | −0.6 (3) | Cl1—Ru2—C25—C31 | 18.9 (2) |
| Ru1—C4—C5—C11 | 123.3 (2) | Cl2—Ru2—C25—C31 | 90.2 (3) |
| C3—C4—C5—Ru1 | 53.3 (2) | C24—C25—C26—C21 | 0.5 (3) |
| C10—C4—C5—Ru1 | −123.9 (2) | C31—C25—C26—C21 | 178.2 (2) |
| C4—Ru1—C5—C6 | 132.6 (2) | Ru2—C25—C26—C21 | 53.7 (2) |
| C3—Ru1—C5—C6 | 103.72 (15) | C24—C25—C26—C32 | −177.1 (2) |
| C2—Ru1—C5—C6 | 66.04 (14) | C31—C25—C26—C32 | 0.6 (3) |
| C1—Ru1—C5—C6 | 29.14 (14) | Ru2—C25—C26—C32 | −123.9 (2) |
| Cl3—Ru1—C5—C6 | −53.60 (15) | C24—C25—C26—Ru2 | −53.2 (2) |
| Cl1—Ru1—C5—C6 | −135.14 (13) | C31—C25—C26—Ru2 | 124.5 (2) |
| Cl2—Ru1—C5—C6 | 152.61 (15) | C22—C21—C26—C25 | −0.8 (3) |
| C6—Ru1—C5—C4 | −132.6 (2) | C27—C21—C26—C25 | −178.1 (2) |
| C3—Ru1—C5—C4 | −28.83 (14) | Ru2—C21—C26—C25 | −53.4 (2) |
| C2—Ru1—C5—C4 | −66.51 (15) | C22—C21—C26—C32 | 176.8 (2) |
| C1—Ru1—C5—C4 | −103.42 (16) | C27—C21—C26—C32 | −0.5 (3) |
| Cl3—Ru1—C5—C4 | 173.84 (12) | Ru2—C21—C26—C32 | 124.2 (2) |
| Cl1—Ru1—C5—C4 | 92.30 (14) | C22—C21—C26—Ru2 | 52.55 (19) |
| Cl2—Ru1—C5—C4 | 20.0 (3) | C27—C21—C26—Ru2 | −124.7 (2) |
| C4—Ru1—C5—C11 | −113.6 (3) | C23—Ru2—C26—C25 | 66.39 (15) |
| C6—Ru1—C5—C11 | 113.8 (3) | C24—Ru2—C26—C25 | 29.07 (14) |
| C3—Ru1—C5—C11 | −142.5 (2) | C22—Ru2—C26—C25 | 104.08 (15) |
| C2—Ru1—C5—C11 | 179.8 (2) | C21—Ru2—C26—C25 | 132.7 (2) |
| C1—Ru1—C5—C11 | 142.9 (2) | Cl3—Ru2—C26—C25 | −138.75 (13) |
| Cl3—Ru1—C5—C11 | 60.2 (2) | Cl1—Ru2—C26—C25 | −56.45 (15) |
| Cl1—Ru1—C5—C11 | −21.3 (2) | Cl2—Ru2—C26—C25 | 145.66 (19) |
| Cl2—Ru1—C5—C11 | −93.6 (3) | C25—Ru2—C26—C21 | −132.7 (2) |
| C4—C5—C6—C1 | 0.2 (3) | C23—Ru2—C26—C21 | −66.28 (15) |
| C11—C5—C6—C1 | −176.3 (2) | C24—Ru2—C26—C21 | −103.61 (15) |
| Ru1—C5—C6—C1 | −52.80 (19) | C22—Ru2—C26—C21 | −28.60 (14) |
| C4—C5—C6—C12 | 177.5 (2) | Cl3—Ru2—C26—C21 | 88.57 (13) |
| C11—C5—C6—C12 | 1.0 (3) | Cl1—Ru2—C26—C21 | 170.87 (12) |
| Ru1—C5—C6—C12 | 124.5 (2) | Cl2—Ru2—C26—C21 | 13.0 (3) |
| C4—C5—C6—Ru1 | 52.98 (19) | C25—Ru2—C26—C32 | 113.2 (3) |
| C11—C5—C6—Ru1 | −123.5 (2) | C23—Ru2—C26—C32 | 179.6 (2) |
| C2—C1—C6—C5 | −0.1 (3) | C24—Ru2—C26—C32 | 142.2 (3) |
| C7—C1—C6—C5 | 177.0 (2) | C22—Ru2—C26—C32 | −142.8 (3) |
| Ru1—C1—C6—C5 | 52.9 (2) | C21—Ru2—C26—C32 | −114.2 (3) |
| C2—C1—C6—C12 | −177.4 (2) | Cl3—Ru2—C26—C32 | −25.6 (2) |
| C7—C1—C6—C12 | −0.3 (3) | Cl1—Ru2—C26—C32 | 56.7 (2) |
| Ru1—C1—C6—C12 | −124.4 (2) | Cl2—Ru2—C26—C32 | −101.2 (3) |
Hydrogen-bond geometry (Å, °)
| D—H···A | D—H | H···A | D···A | D—H···A |
| C9—H9A···Cl3i | 0.96 | 2.80 | 3.629 (3) | 145 |
| C11—H11B···Cl6ii | 0.96 | 2.71 | 3.588 (3) | 153 |
Symmetry codes: (i) x+1, y, z; (ii) x, y−1, z.
Footnotes
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2311).
References
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Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S160053681103621X/su2311sup1.cif
Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681103621X/su2311Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report


