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In the title compound, [Ru2(C10H15)2(C22H18)], the four five-membered rings are approximately eclipsed. The distances from these rings to the corresponding Ru atoms are 1.795 (1) and 1.798 (1) Å for the Cp*, and 1.835 (1) and 1.842 (1) Å for the indenyl five-membered rings.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803001673/bt6233sup1.cif
Contains datablocks 3, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803001673/bt62333sup2.hkl
Contains datablock 3

CCDC reference: 204665

Key indicators

  • Single-crystal X-ray study
  • T = 178 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.028
  • wR factor = 0.071
  • Data-to-parameter ratio = 14.7

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ADDSYM reports no extra symmetry








Comment top

Having prepared and studied various metal complexes of anti-[2.2]indenophanes (Hopf & Dannheim, 1988), we have now prepared ruthenium complexes of syn-[2.2]indenophane, (1). Whereas with the former ligands the metal atoms are oriented in a stepwise fashion, in (1), they were expected to be oriented above each other (eclipsed). Here we present the structure of the doubly-capped ruthenium complex, (3).

The molecule of (3) is shown in Fig. 1. In the following discussion, the rings are defined as ring 1 for atoms C19–C23, ring 2 for C3A/C4/C5/C6/C6A, ring 3 for C12A/C13/C14/C15/C14A, and ring 4 for C19'–C23'; the corresponding centroids are denoted Cent1, Cent2, etc.

The Ru atoms lie 1.795 (1), 1.835 (1), 1.842 (1) and 1.798 (1) Å from the ring planes 1–4, respectively. The general form of the molecule is as expected, in that the four five-membered rings are essentially eclipsed, but there are some deviations from the idealized form (Fig. 2). The sequence Cent1—Ru1—Cent2···Cent3—Ru2—Cent4 is significantly bent at Cent3 (171°), and rings 2 and 3 of the central indenophane ligand are splayed away from each other [interplanar angle 10.92 (4)°]. The distance Cent2···Cent3 is 3.30 Å.

The six-membered rings display the usual flattened boat conformation, in which the bridgehead atoms C3, C7, C12 and C16 lie 0.151 (4), 0.142 (4), 0.149 (4) and 0.151 (4) Å, respectively, out of the plane of the four other atoms; the interplanar angle between the four-atom planes is 1.90 (2)°, and the distance between the corresponding centroids is 3.08 Å.

Experimental top

Hydrocarbon (1) was monometalated using methyl lithium in THF at 233 K. The mixture was stirred for 30 min at 273 K and the pentamethylcyclopentadienyl ruthenium chloride tetramer was then added. Reaction was complete after 1 h at room temperature. The solvent was removed in vacuo and the remaining solid recrystallized from hexane; the monoruthenium complex, (2), was isolated in 92% yield as yellow needles and characterized by spectroscopic and analytical data. Repetition of the reaction sequence furnished the bis-ruthenium complex, (3), as yellow prisms in 91% yield. Spectroscopic data are again in full accord with the structural assignment. For full details, see Hartig (1991).

Refinement top

Methyl H atoms were identified in difference syntheses, idealized and then refined using rigid methyl groups allowed to rotate but not tip. Other H atoms were included using a riding model, with fixed C—H bond lengths (aromatic C—H = 0.95 Å, and methyl and methylene C—H = 0.99 Å); Uiso(H) values were fixed at 1.2Ueq of the parent atom.

Computing details top

Data collection: P3 (Nicolet, 1987); cell refinement: P3; data reduction: XDISK (Nicolet, 1987); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecule of compound (3) in the crystal. Ellipsoids are shown at the 30% probability level. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. Alternative view of compound (3), perpendicular to the plane of ring C19–23. Radii are arbitrary.
Bis(η5-pentamethylcyclopentadienyl)[bis-η5-syn- [2.2](4,7)indenophanyl]diruthenium(II) top
Crystal data top
[Ru2(C10H15)2(C22H18)]F(000) = 1552
Mr = 754.94Dx = 1.473 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 8.647 (2) ÅCell parameters from 50 reflections
b = 13.604 (4) Åθ = 10–11.5°
c = 28.959 (8) ŵ = 0.92 mm1
β = 92.41 (2)°T = 178 K
V = 3403.5 (16) Å3Prism, yellow
Z = 40.7 × 0.4 × 0.15 mm
Data collection top
Nicolet R3
diffractometer
5079 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.020
Graphite monochromatorθmax = 25.0°, θmin = 3.1°
ω–2θ scansh = 010
Absorption correction: part of the refinement model (ΔF)
(DIFABS; Walker & Stuart, 1983)
k = 1610
Tmin = 0.66, Tmax = 0.84l = 3434
11146 measured reflections3 standard reflections every 147 reflections
5984 independent reflections intensity decay: none
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.071H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0398P)2 + 1.6478P]
where P = (Fo2 + 2Fc2)/3
5984 reflections(Δ/σ)max = 0.002
407 parametersΔρmax = 0.42 e Å3
0 restraintsΔρmin = 0.61 e Å3
Crystal data top
[Ru2(C10H15)2(C22H18)]V = 3403.5 (16) Å3
Mr = 754.94Z = 4
Monoclinic, P21/cMo Kα radiation
a = 8.647 (2) ŵ = 0.92 mm1
b = 13.604 (4) ÅT = 178 K
c = 28.959 (8) Å0.7 × 0.4 × 0.15 mm
β = 92.41 (2)°
Data collection top
Nicolet R3
diffractometer
5079 reflections with I > 2σ(I)
Absorption correction: part of the refinement model (ΔF)
(DIFABS; Walker & Stuart, 1983)
Rint = 0.020
Tmin = 0.66, Tmax = 0.843 standard reflections every 147 reflections
11146 measured reflections intensity decay: none
5984 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.071H-atom parameters constrained
S = 1.05Δρmax = 0.42 e Å3
5984 reflectionsΔρmin = 0.61 e Å3
407 parameters
Special details top

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.

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

− 0.2007 (0.0124) x + 1.9710 (0.0193) y + 28.6485 (0.0117) z = 3.1397 (0.0043)

* 0.0024 (0.0018) C19 * −0.0041 (0.0018) C20 * 0.0042 (0.0017) C21 * −0.0027 (0.0018) C22 * 0.0003 (0.0018) C23 1.7952 (0.0014) Ru1

Rms deviation of fitted atoms = 0.0031

− 0.0177 (0.0118) x + 1.4424 (0.0176) y + 28.7727 (0.0109) z = 6.7179 (0.0045)

Angle to previous plane (with approximate e.s.d.) = 2.55 (0.05)

* 0.0089 (0.0016) C3A * −0.0115 (0.0016) C4 * 0.0097 (0.0017) C5 * −0.0041 (0.0017) C6 * −0.0029 (0.0016) C6A −1.8353 (0.0013) Ru1

Rms deviation of fitted atoms = 0.0082

− 0.3566 (0.0121) x − 1.0905 (0.0185) y + 28.8658 (0.0106) z = 9.3512 (0.0071)

Angle to previous plane (with approximate e.s.d.) = 10.92 (0.04)

* −0.0018 (0.0017) C12A * 0.0070 (0.0018) C13 * −0.0096 (0.0018) C14 * 0.0083 (0.0018) C15 * −0.0040 (0.0017) C15A 1.8416 (0.0014) Ru2

Rms deviation of fitted atoms = 0.0068

− 0.2139 (0.0124) x − 1.6263 (0.0186) y + 28.7471 (0.0111) z = 12.8521 (0.0082)

Angle to previous plane (with approximate e.s.d.) = 2.45 (0.05)

* −0.0033 (0.0017) C19' * 0.0019 (0.0017) C20' * 0.0002 (0.0018) C21' * −0.0022 (0.0018) C22' * 0.0034 (0.0017) C23' −1.7978 (0.0014) Ru2

Rms deviation of fitted atoms = 0.0025

− 0.1351 (0.0147) x + 0.4123 (0.0169) y + 28.9356 (0.0102) z = 6.5725 (0.0030)

Angle to previous plane (with approximate e.s.d.) = 8.62 (0.04)

* −0.0086 (0.0013) C3A * 0.0086 (0.0013) C6A * −0.0088 (0.0013) C8 * 0.0087 (0.0013) C9 0.1512 (0.0039) C3 0.1421 (0.0040) C7

Rms deviation of fitted atoms = 0.0087

− 0.1316 (0.0152) x − 0.0392 (0.0175) y + 28.9484 (0.0102) z = 9.6061 (0.0041)

Angle to previous plane (with approximate e.s.d.) = 1.90 (0.02)

* −0.0044 (0.0013) C12A * 0.0044 (0.0013) C15A * −0.0045 (0.0014) C17 * 0.0045 (0.0014) C18 − 0.1487 (0.0042) C12 − 0.1506 (0.0040) C16

Rms deviation of fitted atoms = 0.0044

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*/Ueq
Ru10.21577 (3)0.211206 (16)0.159240 (7)0.01877 (7)
Ru20.24087 (3)0.234186 (17)0.399575 (7)0.02075 (7)
C10.1676 (3)0.1775 (3)0.30503 (10)0.0322 (7)
H1A0.17740.24780.31330.039*
H1B0.25540.14190.31820.039*
C20.1789 (3)0.1672 (2)0.25058 (10)0.0261 (6)
H2A0.26930.12560.24180.031*
H2B0.19710.23310.23690.031*
C30.0370 (3)0.1233 (2)0.23044 (9)0.0202 (6)
C3A0.0977 (3)0.1825 (2)0.22470 (8)0.0172 (5)
C40.1177 (3)0.2861 (2)0.21881 (9)0.0205 (6)
H40.03720.33340.21560.025*
C50.2790 (3)0.3059 (2)0.21866 (9)0.0256 (7)
H50.32460.36910.21620.031*
C60.3611 (3)0.2155 (2)0.22276 (9)0.0241 (6)
H60.47040.20790.22290.029*
C6A0.2501 (3)0.1373 (2)0.22665 (9)0.0202 (6)
C70.2647 (3)0.0334 (2)0.23281 (9)0.0234 (6)
C80.1322 (4)0.0204 (2)0.22775 (9)0.0252 (6)
H80.13980.08970.22460.030*
C90.0179 (3)0.0238 (2)0.22702 (9)0.0235 (6)
H90.10680.01710.22410.028*
C100.4115 (4)0.0097 (2)0.25436 (11)0.0318 (7)
H10A0.50140.01990.23950.038*
H10B0.41300.08120.24820.038*
C110.4287 (4)0.0076 (3)0.30785 (12)0.0424 (9)
H11A0.45190.05600.32330.051*
H11B0.51770.05200.31450.051*
C120.2859 (4)0.0516 (2)0.32807 (10)0.0279 (7)
C12A0.2690 (3)0.1563 (2)0.33312 (9)0.0240 (6)
C130.3779 (4)0.2356 (3)0.33777 (10)0.0311 (7)
H130.48740.22910.33940.037*
C140.2947 (4)0.3256 (3)0.33956 (10)0.0339 (7)
H140.33920.38940.34180.041*
C150.1340 (4)0.3041 (2)0.33739 (9)0.0281 (7)
H150.05270.35080.33870.034*
C15A0.1153 (3)0.1995 (2)0.33278 (9)0.0217 (6)
C160.0177 (3)0.1380 (2)0.32674 (9)0.0238 (6)
C170.0052 (4)0.0390 (2)0.33176 (9)0.0275 (7)
H170.08200.00270.33470.033*
C180.1557 (4)0.0032 (2)0.33269 (10)0.0297 (7)
H180.16580.07230.33670.036*
C190.2579 (4)0.2760 (2)0.09249 (10)0.0310 (7)
C200.1001 (4)0.2469 (2)0.09317 (9)0.0259 (6)
C210.0946 (3)0.1428 (2)0.10058 (9)0.0239 (6)
C220.2515 (3)0.1071 (2)0.10389 (10)0.0276 (7)
C230.3524 (4)0.1892 (3)0.09906 (10)0.0322 (7)
C240.3159 (5)0.3778 (3)0.08325 (11)0.0502 (10)
H24A0.42150.38490.09650.060*
H24B0.24830.42600.09740.060*
H24C0.31580.38900.04980.060*
C250.0383 (4)0.3115 (3)0.08402 (11)0.0412 (8)
H25A0.06810.30970.05100.049*
H25B0.01270.37910.09310.049*
H25C0.12450.28790.10190.049*
C260.0495 (4)0.0825 (2)0.10334 (11)0.0339 (7)
H26A0.12930.12100.11810.041*
H26B0.02690.02310.12160.041*
H26C0.08650.06390.07210.041*
C270.2979 (4)0.0014 (3)0.10996 (12)0.0426 (9)
H27A0.29650.03100.07970.051*
H27B0.22520.03170.12980.051*
H27C0.40250.00210.12430.051*
C280.5257 (4)0.1859 (4)0.09858 (13)0.0575 (11)
H28A0.56420.13060.11740.069*
H28B0.56850.24750.11120.069*
H28C0.55760.17760.06670.069*
C19'0.1257 (3)0.1701 (2)0.45752 (9)0.0234 (6)
C20'0.1327 (4)0.2747 (2)0.46367 (10)0.0261 (7)
C21'0.2919 (4)0.3033 (2)0.46641 (9)0.0271 (7)
C22'0.3850 (4)0.2157 (2)0.46206 (10)0.0274 (7)
C23'0.2813 (4)0.1335 (2)0.45684 (9)0.0264 (6)
C24'0.0181 (4)0.1090 (2)0.45310 (11)0.0336 (7)
H24D0.03880.07950.48310.040*
H24E0.00410.05680.43030.040*
H24F0.10570.15060.44300.040*
C25'0.0034 (4)0.3412 (2)0.46980 (11)0.0369 (8)
H25D0.02940.34190.50240.044*
H25E0.09230.31710.45100.044*
H25F0.02270.40790.46000.044*
C26'0.3520 (4)0.4051 (2)0.47592 (11)0.0378 (8)
H26D0.28310.45320.46050.045*
H26E0.45620.41150.46410.045*
H26F0.35610.41720.50930.045*
C27'0.5576 (4)0.2111 (3)0.46530 (13)0.0448 (9)
H27D0.59250.19990.49750.054*
H27E0.60030.27330.45450.054*
H27F0.59320.15710.44600.054*
C28'0.3259 (4)0.0278 (2)0.45288 (11)0.0354 (8)
H28D0.43320.02320.44340.042*
H28E0.25730.00450.42980.042*
H28F0.31660.00460.48290.042*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.01803 (12)0.01958 (12)0.01875 (12)0.00265 (9)0.00121 (9)0.00049 (8)
Ru20.02073 (13)0.02264 (13)0.01883 (12)0.00141 (9)0.00025 (9)0.00011 (9)
C10.0190 (15)0.044 (2)0.0335 (16)0.0009 (14)0.0049 (13)0.0052 (14)
C20.0158 (14)0.0326 (17)0.0300 (15)0.0002 (12)0.0008 (12)0.0019 (13)
C30.0169 (14)0.0253 (15)0.0181 (13)0.0024 (11)0.0021 (11)0.0019 (11)
C3A0.0163 (13)0.0197 (14)0.0156 (12)0.0002 (11)0.0009 (10)0.0006 (10)
C40.0252 (15)0.0177 (14)0.0186 (13)0.0001 (12)0.0010 (11)0.0001 (10)
C50.0278 (16)0.0256 (16)0.0232 (14)0.0121 (13)0.0002 (12)0.0004 (12)
C60.0173 (14)0.0316 (17)0.0232 (14)0.0043 (12)0.0016 (11)0.0023 (12)
C6A0.0157 (14)0.0282 (16)0.0166 (13)0.0016 (12)0.0002 (11)0.0015 (11)
C70.0260 (16)0.0250 (15)0.0194 (13)0.0064 (12)0.0033 (12)0.0021 (11)
C80.0375 (18)0.0179 (14)0.0205 (14)0.0005 (13)0.0045 (12)0.0000 (11)
C90.0239 (15)0.0235 (15)0.0227 (14)0.0082 (12)0.0027 (12)0.0008 (11)
C100.0270 (17)0.0339 (18)0.0349 (17)0.0116 (14)0.0057 (14)0.0045 (13)
C110.0325 (19)0.055 (2)0.0390 (19)0.0213 (17)0.0116 (15)0.0152 (16)
C120.0307 (17)0.0326 (17)0.0201 (14)0.0115 (14)0.0039 (12)0.0033 (12)
C12A0.0209 (15)0.0360 (17)0.0151 (13)0.0007 (13)0.0013 (11)0.0026 (12)
C130.0228 (16)0.048 (2)0.0224 (14)0.0069 (14)0.0034 (12)0.0036 (14)
C140.044 (2)0.0337 (18)0.0242 (15)0.0143 (15)0.0007 (14)0.0019 (13)
C150.0400 (18)0.0249 (16)0.0190 (13)0.0010 (14)0.0019 (13)0.0020 (12)
C15A0.0230 (15)0.0255 (15)0.0167 (13)0.0020 (12)0.0007 (11)0.0005 (11)
C160.0227 (15)0.0308 (16)0.0182 (13)0.0001 (12)0.0047 (11)0.0021 (12)
C170.0291 (17)0.0316 (17)0.0220 (14)0.0085 (13)0.0040 (12)0.0002 (12)
C180.0439 (19)0.0238 (16)0.0212 (15)0.0039 (14)0.0003 (13)0.0005 (12)
C190.0423 (19)0.0333 (17)0.0177 (14)0.0113 (15)0.0035 (13)0.0016 (12)
C200.0373 (17)0.0220 (15)0.0183 (13)0.0001 (13)0.0020 (12)0.0021 (11)
C210.0273 (16)0.0259 (16)0.0183 (13)0.0015 (13)0.0003 (12)0.0027 (11)
C220.0285 (16)0.0319 (17)0.0225 (14)0.0046 (13)0.0037 (12)0.0055 (12)
C230.0271 (17)0.047 (2)0.0231 (15)0.0052 (15)0.0087 (13)0.0031 (14)
C240.077 (3)0.046 (2)0.0278 (17)0.033 (2)0.0046 (18)0.0046 (15)
C250.054 (2)0.0330 (19)0.0359 (18)0.0146 (17)0.0123 (16)0.0040 (14)
C260.0343 (18)0.0336 (18)0.0335 (17)0.0132 (15)0.0015 (14)0.0082 (14)
C270.051 (2)0.038 (2)0.0391 (19)0.0177 (17)0.0055 (17)0.0063 (15)
C280.029 (2)0.095 (3)0.050 (2)0.010 (2)0.0164 (17)0.008 (2)
C19'0.0293 (16)0.0229 (15)0.0181 (13)0.0017 (13)0.0026 (12)0.0024 (11)
C20'0.0335 (17)0.0244 (16)0.0206 (14)0.0042 (13)0.0033 (12)0.0031 (11)
C21'0.0354 (18)0.0274 (16)0.0183 (13)0.0025 (14)0.0026 (12)0.0006 (12)
C22'0.0284 (16)0.0299 (17)0.0234 (14)0.0023 (13)0.0056 (12)0.0001 (12)
C23'0.0325 (17)0.0267 (16)0.0197 (14)0.0037 (13)0.0015 (12)0.0026 (12)
C24'0.0352 (18)0.0320 (18)0.0342 (17)0.0059 (14)0.0093 (14)0.0029 (14)
C25'0.044 (2)0.0310 (18)0.0362 (17)0.0116 (15)0.0102 (15)0.0046 (14)
C26'0.052 (2)0.0306 (18)0.0299 (17)0.0077 (16)0.0061 (15)0.0034 (13)
C27'0.0293 (19)0.058 (2)0.047 (2)0.0002 (17)0.0090 (16)0.0019 (17)
C28'0.043 (2)0.0269 (17)0.0359 (17)0.0111 (15)0.0006 (15)0.0007 (14)
Geometric parameters (Å, º) top
Ru1—C232.167 (3)C15—C15A1.438 (4)
Ru1—C212.168 (3)C15—H150.9500
Ru1—C192.169 (3)C15A—C161.428 (4)
Ru1—C222.171 (3)C16—C171.367 (4)
Ru1—C202.176 (3)C17—C181.422 (4)
Ru1—C62.185 (3)C17—H170.9500
Ru1—C52.200 (3)C18—H180.9500
Ru1—C42.204 (3)C19—C201.422 (4)
Ru1—C6A2.205 (3)C19—C231.444 (5)
Ru1—C3A2.225 (3)C19—C241.500 (4)
Ru2—C23'2.168 (3)C20—C211.433 (4)
Ru2—C22'2.168 (3)C20—C251.499 (4)
Ru2—C19'2.170 (3)C21—C221.441 (4)
Ru2—C21'2.180 (3)C21—C261.497 (4)
Ru2—C20'2.184 (3)C22—C231.428 (4)
Ru2—C132.188 (3)C22—C271.501 (4)
Ru2—C142.203 (3)C23—C281.500 (4)
Ru2—C152.205 (3)C24—H24A0.9800
Ru2—C12A2.219 (3)C24—H24B0.9800
Ru2—C15A2.228 (3)C24—H24C0.9800
C1—C161.515 (4)C25—H25A0.9800
C1—C21.582 (4)C25—H25B0.9800
C1—H1A0.9900C25—H25C0.9800
C1—H1B0.9900C26—H26A0.9800
C2—C31.504 (4)C26—H26B0.9800
C2—H2A0.9900C26—H26C0.9800
C2—H2B0.9900C27—H27A0.9800
C3—C91.368 (4)C27—H27B0.9800
C3—C3A1.431 (4)C27—H27C0.9800
C3A—C41.430 (4)C28—H28A0.9800
C3A—C6A1.454 (4)C28—H28B0.9800
C4—C51.421 (4)C28—H28C0.9800
C4—H40.9500C19'—C20'1.435 (4)
C5—C61.423 (4)C19'—C23'1.436 (4)
C5—H50.9500C19'—C24'1.497 (4)
C6—C6A1.440 (4)C20'—C21'1.430 (4)
C6—H60.9500C20'—C25'1.500 (4)
C6A—C71.430 (4)C21'—C22'1.446 (4)
C7—C81.362 (4)C21'—C26'1.501 (4)
C7—C101.509 (4)C22'—C23'1.437 (4)
C8—C91.430 (4)C22'—C27'1.493 (4)
C8—H80.9500C23'—C28'1.495 (4)
C9—H90.9500C24'—H24D0.9800
C10—C111.568 (4)C24'—H24E0.9800
C10—H10A0.9900C24'—H24F0.9800
C10—H10B0.9900C25'—H25D0.9800
C11—C121.512 (4)C25'—H25E0.9800
C11—H11A0.9900C25'—H25F0.9800
C11—H11B0.9900C26'—H26D0.9800
C12—C181.362 (4)C26'—H26E0.9800
C12—C12A1.440 (4)C26'—H26F0.9800
C12A—C131.435 (4)C27'—H27D0.9800
C12A—C15A1.453 (4)C27'—H27E0.9800
C13—C141.422 (5)C27'—H27F0.9800
C13—H130.9500C28'—H28D0.9800
C14—C151.419 (4)C28'—H28E0.9800
C14—H140.9500C28'—H28F0.9800
C23—Ru1—C2164.67 (11)C13—C12A—C12133.2 (3)
C23—Ru1—C1938.91 (13)C13—C12A—C15A107.0 (3)
C21—Ru1—C1964.53 (11)C12—C12A—C15A119.8 (3)
C23—Ru1—C2238.43 (12)C13—C12A—Ru269.81 (16)
C21—Ru1—C2238.79 (11)C12—C12A—Ru2125.1 (2)
C19—Ru1—C2264.72 (12)C15A—C12A—Ru271.28 (15)
C23—Ru1—C2064.51 (12)C14—C13—C12A108.7 (3)
C21—Ru1—C2038.51 (11)C14—C13—Ru271.67 (17)
C19—Ru1—C2038.21 (12)C12A—C13—Ru272.20 (16)
C22—Ru1—C2064.58 (11)C14—C13—H13125.7
C23—Ru1—C6111.54 (11)C12A—C13—H13125.7
C21—Ru1—C6155.96 (11)Ru2—C13—H13122.1
C19—Ru1—C6128.84 (11)C15—C14—C13108.5 (3)
C22—Ru1—C6122.98 (11)C15—C14—Ru271.31 (17)
C20—Ru1—C6164.01 (11)C13—C14—Ru270.53 (17)
C23—Ru1—C5125.74 (11)C15—C14—H14125.8
C21—Ru1—C5163.78 (11)C13—C14—H14125.8
C19—Ru1—C5114.41 (11)Ru2—C14—H14124.0
C22—Ru1—C5157.10 (11)C14—C15—C15A108.3 (3)
C20—Ru1—C5130.32 (11)C14—C15—Ru271.14 (17)
C6—Ru1—C537.87 (11)C15A—C15—Ru271.97 (16)
C23—Ru1—C4159.12 (12)C14—C15—H15125.8
C21—Ru1—C4128.51 (11)C15A—C15—H15125.8
C19—Ru1—C4126.46 (12)Ru2—C15—H15122.7
C22—Ru1—C4161.99 (11)C16—C15A—C15132.7 (3)
C20—Ru1—C4114.05 (11)C16—C15A—C12A119.7 (3)
C6—Ru1—C463.59 (11)C15—C15A—C12A107.5 (3)
C5—Ru1—C437.65 (10)C16—C15A—Ru2126.24 (19)
C23—Ru1—C6A126.26 (12)C15—C15A—Ru270.19 (16)
C21—Ru1—C6A122.75 (11)C12A—C15A—Ru270.60 (15)
C19—Ru1—C6A162.34 (12)C17—C16—C15A116.9 (3)
C22—Ru1—C6A109.77 (11)C17—C16—C1120.7 (3)
C20—Ru1—C6A156.92 (11)C15A—C16—C1120.9 (3)
C6—Ru1—C6A38.30 (10)C16—C17—C18121.9 (3)
C5—Ru1—C6A63.55 (11)C16—C17—H17119.1
C4—Ru1—C6A63.86 (10)C18—C17—H17119.1
C23—Ru1—C3A161.11 (12)C12—C18—C17122.5 (3)
C21—Ru1—C3A111.61 (10)C12—C18—H18118.8
C19—Ru1—C3A158.54 (12)C17—C18—H18118.8
C22—Ru1—C3A126.81 (11)C20—C19—C23107.9 (3)
C20—Ru1—C3A125.28 (11)C20—C19—C24126.0 (3)
C6—Ru1—C3A63.62 (10)C23—C19—C24126.0 (3)
C5—Ru1—C3A62.89 (10)C20—C19—Ru171.16 (16)
C4—Ru1—C3A37.68 (10)C23—C19—Ru170.45 (16)
C6A—Ru1—C3A38.31 (10)C24—C19—Ru1127.2 (2)
C23'—Ru2—C22'38.72 (11)C19—C20—C21108.4 (3)
C23'—Ru2—C19'38.67 (11)C19—C20—C25126.4 (3)
C22'—Ru2—C19'64.81 (11)C21—C20—C25125.1 (3)
C23'—Ru2—C21'64.74 (11)C19—C20—Ru170.63 (17)
C22'—Ru2—C21'38.85 (11)C21—C20—Ru170.43 (16)
C19'—Ru2—C21'64.48 (11)C25—C20—Ru1128.3 (2)
C23'—Ru2—C20'64.58 (11)C20—C21—C22107.8 (3)
C22'—Ru2—C20'64.64 (12)C20—C21—C26125.6 (3)
C19'—Ru2—C20'38.49 (11)C22—C21—C26126.5 (3)
C21'—Ru2—C20'38.25 (11)C20—C21—Ru171.06 (16)
C23'—Ru2—C13123.77 (12)C22—C21—Ru170.72 (16)
C22'—Ru2—C13111.83 (12)C26—C21—Ru1124.7 (2)
C19'—Ru2—C13156.68 (12)C23—C22—C21107.9 (3)
C21'—Ru2—C13128.76 (12)C23—C22—C27126.8 (3)
C20'—Ru2—C13163.55 (12)C21—C22—C27125.3 (3)
C23'—Ru2—C14158.07 (12)C23—C22—Ru170.63 (17)
C22'—Ru2—C14126.22 (12)C21—C22—Ru170.49 (16)
C19'—Ru2—C14162.95 (12)C27—C22—Ru1125.8 (2)
C21'—Ru2—C14114.54 (12)C22—C23—C19108.0 (3)
C20'—Ru2—C14129.80 (12)C22—C23—C28126.4 (3)
C13—Ru2—C1437.80 (13)C19—C23—C28125.6 (3)
C23'—Ru2—C15161.08 (12)C22—C23—Ru170.94 (16)
C22'—Ru2—C15159.73 (12)C19—C23—Ru170.64 (17)
C19'—Ru2—C15127.93 (11)C28—C23—Ru1126.2 (2)
C21'—Ru2—C15126.97 (11)C19—C24—H24A109.5
C20'—Ru2—C15113.92 (11)C19—C24—H24B109.5
C13—Ru2—C1563.30 (12)H24A—C24—H24B109.5
C14—Ru2—C1537.55 (11)C19—C24—H24C109.5
C23'—Ru2—C12A109.98 (11)H24A—C24—H24C109.5
C22'—Ru2—C12A126.04 (11)H24B—C24—H24C109.5
C19'—Ru2—C12A123.33 (11)C20—C25—H25A109.5
C21'—Ru2—C12A161.85 (11)C20—C25—H25B109.5
C20'—Ru2—C12A157.52 (11)H25A—C25—H25B109.5
C13—Ru2—C12A37.99 (11)C20—C25—H25C109.5
C14—Ru2—C12A63.31 (12)H25A—C25—H25C109.5
C15—Ru2—C12A63.58 (11)H25B—C25—H25C109.5
C23'—Ru2—C15A125.97 (11)C21—C26—H26A109.5
C22'—Ru2—C15A160.36 (11)C21—C26—H26B109.5
C19'—Ru2—C15A111.32 (11)H26A—C26—H26B109.5
C21'—Ru2—C15A159.23 (11)C21—C26—H26C109.5
C20'—Ru2—C15A125.50 (11)H26A—C26—H26C109.5
C13—Ru2—C15A63.41 (11)H26B—C26—H26C109.5
C14—Ru2—C15A63.00 (11)C22—C27—H27A109.5
C15—Ru2—C15A37.84 (10)C22—C27—H27B109.5
C12A—Ru2—C15A38.12 (10)H27A—C27—H27B109.5
C16—C1—C2113.5 (2)C22—C27—H27C109.5
C16—C1—H1A108.9H27A—C27—H27C109.5
C2—C1—H1A108.9H27B—C27—H27C109.5
C16—C1—H1B108.9C23—C28—H28A109.5
C2—C1—H1B108.9C23—C28—H28B109.5
H1A—C1—H1B107.7H28A—C28—H28B109.5
C3—C2—C1113.8 (2)C23—C28—H28C109.5
C3—C2—H2A108.8H28A—C28—H28C109.5
C1—C2—H2A108.8H28B—C28—H28C109.5
C3—C2—H2B108.8C20'—C19'—C23'108.1 (3)
C1—C2—H2B108.8C20'—C19'—C24'126.3 (3)
H2A—C2—H2B107.7C23'—C19'—C24'125.6 (3)
C9—C3—C3A116.6 (3)C20'—C19'—Ru271.30 (16)
C9—C3—C2121.6 (3)C23'—C19'—Ru270.59 (16)
C3A—C3—C2120.2 (3)C24'—C19'—Ru2124.3 (2)
C4—C3A—C3132.2 (3)C21'—C20'—C19'108.2 (3)
C4—C3A—C6A107.9 (2)C21'—C20'—C25'126.0 (3)
C3—C3A—C6A119.9 (2)C19'—C20'—C25'125.7 (3)
C4—C3A—Ru170.34 (15)C21'—C20'—Ru270.72 (16)
C3—C3A—Ru1127.04 (18)C19'—C20'—Ru270.21 (16)
C6A—C3A—Ru170.08 (14)C25'—C20'—Ru2128.2 (2)
C5—C4—C3A108.1 (2)C20'—C21'—C22'108.0 (3)
C5—C4—Ru171.05 (16)C20'—C21'—C26'125.9 (3)
C3A—C4—Ru171.98 (15)C22'—C21'—C26'125.9 (3)
C5—C4—H4125.9C20'—C21'—Ru271.02 (16)
C3A—C4—H4125.9C22'—C21'—Ru270.13 (16)
Ru1—C4—H4122.7C26'—C21'—Ru2128.1 (2)
C4—C5—C6108.8 (3)C23'—C22'—C21'107.7 (3)
C4—C5—Ru171.31 (15)C23'—C22'—C27'126.3 (3)
C6—C5—Ru170.47 (16)C21'—C22'—C27'126.0 (3)
C4—C5—H5125.6C23'—C22'—Ru270.63 (16)
C6—C5—H5125.6C21'—C22'—Ru271.03 (16)
Ru1—C5—H5124.2C27'—C22'—Ru2126.5 (2)
C5—C6—C6A108.2 (3)C19'—C23'—C22'108.0 (3)
C5—C6—Ru171.66 (16)C19'—C23'—C28'125.4 (3)
C6A—C6—Ru171.61 (15)C22'—C23'—C28'126.5 (3)
C5—C6—H6125.9C19'—C23'—Ru270.74 (16)
C6A—C6—H6125.9C22'—C23'—Ru270.66 (16)
Ru1—C6—H6122.5C28'—C23'—Ru2125.7 (2)
C7—C6A—C6133.2 (3)C19'—C24'—H24D109.5
C7—C6A—C3A119.9 (2)C19'—C24'—H24E109.5
C6—C6A—C3A106.9 (2)H24D—C24'—H24E109.5
C7—C6A—Ru1124.69 (19)C19'—C24'—H24F109.5
C6—C6A—Ru170.09 (15)H24D—C24'—H24F109.5
C3A—C6A—Ru171.61 (15)H24E—C24'—H24F109.5
C8—C7—C6A116.6 (3)C20'—C25'—H25D109.5
C8—C7—C10121.6 (3)C20'—C25'—H25E109.5
C6A—C7—C10120.3 (3)H25D—C25'—H25E109.5
C7—C8—C9122.3 (3)C20'—C25'—H25F109.5
C7—C8—H8118.9H25D—C25'—H25F109.5
C9—C8—H8118.9H25E—C25'—H25F109.5
C3—C9—C8121.8 (3)C21'—C26'—H26D109.5
C3—C9—H9119.1C21'—C26'—H26E109.5
C8—C9—H9119.1H26D—C26'—H26E109.5
C7—C10—C11113.2 (2)C21'—C26'—H26F109.5
C7—C10—H10A108.9H26D—C26'—H26F109.5
C11—C10—H10A108.9H26E—C26'—H26F109.5
C7—C10—H10B108.9C22'—C27'—H27D109.5
C11—C10—H10B108.9C22'—C27'—H27E109.5
H10A—C10—H10B107.8H27D—C27'—H27E109.5
C12—C11—C10113.4 (3)C22'—C27'—H27F109.5
C12—C11—H11A108.9H27D—C27'—H27F109.5
C10—C11—H11A108.9H27E—C27'—H27F109.5
C12—C11—H11B108.9C23'—C28'—H28D109.5
C10—C11—H11B108.9C23'—C28'—H28E109.5
H11A—C11—H11B107.7H28D—C28'—H28E109.5
C18—C12—C12A116.3 (3)C23'—C28'—H28F109.5
C18—C12—C11120.9 (3)H28D—C28'—H28F109.5
C12A—C12—C11121.3 (3)H28E—C28'—H28F109.5

Experimental details

Crystal data
Chemical formula[Ru2(C10H15)2(C22H18)]
Mr754.94
Crystal system, space groupMonoclinic, P21/c
Temperature (K)178
a, b, c (Å)8.647 (2), 13.604 (4), 28.959 (8)
β (°) 92.41 (2)
V3)3403.5 (16)
Z4
Radiation typeMo Kα
µ (mm1)0.92
Crystal size (mm)0.7 × 0.4 × 0.15
Data collection
DiffractometerNicolet R3
diffractometer
Absorption correctionPart of the refinement model (ΔF)
(DIFABS; Walker & Stuart, 1983)
Tmin, Tmax0.66, 0.84
No. of measured, independent and
observed [I > 2σ(I)] reflections
11146, 5984, 5079
Rint0.020
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.071, 1.05
No. of reflections5984
No. of parameters407
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.42, 0.61

Computer programs: P3 (Nicolet, 1987), P3, XDISK (Nicolet, 1987), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1994), SHELXL97.

 

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