Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536812033454/su2478sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536812033454/su2478Isup2.hkl |
CCDC reference: 899575
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.005 Å
- R factor = 0.032
- wR factor = 0.077
- Data-to-parameter ratio = 15.1
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT230_ALERT_2_C Hirshfeld Test Diff for O3 -- C26 .. 6.0 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru1 -- C23 .. 7.3 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru2 -- C25 .. 6.0 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru2 -- C26 .. 6.9 su PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.595 76
Alert level G PLAT005_ALERT_5_G No _iucr_refine_instructions_details in CIF .... ? PLAT909_ALERT_3_G Percentage of Observed Data at Theta(Max) still 76 Perc.
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 5 ALERT level C = Check. Ensure it is not caused by an omission or oversight 2 ALERT level G = General information/check it is not something unexpected 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
A solution of (C5H3tBu)(SiMe2))2 (80 mg, 0.22 mmol) and Ru3(CO)12 (80 mg, 0.13 mmol) in xylene (20 ml) was refluxed for 15 h. After removal of the solvent under reduced pressure, the residue, which was dissolved in a minimum amount of CH2Cl2, the solution was chromatographed on an alumina column using petroleum ether–CH2Cl2 (5:1) as eluent. A yellow band was eluted and collected. After removal of the solvents under vacuum from the above eluate, the residue was recrystallized from n-hexane/CH2Cl2 (1:1) at 263 K to give colourless crystals of the title compound (54 mg, 36%). Anal. Calcd for C26H34O4Ru2Si2: C, 46.69; H, 5.12. Found: C, 46.82; H, 5.17. Spectroscopic data for the title compound is given in the archived CIF.
All the hydrogen atoms could be located in difference electron density maps. In th final cycles of refinement they were included in calculated positions and treated as riding atoms: C-H = 0.98 and 1.00 Å for CH3 and CH H-atoms, respectively, with Uiso(H) = k × Ueq(parent C-atom), where k = 1.5 for CH3 H-atoms and = 1.2 for other H-atoms.
Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
Fig. 1. A view of the molecular structure of the title compound with the atom numbering. Displacement ellipsoids are drawn at the 30% probability level. |
[Ru2(C22H34Si2)(CO)4] | Z = 2 |
Mr = 668.85 | F(000) = 676 |
Triclinic, P1 | Dx = 1.605 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.632 (3) Å | Cell parameters from 3308 reflections |
b = 10.886 (3) Å | θ = 2.4–28.3° |
c = 14.546 (5) Å | µ = 1.21 mm−1 |
α = 89.518 (5)° | T = 173 K |
β = 71.581 (4)° | Block, yellow |
γ = 61.560 (4)° | 0.17 × 0.16 × 0.15 mm |
V = 1384.0 (7) Å3 |
Bruker APEXII CCD diffractometer | 4802 independent reflections |
Radiation source: fine-focus sealed tube | 4101 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Bruker, 2005) | h = −12→11 |
Tmin = 0.821, Tmax = 0.840 | k = −12→6 |
6921 measured reflections | l = −17→17 |
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)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.077 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0409P)2] where P = (Fo2 + 2Fc2)/3 |
4802 reflections | (Δ/σ)max < 0.001 |
317 parameters | Δρmax = 0.92 e Å−3 |
0 restraints | Δρmin = −0.86 e Å−3 |
[Ru2(C22H34Si2)(CO)4] | γ = 61.560 (4)° |
Mr = 668.85 | V = 1384.0 (7) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.632 (3) Å | Mo Kα radiation |
b = 10.886 (3) Å | µ = 1.21 mm−1 |
c = 14.546 (5) Å | T = 173 K |
α = 89.518 (5)° | 0.17 × 0.16 × 0.15 mm |
β = 71.581 (4)° |
Bruker APEXII CCD diffractometer | 4802 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2005) | 4101 reflections with I > 2σ(I) |
Tmin = 0.821, Tmax = 0.840 | Rint = 0.029 |
6921 measured reflections |
R[F2 > 2σ(F2)] = 0.032 | 0 restraints |
wR(F2) = 0.077 | H-atom parameters constrained |
S = 1.04 | Δρmax = 0.92 e Å−3 |
4802 reflections | Δρmin = −0.86 e Å−3 |
317 parameters |
Experimental. Spectroscopic data for the title compound: 1H NMR (CDCl3): δ 5.26 (s, 4H, C5H2), 1.33 (s, 18H, C(CH3)3), 0.44 (s, 6H, Si(CH3)), 0.23 (s, 6H, Si(CH3)). IR (νCO): 2016(s), 1964(s), 1953(s), 1918(s) cm-1. |
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 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. |
x | y | z | Uiso*/Ueq | ||
Ru1 | 0.18780 (3) | 0.25054 (2) | 0.24573 (2) | 0.0120 (1) | |
Ru2 | −0.01860 (3) | 0.14546 (3) | 0.30871 (2) | 0.0119 (1) | |
Si1 | 0.05491 (10) | 0.22259 (9) | 0.06637 (7) | 0.0147 (2) | |
Si2 | −0.20390 (10) | 0.49039 (9) | 0.27597 (7) | 0.0155 (3) | |
O1 | 0.2229 (3) | 0.2477 (3) | 0.44361 (19) | 0.0323 (9) | |
O2 | 0.4503 (3) | −0.0461 (2) | 0.16495 (19) | 0.0268 (8) | |
O3 | −0.0771 (3) | 0.2370 (3) | 0.51910 (18) | 0.0369 (9) | |
O4 | 0.2411 (3) | −0.1387 (2) | 0.3097 (2) | 0.0320 (9) | |
C1 | 0.1049 (4) | 0.3370 (3) | 0.1239 (2) | 0.0144 (9) | |
C2 | 0.0009 (4) | 0.4414 (3) | 0.2140 (2) | 0.0135 (9) | |
C3 | 0.0875 (3) | 0.4865 (3) | 0.2459 (2) | 0.0140 (9) | |
C4 | 0.2440 (4) | 0.4151 (3) | 0.1790 (2) | 0.0147 (9) | |
C5 | 0.2514 (4) | 0.3265 (3) | 0.1043 (2) | 0.0148 (9) | |
C6 | 0.3673 (4) | 0.4458 (3) | 0.1819 (2) | 0.0144 (9) | |
C7 | 0.3545 (4) | 0.4787 (4) | 0.2878 (2) | 0.0205 (11) | |
C8 | 0.3461 (4) | 0.5772 (3) | 0.1329 (3) | 0.0222 (11) | |
C9 | 0.5264 (4) | 0.3196 (3) | 0.1258 (3) | 0.0204 (10) | |
C10 | −0.0830 (3) | 0.2036 (3) | 0.1740 (2) | 0.0138 (9) | |
C11 | −0.0919 (3) | 0.0804 (3) | 0.1964 (2) | 0.0124 (9) | |
C12 | −0.2045 (3) | 0.1098 (3) | 0.2926 (2) | 0.0152 (9) | |
C13 | −0.2670 (3) | 0.2564 (3) | 0.3280 (2) | 0.0141 (9) | |
C14 | −0.1938 (3) | 0.3164 (3) | 0.2584 (2) | 0.0141 (9) | |
C15 | −0.2601 (4) | 0.0125 (3) | 0.3415 (2) | 0.0153 (9) | |
C16 | −0.3307 (4) | 0.0588 (4) | 0.4535 (2) | 0.0262 (11) | |
C17 | −0.3792 (4) | 0.0198 (4) | 0.3014 (3) | 0.0267 (11) | |
C18 | −0.1273 (4) | −0.1413 (3) | 0.3170 (3) | 0.0210 (10) | |
C19 | −0.0376 (4) | 0.3094 (4) | −0.0237 (3) | 0.0242 (11) | |
C20 | 0.2232 (4) | 0.0455 (3) | 0.0048 (2) | 0.0220 (10) | |
C21 | −0.2787 (4) | 0.5623 (3) | 0.4091 (3) | 0.0237 (11) | |
C22 | −0.3234 (4) | 0.6240 (3) | 0.2140 (3) | 0.0261 (11) | |
C23 | 0.2077 (4) | 0.2457 (3) | 0.3686 (3) | 0.0219 (11) | |
C24 | 0.3476 (4) | 0.0650 (3) | 0.1998 (2) | 0.0165 (10) | |
C25 | 0.1445 (4) | −0.0298 (3) | 0.3083 (3) | 0.0189 (10) | |
C26 | −0.0499 (4) | 0.2012 (4) | 0.4378 (3) | 0.0226 (11) | |
H3 | 0.04540 | 0.55950 | 0.30500 | 0.0170* | |
H5 | 0.34450 | 0.26760 | 0.04500 | 0.0180* | |
H7A | 0.25240 | 0.55820 | 0.32450 | 0.0310* | |
H7B | 0.43190 | 0.50370 | 0.28730 | 0.0310* | |
H7C | 0.37120 | 0.39500 | 0.31920 | 0.0310* | |
H8A | 0.35170 | 0.55850 | 0.06550 | 0.0330* | |
H8B | 0.42700 | 0.59750 | 0.13150 | 0.0330* | |
H8C | 0.24610 | 0.65890 | 0.17040 | 0.0330* | |
H9A | 0.53660 | 0.23440 | 0.15360 | 0.0310* | |
H9B | 0.60470 | 0.33920 | 0.13170 | 0.0310* | |
H9C | 0.53960 | 0.30440 | 0.05630 | 0.0310* | |
H11 | −0.03090 | −0.01300 | 0.15120 | 0.0150* | |
H13 | −0.35290 | 0.31030 | 0.39170 | 0.0170* | |
H16A | −0.25520 | 0.05990 | 0.47790 | 0.0390* | |
H16B | −0.36150 | −0.00790 | 0.48400 | 0.0390* | |
H16C | −0.42060 | 0.15410 | 0.47030 | 0.0390* | |
H17A | −0.46140 | 0.11850 | 0.31340 | 0.0400* | |
H17B | −0.42160 | −0.03800 | 0.33450 | 0.0400* | |
H17C | −0.33110 | −0.01620 | 0.23060 | 0.0400* | |
H18A | −0.08330 | −0.17310 | 0.24570 | 0.0310* | |
H18B | −0.16540 | −0.20260 | 0.34930 | 0.0310* | |
H18C | −0.04840 | −0.14630 | 0.34060 | 0.0310* | |
H19A | 0.03670 | 0.31820 | −0.07970 | 0.0370* | |
H19B | −0.12490 | 0.40380 | 0.00820 | 0.0370* | |
H19C | −0.07320 | 0.25180 | −0.04680 | 0.0370* | |
H20A | 0.30570 | 0.05720 | −0.04050 | 0.0330* | |
H20B | 0.19430 | −0.00550 | −0.03200 | 0.0330* | |
H20C | 0.25830 | −0.00850 | 0.05440 | 0.0330* | |
H21A | −0.37670 | 0.56560 | 0.44120 | 0.0360* | |
H21B | −0.29370 | 0.65810 | 0.41720 | 0.0360* | |
H21C | −0.20530 | 0.50100 | 0.43920 | 0.0360* | |
H22A | −0.28710 | 0.58440 | 0.14440 | 0.0390* | |
H22B | −0.31540 | 0.70950 | 0.21930 | 0.0390* | |
H22C | −0.43040 | 0.64830 | 0.24560 | 0.0390* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.0114 (1) | 0.0114 (1) | 0.0144 (2) | −0.0058 (1) | −0.0059 (1) | 0.0043 (1) |
Ru2 | 0.0112 (1) | 0.0122 (1) | 0.0127 (2) | −0.0060 (1) | −0.0045 (1) | 0.0041 (1) |
Si1 | 0.0167 (4) | 0.0169 (4) | 0.0132 (4) | −0.0095 (4) | −0.0069 (4) | 0.0049 (4) |
Si2 | 0.0113 (4) | 0.0105 (4) | 0.0237 (5) | −0.0045 (3) | −0.0067 (4) | 0.0036 (4) |
O1 | 0.0476 (17) | 0.0405 (16) | 0.0266 (15) | −0.0297 (14) | −0.0226 (14) | 0.0152 (13) |
O2 | 0.0179 (12) | 0.0184 (13) | 0.0359 (15) | −0.0051 (11) | −0.0060 (11) | 0.0046 (11) |
O3 | 0.0342 (15) | 0.0594 (19) | 0.0155 (14) | −0.0219 (14) | −0.0090 (12) | 0.0016 (13) |
O4 | 0.0219 (13) | 0.0200 (13) | 0.0533 (18) | −0.0085 (12) | −0.0159 (13) | 0.0177 (12) |
C1 | 0.0159 (16) | 0.0147 (16) | 0.0168 (17) | −0.0103 (13) | −0.0066 (14) | 0.0086 (13) |
C2 | 0.0137 (15) | 0.0096 (15) | 0.0185 (17) | −0.0062 (13) | −0.0068 (14) | 0.0058 (13) |
C3 | 0.0158 (16) | 0.0088 (15) | 0.0181 (17) | −0.0057 (13) | −0.0075 (14) | 0.0032 (13) |
C4 | 0.0181 (16) | 0.0127 (15) | 0.0146 (16) | −0.0086 (13) | −0.0060 (14) | 0.0071 (13) |
C5 | 0.0187 (16) | 0.0167 (16) | 0.0133 (16) | −0.0118 (14) | −0.0060 (14) | 0.0055 (13) |
C6 | 0.0159 (16) | 0.0169 (16) | 0.0152 (16) | −0.0109 (14) | −0.0068 (14) | 0.0031 (13) |
C7 | 0.0236 (18) | 0.0253 (18) | 0.0234 (19) | −0.0166 (15) | −0.0143 (16) | 0.0055 (15) |
C8 | 0.0194 (17) | 0.0210 (18) | 0.032 (2) | −0.0123 (15) | −0.0127 (16) | 0.0119 (16) |
C9 | 0.0161 (17) | 0.0212 (17) | 0.0256 (19) | −0.0099 (14) | −0.0087 (15) | 0.0048 (15) |
C10 | 0.0140 (16) | 0.0133 (15) | 0.0169 (17) | −0.0061 (13) | −0.0102 (14) | 0.0053 (13) |
C11 | 0.0127 (15) | 0.0132 (15) | 0.0158 (16) | −0.0080 (13) | −0.0082 (13) | 0.0025 (13) |
C12 | 0.0127 (15) | 0.0160 (16) | 0.0176 (17) | −0.0066 (13) | −0.0070 (14) | 0.0031 (13) |
C13 | 0.0082 (14) | 0.0137 (16) | 0.0215 (17) | −0.0046 (13) | −0.0080 (13) | 0.0031 (13) |
C14 | 0.0099 (15) | 0.0139 (16) | 0.0175 (17) | −0.0040 (13) | −0.0068 (13) | 0.0048 (13) |
C15 | 0.0157 (16) | 0.0126 (15) | 0.0196 (17) | −0.0087 (13) | −0.0062 (14) | 0.0065 (13) |
C16 | 0.032 (2) | 0.0204 (18) | 0.0217 (19) | −0.0150 (16) | −0.0009 (16) | 0.0039 (15) |
C17 | 0.0237 (19) | 0.029 (2) | 0.039 (2) | −0.0179 (16) | −0.0178 (17) | 0.0178 (17) |
C18 | 0.0185 (17) | 0.0165 (17) | 0.0252 (19) | −0.0086 (14) | −0.0047 (15) | 0.0088 (15) |
C19 | 0.031 (2) | 0.030 (2) | 0.0216 (18) | −0.0191 (17) | −0.0154 (16) | 0.0109 (16) |
C20 | 0.0219 (18) | 0.0234 (18) | 0.0202 (18) | −0.0117 (15) | −0.0061 (15) | −0.0003 (15) |
C21 | 0.0208 (18) | 0.0196 (18) | 0.030 (2) | −0.0114 (15) | −0.0060 (16) | −0.0016 (15) |
C22 | 0.0214 (18) | 0.0153 (17) | 0.045 (2) | −0.0094 (15) | −0.0155 (17) | 0.0089 (16) |
C23 | 0.0251 (19) | 0.0179 (17) | 0.028 (2) | −0.0140 (15) | −0.0106 (17) | 0.0082 (15) |
C24 | 0.0160 (17) | 0.0173 (17) | 0.0200 (17) | −0.0100 (15) | −0.0084 (14) | 0.0096 (14) |
C25 | 0.0195 (17) | 0.0229 (18) | 0.0228 (18) | −0.0156 (16) | −0.0097 (15) | 0.0104 (15) |
C26 | 0.0160 (17) | 0.0288 (19) | 0.025 (2) | −0.0124 (15) | −0.0079 (16) | 0.0075 (16) |
Ru1—Ru2 | 2.8401 (11) | C12—C15 | 1.515 (5) |
Ru1—C1 | 2.230 (3) | C13—C14 | 1.426 (4) |
Ru1—C2 | 2.260 (4) | C15—C16 | 1.534 (4) |
Ru1—C3 | 2.264 (3) | C15—C17 | 1.523 (7) |
Ru1—C4 | 2.265 (4) | C15—C18 | 1.538 (5) |
Ru1—C5 | 2.236 (3) | C3—H3 | 1.0000 |
Ru1—C23 | 1.863 (4) | C5—H5 | 1.0000 |
Ru1—C24 | 1.857 (3) | C7—H7A | 0.9800 |
Ru2—C10 | 2.263 (3) | C7—H7B | 0.9800 |
Ru2—C11 | 2.264 (3) | C7—H7C | 0.9800 |
Ru2—C12 | 2.267 (4) | C8—H8A | 0.9800 |
Ru2—C13 | 2.239 (4) | C8—H8B | 0.9800 |
Ru2—C14 | 2.237 (3) | C8—H8C | 0.9800 |
Ru2—C25 | 1.868 (3) | C9—H9A | 0.9800 |
Ru2—C26 | 1.854 (4) | C9—H9B | 0.9800 |
Si1—C1 | 1.861 (4) | C9—H9C | 0.9800 |
Si1—C10 | 1.865 (3) | C11—H11 | 1.0000 |
Si1—C19 | 1.867 (4) | C13—H13 | 1.0000 |
Si1—C20 | 1.858 (3) | C16—H16A | 0.9800 |
Si2—C2 | 1.871 (4) | C16—H16B | 0.9800 |
Si2—C14 | 1.861 (3) | C16—H16C | 0.9800 |
Si2—C21 | 1.859 (4) | C17—H17A | 0.9800 |
Si2—C22 | 1.867 (4) | C17—H17B | 0.9800 |
O1—C23 | 1.154 (5) | C17—H17C | 0.9800 |
O2—C24 | 1.147 (4) | C18—H18A | 0.9800 |
O3—C26 | 1.148 (5) | C18—H18B | 0.9800 |
O4—C25 | 1.146 (4) | C18—H18C | 0.9800 |
C1—C2 | 1.464 (4) | C19—H19A | 0.9800 |
C1—C5 | 1.439 (6) | C19—H19B | 0.9800 |
C2—C3 | 1.417 (6) | C19—H19C | 0.9800 |
C3—C4 | 1.441 (5) | C20—H20A | 0.9800 |
C4—C5 | 1.417 (5) | C20—H20B | 0.9800 |
C4—C6 | 1.511 (6) | C20—H20C | 0.9800 |
C6—C7 | 1.533 (4) | C21—H21A | 0.9800 |
C6—C8 | 1.543 (4) | C21—H21B | 0.9800 |
C6—C9 | 1.532 (5) | C21—H21C | 0.9800 |
C10—C11 | 1.417 (4) | C22—H22A | 0.9800 |
C10—C14 | 1.462 (4) | C22—H22B | 0.9800 |
C11—C12 | 1.441 (4) | C22—H22C | 0.9800 |
C12—C13 | 1.429 (4) | ||
Ru2—Ru1—C1 | 92.46 (11) | Si1—C10—C14 | 123.8 (2) |
Ru2—Ru1—C2 | 87.88 (11) | C11—C10—C14 | 107.0 (3) |
Ru2—Ru1—C3 | 117.71 (9) | Ru2—C11—C10 | 71.73 (18) |
Ru2—Ru1—C4 | 150.11 (11) | Ru2—C11—C12 | 71.53 (18) |
Ru2—Ru1—C5 | 127.88 (12) | C10—C11—C12 | 110.4 (2) |
Ru2—Ru1—C23 | 90.24 (14) | Ru2—C12—C11 | 71.4 (2) |
Ru2—Ru1—C24 | 88.90 (13) | Ru2—C12—C13 | 70.5 (2) |
C1—Ru1—C2 | 38.06 (10) | Ru2—C12—C15 | 128.1 (2) |
C1—Ru1—C3 | 62.19 (11) | C11—C12—C13 | 105.4 (3) |
C1—Ru1—C4 | 62.96 (14) | C11—C12—C15 | 127.8 (3) |
C1—Ru1—C5 | 37.60 (16) | C13—C12—C15 | 126.5 (3) |
C1—Ru1—C23 | 159.41 (12) | Ru2—C13—C12 | 72.6 (2) |
C1—Ru1—C24 | 108.96 (12) | Ru2—C13—C14 | 71.4 (2) |
C2—Ru1—C3 | 36.51 (14) | C12—C13—C14 | 110.6 (3) |
C2—Ru1—C4 | 62.34 (15) | Ru2—C14—Si2 | 113.04 (17) |
C2—Ru1—C5 | 62.11 (13) | Ru2—C14—C10 | 72.03 (17) |
C2—Ru1—C23 | 121.78 (13) | Ru2—C14—C13 | 71.48 (18) |
C2—Ru1—C24 | 146.58 (13) | Si2—C14—C10 | 124.1 (2) |
C3—Ru1—C4 | 37.11 (12) | Si2—C14—C13 | 128.4 (2) |
C3—Ru1—C5 | 60.99 (10) | C10—C14—C13 | 106.6 (3) |
C3—Ru1—C23 | 98.65 (12) | C12—C15—C16 | 110.7 (3) |
C3—Ru1—C24 | 151.24 (14) | C12—C15—C17 | 107.6 (3) |
C4—Ru1—C5 | 36.70 (12) | C12—C15—C18 | 110.7 (3) |
C4—Ru1—C23 | 107.05 (15) | C16—C15—C17 | 110.2 (3) |
C4—Ru1—C24 | 114.14 (15) | C16—C15—C18 | 108.8 (3) |
C5—Ru1—C23 | 141.38 (17) | C17—C15—C18 | 108.9 (3) |
C5—Ru1—C24 | 94.77 (12) | Ru1—C23—O1 | 176.4 (4) |
C23—Ru1—C24 | 91.48 (14) | Ru1—C24—O2 | 174.7 (3) |
Ru1—Ru2—C10 | 88.92 (9) | Ru2—C25—O4 | 177.7 (4) |
Ru1—Ru2—C11 | 118.88 (8) | Ru2—C26—O3 | 176.4 (4) |
Ru1—Ru2—C12 | 151.16 (7) | Ru1—C3—H3 | 125.00 |
Ru1—Ru2—C13 | 127.78 (8) | C2—C3—H3 | 125.00 |
Ru1—Ru2—C14 | 93.14 (9) | C4—C3—H3 | 125.00 |
Ru1—Ru2—C25 | 89.05 (14) | Ru1—C5—H5 | 125.00 |
Ru1—Ru2—C26 | 88.82 (15) | C1—C5—H5 | 125.00 |
C10—Ru2—C11 | 36.47 (11) | C4—C5—H5 | 125.00 |
C10—Ru2—C12 | 62.40 (11) | C6—C7—H7A | 109.00 |
C10—Ru2—C13 | 61.87 (11) | C6—C7—H7B | 109.00 |
C10—Ru2—C14 | 37.90 (10) | C6—C7—H7C | 109.00 |
C10—Ru2—C25 | 122.62 (15) | H7A—C7—H7B | 110.00 |
C10—Ru2—C26 | 148.19 (15) | H7A—C7—H7C | 110.00 |
C11—Ru2—C12 | 37.10 (11) | H7B—C7—H7C | 109.00 |
C11—Ru2—C13 | 60.93 (11) | C6—C8—H8A | 109.00 |
C11—Ru2—C14 | 61.88 (11) | C6—C8—H8B | 110.00 |
C11—Ru2—C25 | 100.00 (15) | C6—C8—H8C | 110.00 |
C11—Ru2—C26 | 150.71 (17) | H8A—C8—H8B | 109.00 |
C12—Ru2—C13 | 36.97 (11) | H8A—C8—H8C | 109.00 |
C12—Ru2—C14 | 62.81 (12) | H8B—C8—H8C | 110.00 |
C12—Ru2—C25 | 108.32 (16) | C6—C9—H9A | 109.00 |
C12—Ru2—C26 | 113.61 (17) | C6—C9—H9B | 109.00 |
C13—Ru2—C14 | 37.15 (11) | C6—C9—H9C | 109.00 |
C13—Ru2—C25 | 142.88 (16) | H9A—C9—H9B | 109.00 |
C13—Ru2—C26 | 95.42 (16) | H9A—C9—H9C | 109.00 |
C14—Ru2—C25 | 160.22 (15) | H9B—C9—H9C | 110.00 |
C14—Ru2—C26 | 110.62 (15) | Ru2—C11—H11 | 125.00 |
C25—Ru2—C26 | 89.06 (18) | C10—C11—H11 | 125.00 |
C1—Si1—C10 | 102.63 (14) | C12—C11—H11 | 125.00 |
C1—Si1—C19 | 111.50 (17) | Ru2—C13—H13 | 125.00 |
C1—Si1—C20 | 112.56 (19) | C12—C13—H13 | 125.00 |
C10—Si1—C19 | 110.73 (19) | C14—C13—H13 | 125.00 |
C10—Si1—C20 | 109.94 (14) | C15—C16—H16A | 109.00 |
C19—Si1—C20 | 109.34 (16) | C15—C16—H16B | 109.00 |
C2—Si2—C14 | 101.74 (15) | C15—C16—H16C | 110.00 |
C2—Si2—C21 | 112.61 (19) | H16A—C16—H16B | 109.00 |
C2—Si2—C22 | 109.47 (17) | H16A—C16—H16C | 109.00 |
C14—Si2—C21 | 110.45 (14) | H16B—C16—H16C | 109.00 |
C14—Si2—C22 | 113.01 (17) | C15—C17—H17A | 109.00 |
C21—Si2—C22 | 109.43 (17) | C15—C17—H17B | 109.00 |
Ru1—C1—Si1 | 112.78 (14) | C15—C17—H17C | 109.00 |
Ru1—C1—C2 | 72.10 (18) | H17A—C17—H17B | 110.00 |
Ru1—C1—C5 | 71.42 (19) | H17A—C17—H17C | 109.00 |
Si1—C1—C2 | 123.5 (3) | H17B—C17—H17C | 110.00 |
Si1—C1—C5 | 129.5 (2) | C15—C18—H18A | 110.00 |
C2—C1—C5 | 106.0 (3) | C15—C18—H18B | 109.00 |
Ru1—C2—Si2 | 120.17 (15) | C15—C18—H18C | 109.00 |
Ru1—C2—C1 | 69.84 (18) | H18A—C18—H18B | 110.00 |
Ru1—C2—C3 | 71.9 (2) | H18A—C18—H18C | 109.00 |
Si2—C2—C1 | 124.1 (3) | H18B—C18—H18C | 109.00 |
Si2—C2—C3 | 128.5 (2) | Si1—C19—H19A | 109.00 |
C1—C2—C3 | 107.3 (3) | Si1—C19—H19B | 109.00 |
Ru1—C3—C2 | 71.62 (17) | Si1—C19—H19C | 109.00 |
Ru1—C3—C4 | 71.51 (17) | H19A—C19—H19B | 109.00 |
C2—C3—C4 | 110.1 (3) | H19A—C19—H19C | 110.00 |
Ru1—C4—C3 | 71.38 (19) | H19B—C19—H19C | 109.00 |
Ru1—C4—C5 | 70.51 (19) | Si1—C20—H20A | 109.00 |
Ru1—C4—C6 | 129.1 (2) | Si1—C20—H20B | 109.00 |
C3—C4—C5 | 106.0 (4) | Si1—C20—H20C | 109.00 |
C3—C4—C6 | 125.9 (3) | H20A—C20—H20B | 109.00 |
C5—C4—C6 | 127.6 (3) | H20A—C20—H20C | 109.00 |
Ru1—C5—C1 | 70.98 (17) | H20B—C20—H20C | 110.00 |
Ru1—C5—C4 | 72.79 (17) | Si2—C21—H21A | 109.00 |
C1—C5—C4 | 110.5 (3) | Si2—C21—H21B | 110.00 |
C4—C6—C7 | 111.5 (3) | Si2—C21—H21C | 109.00 |
C4—C6—C8 | 107.7 (3) | H21A—C21—H21B | 109.00 |
C4—C6—C9 | 110.7 (3) | H21A—C21—H21C | 109.00 |
C7—C6—C8 | 108.5 (3) | H21B—C21—H21C | 109.00 |
C7—C6—C9 | 109.0 (3) | Si2—C22—H22A | 109.00 |
C8—C6—C9 | 109.5 (3) | Si2—C22—H22B | 110.00 |
Ru2—C10—Si1 | 118.11 (18) | Si2—C22—H22C | 110.00 |
Ru2—C10—C11 | 71.80 (17) | H22A—C22—H22B | 109.00 |
Ru2—C10—C14 | 70.08 (16) | H22A—C22—H22C | 109.00 |
Si1—C10—C11 | 128.8 (2) | H22B—C22—H22C | 109.00 |
C1—Ru1—Ru2—C10 | 7.43 (11) | C26—Ru2—C11—C10 | 120.7 (3) |
C1—Ru1—Ru2—C11 | 29.18 (12) | C26—Ru2—C11—C12 | 0.9 (4) |
C1—Ru1—Ru2—C12 | 1.64 (17) | Ru1—Ru2—C12—C11 | 42.2 (2) |
C1—Ru1—Ru2—C13 | −44.89 (12) | Ru1—Ru2—C12—C13 | −72.5 (2) |
C1—Ru1—Ru2—C14 | −30.24 (10) | Ru1—Ru2—C12—C15 | 165.97 (16) |
C1—Ru1—Ru2—C25 | 130.09 (15) | C10—Ru2—C12—C11 | 35.62 (16) |
C1—Ru1—Ru2—C26 | −140.84 (15) | C10—Ru2—C12—C13 | −79.05 (17) |
C2—Ru1—Ru2—C10 | 45.23 (10) | C10—Ru2—C12—C15 | 159.4 (3) |
C2—Ru1—Ru2—C11 | 66.97 (11) | C11—Ru2—C12—C13 | −114.7 (2) |
C2—Ru1—Ru2—C12 | 39.44 (17) | C11—Ru2—C12—C15 | 123.8 (3) |
C2—Ru1—Ru2—C13 | −7.10 (12) | C13—Ru2—C12—C11 | 114.7 (2) |
C2—Ru1—Ru2—C14 | 7.55 (10) | C13—Ru2—C12—C15 | −121.5 (3) |
C2—Ru1—Ru2—C25 | 167.88 (15) | C14—Ru2—C12—C11 | 78.52 (17) |
C2—Ru1—Ru2—C26 | −103.04 (15) | C14—Ru2—C12—C13 | −36.14 (16) |
C3—Ru1—Ru2—C10 | 67.10 (11) | C14—Ru2—C12—C15 | −157.7 (3) |
C3—Ru1—Ru2—C11 | 88.85 (12) | C25—Ru2—C12—C11 | −82.3 (2) |
C3—Ru1—Ru2—C12 | 61.31 (17) | C25—Ru2—C12—C13 | 163.07 (19) |
C3—Ru1—Ru2—C13 | 14.78 (12) | C25—Ru2—C12—C15 | 41.6 (3) |
C3—Ru1—Ru2—C14 | 29.43 (11) | C26—Ru2—C12—C11 | −179.50 (19) |
C3—Ru1—Ru2—C25 | −170.24 (15) | C26—Ru2—C12—C13 | 65.8 (2) |
C3—Ru1—Ru2—C26 | −81.16 (15) | C26—Ru2—C12—C15 | −55.7 (3) |
C4—Ru1—Ru2—C10 | 40.45 (16) | Ru1—Ru2—C13—C12 | 144.40 (13) |
C4—Ru1—Ru2—C11 | 62.19 (17) | Ru1—Ru2—C13—C14 | 24.7 (2) |
C4—Ru1—Ru2—C12 | 34.7 (2) | C10—Ru2—C13—C12 | 80.59 (17) |
C4—Ru1—Ru2—C13 | −11.88 (17) | C10—Ru2—C13—C14 | −39.09 (17) |
C4—Ru1—Ru2—C14 | 2.77 (16) | C11—Ru2—C13—C12 | 38.84 (16) |
C4—Ru1—Ru2—C25 | 163.10 (19) | C11—Ru2—C13—C14 | −80.84 (18) |
C4—Ru1—Ru2—C26 | −107.82 (19) | C12—Ru2—C13—C14 | −119.7 (2) |
C5—Ru1—Ru2—C10 | −6.32 (12) | C14—Ru2—C13—C12 | 119.7 (2) |
C5—Ru1—Ru2—C11 | 15.43 (13) | C25—Ru2—C13—C12 | −27.3 (3) |
C5—Ru1—Ru2—C12 | −12.11 (18) | C25—Ru2—C13—C14 | −146.9 (3) |
C5—Ru1—Ru2—C13 | −58.64 (13) | C26—Ru2—C13—C12 | −122.88 (19) |
C5—Ru1—Ru2—C14 | −43.99 (12) | C26—Ru2—C13—C14 | 117.4 (2) |
C5—Ru1—Ru2—C25 | 116.34 (16) | Ru1—Ru2—C14—Si2 | −36.01 (14) |
C5—Ru1—Ru2—C26 | −154.58 (16) | Ru1—Ru2—C14—C10 | 84.19 (18) |
C23—Ru1—Ru2—C10 | 167.02 (13) | Ru1—Ru2—C14—C13 | −160.67 (16) |
C23—Ru1—Ru2—C11 | −171.24 (13) | C10—Ru2—C14—Si2 | −120.2 (3) |
C23—Ru1—Ru2—C12 | 161.23 (18) | C10—Ru2—C14—C13 | 115.1 (3) |
C23—Ru1—Ru2—C13 | 114.70 (14) | C11—Ru2—C14—Si2 | −157.3 (2) |
C23—Ru1—Ru2—C14 | 129.34 (12) | C11—Ru2—C14—C10 | −37.08 (19) |
C23—Ru1—Ru2—C25 | −70.33 (16) | C11—Ru2—C14—C13 | 78.06 (19) |
C23—Ru1—Ru2—C26 | 18.75 (16) | C12—Ru2—C14—Si2 | 160.63 (18) |
C24—Ru1—Ru2—C10 | −101.50 (12) | C12—Ru2—C14—C10 | −79.2 (2) |
C24—Ru1—Ru2—C11 | −79.76 (13) | C12—Ru2—C14—C13 | 35.97 (17) |
C24—Ru1—Ru2—C12 | −107.29 (18) | C13—Ru2—C14—Si2 | 124.7 (2) |
C24—Ru1—Ru2—C13 | −153.83 (13) | C13—Ru2—C14—C10 | −115.1 (3) |
C24—Ru1—Ru2—C14 | −139.18 (12) | C26—Ru2—C14—Si2 | 53.9 (2) |
C24—Ru1—Ru2—C25 | 21.15 (16) | C26—Ru2—C14—C10 | 174.1 (2) |
C24—Ru1—Ru2—C26 | 110.23 (16) | C26—Ru2—C14—C13 | −70.8 (2) |
Ru2—Ru1—C1—Si1 | −36.22 (17) | C10—Si1—C1—Ru1 | 54.0 (2) |
Ru2—Ru1—C1—C2 | 83.4 (2) | C10—Si1—C1—C2 | −29.0 (3) |
Ru2—Ru1—C1—C5 | −162.10 (15) | C10—Si1—C1—C5 | 138.2 (3) |
C2—Ru1—C1—Si1 | −119.6 (3) | C19—Si1—C1—Ru1 | 172.57 (18) |
C2—Ru1—C1—C5 | 114.5 (3) | C19—Si1—C1—C2 | 89.6 (3) |
C3—Ru1—C1—Si1 | −156.5 (2) | C19—Si1—C1—C5 | −103.3 (3) |
C3—Ru1—C1—C2 | −36.8 (2) | C20—Si1—C1—Ru1 | −64.1 (2) |
C3—Ru1—C1—C5 | 77.66 (19) | C20—Si1—C1—C2 | −147.1 (2) |
C4—Ru1—C1—Si1 | 161.5 (2) | C20—Si1—C1—C5 | 20.0 (3) |
C4—Ru1—C1—C2 | −78.9 (2) | C1—Si1—C10—Ru2 | −48.10 (19) |
C4—Ru1—C1—C5 | 35.65 (17) | C1—Si1—C10—C11 | −136.7 (3) |
C5—Ru1—C1—Si1 | 125.9 (2) | C1—Si1—C10—C14 | 35.8 (3) |
C5—Ru1—C1—C2 | −114.5 (3) | C19—Si1—C10—Ru2 | −167.21 (17) |
C23—Ru1—C1—Si1 | −133.5 (4) | C19—Si1—C10—C11 | 104.2 (3) |
C23—Ru1—C1—C2 | −13.9 (6) | C19—Si1—C10—C14 | −83.4 (3) |
C23—Ru1—C1—C5 | 100.7 (5) | C20—Si1—C10—Ru2 | 71.9 (2) |
C24—Ru1—C1—Si1 | 53.5 (2) | C20—Si1—C10—C11 | −16.7 (4) |
C24—Ru1—C1—C2 | 173.1 (2) | C20—Si1—C10—C14 | 155.7 (3) |
C24—Ru1—C1—C5 | −72.4 (2) | C14—Si2—C2—Ru1 | −47.3 (2) |
Ru2—Ru1—C2—Si2 | 21.74 (17) | C14—Si2—C2—C1 | 37.6 (3) |
Ru2—Ru1—C2—C1 | −96.7 (2) | C14—Si2—C2—C3 | −137.5 (3) |
Ru2—Ru1—C2—C3 | 146.33 (16) | C21—Si2—C2—Ru1 | 70.9 (2) |
C1—Ru1—C2—Si2 | 118.5 (3) | C21—Si2—C2—C1 | 155.9 (2) |
C1—Ru1—C2—C3 | −117.0 (3) | C21—Si2—C2—C3 | −19.2 (3) |
C3—Ru1—C2—Si2 | −124.6 (2) | C22—Si2—C2—Ru1 | −167.09 (18) |
C3—Ru1—C2—C1 | 117.0 (3) | C22—Si2—C2—C1 | −82.2 (3) |
C4—Ru1—C2—Si2 | −161.0 (2) | C22—Si2—C2—C3 | 102.8 (3) |
C4—Ru1—C2—C1 | 80.6 (2) | C2—Si2—C14—Ru2 | 52.36 (17) |
C4—Ru1—C2—C3 | −36.36 (17) | C2—Si2—C14—C10 | −30.9 (3) |
C5—Ru1—C2—Si2 | 157.4 (2) | C2—Si2—C14—C13 | 136.4 (3) |
C5—Ru1—C2—C1 | 38.9 (2) | C21—Si2—C14—Ru2 | −67.4 (2) |
C5—Ru1—C2—C3 | −78.1 (2) | C21—Si2—C14—C10 | −150.7 (3) |
C23—Ru1—C2—Si2 | −67.2 (3) | C21—Si2—C14—C13 | 16.6 (4) |
C23—Ru1—C2—C1 | 174.3 (2) | C22—Si2—C14—Ru2 | 169.62 (17) |
C23—Ru1—C2—C3 | 57.4 (3) | C22—Si2—C14—C10 | 86.3 (3) |
C24—Ru1—C2—Si2 | 106.5 (3) | C22—Si2—C14—C13 | −106.3 (3) |
C24—Ru1—C2—C1 | −11.9 (4) | Ru1—C1—C2—Si2 | −113.5 (2) |
C24—Ru1—C2—C3 | −128.9 (3) | Ru1—C1—C2—C3 | 62.5 (2) |
Ru2—Ru1—C3—C2 | −38.75 (18) | Si1—C1—C2—Ru1 | 105.9 (2) |
Ru2—Ru1—C3—C4 | −158.25 (17) | Si1—C1—C2—Si2 | −7.6 (4) |
C1—Ru1—C3—C2 | 38.41 (19) | Si1—C1—C2—C3 | 168.4 (2) |
C1—Ru1—C3—C4 | −81.1 (2) | C5—C1—C2—Ru1 | −63.8 (2) |
C2—Ru1—C3—C4 | −119.5 (3) | C5—C1—C2—Si2 | −177.3 (2) |
C4—Ru1—C3—C2 | 119.5 (3) | C5—C1—C2—C3 | −1.3 (3) |
C5—Ru1—C3—C2 | 81.4 (2) | Ru1—C1—C5—C4 | −62.4 (2) |
C5—Ru1—C3—C4 | −38.1 (2) | Si1—C1—C5—Ru1 | −104.6 (2) |
C23—Ru1—C3—C2 | −133.6 (2) | Si1—C1—C5—C4 | −167.0 (2) |
C23—Ru1—C3—C4 | 106.9 (2) | C2—C1—C5—Ru1 | 64.29 (19) |
C24—Ru1—C3—C2 | 117.0 (3) | C2—C1—C5—C4 | 1.9 (3) |
C24—Ru1—C3—C4 | −2.5 (4) | Ru1—C2—C3—C4 | 61.5 (2) |
Ru2—Ru1—C4—C3 | 41.2 (3) | Si2—C2—C3—Ru1 | 114.5 (2) |
Ru2—Ru1—C4—C5 | −74.2 (3) | Si2—C2—C3—C4 | 176.0 (2) |
Ru2—Ru1—C4—C6 | 162.69 (17) | C1—C2—C3—Ru1 | −61.20 (19) |
C1—Ru1—C4—C3 | 78.8 (2) | C1—C2—C3—C4 | 0.3 (3) |
C1—Ru1—C4—C5 | −36.5 (2) | Ru1—C3—C4—C5 | 62.4 (2) |
C1—Ru1—C4—C6 | −159.6 (3) | Ru1—C3—C4—C6 | −125.3 (3) |
C2—Ru1—C4—C3 | 35.78 (18) | C2—C3—C4—Ru1 | −61.6 (2) |
C2—Ru1—C4—C5 | −79.6 (2) | C2—C3—C4—C5 | 0.9 (3) |
C2—Ru1—C4—C6 | 157.3 (3) | C2—C3—C4—C6 | 173.2 (3) |
C3—Ru1—C4—C5 | −115.4 (3) | Ru1—C4—C5—C1 | 61.3 (2) |
C3—Ru1—C4—C6 | 121.5 (3) | C3—C4—C5—Ru1 | −63.0 (2) |
C5—Ru1—C4—C3 | 115.4 (3) | C3—C4—C5—C1 | −1.7 (3) |
C5—Ru1—C4—C6 | −123.1 (4) | C6—C4—C5—Ru1 | 124.9 (3) |
C23—Ru1—C4—C3 | −81.7 (2) | C6—C4—C5—C1 | −173.9 (3) |
C23—Ru1—C4—C5 | 163.0 (2) | Ru1—C4—C6—C7 | −56.1 (3) |
C23—Ru1—C4—C6 | 39.8 (3) | Ru1—C4—C6—C8 | −175.0 (2) |
C24—Ru1—C4—C3 | 178.7 (2) | Ru1—C4—C6—C9 | 65.3 (3) |
C24—Ru1—C4—C5 | 63.3 (3) | C3—C4—C6—C7 | 38.4 (4) |
C24—Ru1—C4—C6 | −59.8 (3) | C3—C4—C6—C8 | −80.4 (3) |
Ru2—Ru1—C5—C1 | 22.90 (19) | C3—C4—C6—C9 | 159.9 (3) |
Ru2—Ru1—C5—C4 | 142.6 (2) | C5—C4—C6—C7 | −150.9 (3) |
C1—Ru1—C5—C4 | 119.7 (3) | C5—C4—C6—C8 | 90.3 (4) |
C2—Ru1—C5—C1 | −39.40 (18) | C5—C4—C6—C9 | −29.4 (4) |
C2—Ru1—C5—C4 | 80.3 (2) | Ru2—C10—C11—C12 | 61.4 (2) |
C3—Ru1—C5—C1 | −81.12 (19) | Si1—C10—C11—Ru2 | 111.8 (3) |
C3—Ru1—C5—C4 | 38.6 (2) | Si1—C10—C11—C12 | 173.3 (3) |
C4—Ru1—C5—C1 | −119.7 (3) | C14—C10—C11—Ru2 | −61.6 (2) |
C23—Ru1—C5—C1 | −146.4 (2) | C14—C10—C11—C12 | −0.2 (4) |
C23—Ru1—C5—C4 | −26.7 (3) | Ru2—C10—C14—Si2 | 106.1 (3) |
C24—Ru1—C5—C1 | 115.2 (2) | Ru2—C10—C14—C13 | −63.6 (2) |
C24—Ru1—C5—C4 | −125.1 (3) | Si1—C10—C14—Ru2 | −111.1 (3) |
Ru1—Ru2—C10—Si1 | 22.01 (14) | Si1—C10—C14—Si2 | −5.0 (4) |
Ru1—Ru2—C10—C11 | 146.93 (18) | Si1—C10—C14—C13 | −174.7 (2) |
Ru1—Ru2—C10—C14 | −96.51 (18) | C11—C10—C14—Ru2 | 62.7 (2) |
C11—Ru2—C10—Si1 | −124.9 (3) | C11—C10—C14—Si2 | 168.8 (2) |
C11—Ru2—C10—C14 | 116.6 (3) | C11—C10—C14—C13 | −0.9 (4) |
C12—Ru2—C10—Si1 | −161.1 (2) | Ru2—C11—C12—C13 | 62.7 (2) |
C12—Ru2—C10—C11 | −36.22 (18) | Ru2—C11—C12—C15 | −124.2 (4) |
C12—Ru2—C10—C14 | 80.3 (2) | C10—C11—C12—Ru2 | −61.6 (2) |
C13—Ru2—C10—Si1 | 156.8 (2) | C10—C11—C12—C13 | 1.1 (4) |
C13—Ru2—C10—C11 | −78.3 (2) | C10—C11—C12—C15 | 174.2 (3) |
C13—Ru2—C10—C14 | 38.31 (19) | Ru2—C12—C13—C14 | 61.6 (3) |
C14—Ru2—C10—Si1 | 118.5 (3) | C11—C12—C13—Ru2 | −63.3 (2) |
C14—Ru2—C10—C11 | −116.6 (3) | C11—C12—C13—C14 | −1.7 (4) |
C25—Ru2—C10—Si1 | −66.2 (2) | C15—C12—C13—Ru2 | 123.5 (3) |
C25—Ru2—C10—C11 | 58.7 (3) | C15—C12—C13—C14 | −174.9 (3) |
C25—Ru2—C10—C14 | 175.3 (2) | Ru2—C12—C15—C16 | 63.2 (4) |
C26—Ru2—C10—Si1 | 108.0 (3) | Ru2—C12—C15—C17 | −176.4 (2) |
C26—Ru2—C10—C11 | −127.1 (3) | Ru2—C12—C15—C18 | −57.5 (3) |
C26—Ru2—C10—C14 | −10.5 (4) | C11—C12—C15—C16 | 158.5 (4) |
Ru1—Ru2—C11—C10 | −38.5 (2) | C11—C12—C15—C17 | −81.0 (4) |
Ru1—Ru2—C11—C12 | −158.30 (14) | C11—C12—C15—C18 | 37.8 (5) |
C10—Ru2—C11—C12 | −119.8 (3) | C13—C12—C15—C16 | −29.7 (5) |
C12—Ru2—C11—C10 | 119.8 (3) | C13—C12—C15—C17 | 90.7 (4) |
C13—Ru2—C11—C10 | 81.06 (19) | C13—C12—C15—C18 | −150.4 (3) |
C13—Ru2—C11—C12 | −38.71 (17) | Ru2—C13—C14—Si2 | −105.2 (3) |
C14—Ru2—C11—C10 | 38.53 (18) | Ru2—C13—C14—C10 | 64.0 (2) |
C14—Ru2—C11—C12 | −81.23 (18) | C12—C13—C14—Ru2 | −62.3 (2) |
C25—Ru2—C11—C10 | −133.0 (2) | C12—C13—C14—Si2 | −167.5 (3) |
C25—Ru2—C11—C12 | 107.2 (2) | C12—C13—C14—C10 | 1.6 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
C20—H20A···O2i | 0.98 | 2.60 | 3.571 (5) | 171 |
Symmetry code: (i) −x+1, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | [Ru2(C22H34Si2)(CO)4] |
Mr | 668.85 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 173 |
a, b, c (Å) | 10.632 (3), 10.886 (3), 14.546 (5) |
α, β, γ (°) | 89.518 (5), 71.581 (4), 61.560 (4) |
V (Å3) | 1384.0 (7) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.21 |
Crystal size (mm) | 0.17 × 0.16 × 0.15 |
Data collection | |
Diffractometer | Bruker APEXII CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2005) |
Tmin, Tmax | 0.821, 0.840 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6921, 4802, 4101 |
Rint | 0.029 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.032, 0.077, 1.04 |
No. of reflections | 4802 |
No. of parameters | 317 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.92, −0.86 |
Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
C20—H20A···O2i | 0.98 | 2.60 | 3.571 (5) | 171 |
Symmetry code: (i) −x+1, −y, −z. |
Recently, a series of reactions of doubly-bridged ligand precursors (C5H4(E))(C5H4(E')) (E, E' = CH2, CMe2, SiMe2, or GeMe2) with Ru3(CO)12 have been reported by the group of Professor Angelici (Ovchinnikov et al., 2002) and our groups (Zhu et al., 2012), which generally afforded the corresponding doubly-bridged bis(cyclopentadienyl) dinuclear complex containing an elongated Ru—Ru bond. To develop a deeper understanding of the relationship between the structure of the ligand and the Ru—Ru bond distance, and make a comparison of the Ru—Ru bond distance with those in the respective non-bridged and singly-bridged bis(cyclopentadienyl) ruthenium analogues, we carried out the reaction of the doubly-bridged ligand precursor (tBuC5H3)2(SiMe2)2 with Ru3(CO)12 in refluxing xylene, which afforded the expected title product whose crystal structure we report on herein.
The molecular structure of title compound is presented in Fig. 1. It has approximate C2v symmetry, as reflected in the small torsion angle DCp(centroid)–Ru1–Ru2–Cp(centroid) (ca. 15.8°). The dihedral angle between the planes of the Cp rings of the (η5-C5H2tBu)2(SiMe2)2 ligand is rather large, 123.13 (19) °, which results in a longer than normal Ru1–Ru2 single bond distance of 2.8401 (7) Å, longer than that [2.8180 (3) Å] in its parent complex [(η5-C5H3)2(SiMe2)2]Ru2(CO)4 (Ovchinnikov et al., 2002). Therefore, the two tBu substituents on title compound have considerable effect on the geometry of the system.
The elongated Ru—Ru distance makes CO bridging unfavorable. This situation is similar to that in other doubly-bridged analogues, for example 2.8420 (8) Å in [(η5-C5H3)2(CMe2)(SiMe2)]Ru2(CO)4, 2.824 (1) Å in [(η5-C5H3)2(CMe2)(GeMe2)]Ru2(CO)4, 2.8382 (9) Å in [(η5-C5H3)2(CH2)(SiMe2)]Ru2(CO)4, 2.8429 (7) Å in [(η5-C5H3)2(CH2)(GeMe2)]Ru2(CO)4 (Zhu et al., 2012), and 2.821 (1) Å in the fulvalene diruthenium carbonyl complex (η5:η5-C10H8)Ru2(CO)4 (Boese et al., 1997).
Generally, due to the rigid structure of the doubly-bridged ligand, the Ru—Ru bond distances in the above-mentioned complexes are obviously longer than those in the respective non-bridged and singly-bridged analogues, for example 2.735 (2) Å in trans-[(η5-C5H5)Ru(CO)(µ-CO)]2 (Mills et al., 1967), 2.7879 (4) Å in (CMe2)[(η5-C5H4)Ru(CO)2]2 (Burger, 2001), or 2.705 Å in (SiMe2)[(η5-C5H4)Ru(CO)(µ-CO)]2 (Zhou et al., 1997; Bitterwolf et al., 1996).