Nonacarbon­yl(μ2-methane­thiol­ato)(μ3-trimethyl­silylacetyl­ene)triruthenium

Koentjoro, O.F.; Sparkes, H.A.; Raithby, P.R.

doi:10.1107/S1600536806038451

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 62| Part 12| December 2006| Pages m3220-m3221

https://doi.org/10.1107/S1600536806038451

Nonacarbonyl(μ₂-methanethiolato)(μ₃-trimethylsilylacetylene)triruthenium

Olivia F. Koentjoro,^a Hazel A. Sparkes ^a and Paul R. Raithby ^a,^b ^*

^aDepartment of Chemsitry, University of Bath, Claverton Down, Bath BA2 7AY, England, and ^bCCLRC Daresbury Laboratory, Warrington WA4 4AD, England
^*Correspondence e-mail: p.r.raithby@bath.ac.uk

(Received 13 September 2006; accepted 20 September 2006; online 8 November 2006)

The structure of the title compound, [Ru₃(μ₂CH₃S){μ₃-C₂Si(CH₃)₃}(CO)₉], contains an open triangle of Ru atoms. The open edge is bridged on one side by a μ₂-S(CH₃) unit, and the other side of the triangle is capped by a [C≡CSi(CH₃)₃] group, with the acetylenic bond perpendicular to the open Ru⋯Ru edge.

Comment

The homogeneous desulfurization of thiophene with transition metal compounds has provided an important model for the catalytic heterogeneous dehydrosulfurization of thiophenic components of crude oil (Rauschfuss, 1991 ). Increased catalytic activity has been observed, particularly toward thiophenes, when late transition metals (group 8) are employed (Angelici, 1997 ).

In the context of catalysis, we have been investigating the reactivity of ruthenium carbonyl clusters with thiol derivatives. The reaction of Ru₃(CO)₁₂ with the asymmetric acetylene derivative Me₃SC≡CSiMe₃ under reflux in hexane afforded [Ru₃(CO)₉(μ₂-H₃CS)(μ₃-C₂Si(CH₃)₃], (I), in which the ruthenium cluster has inserted into a C—S bond. This type of reaction has been observed previously (Arce et al., 1994 ).

The cluster consists of an open ruthenium triangle (Fig. 1), with the `non bonding' edge having an Ru⋯Ru distance of 3.360 (1) Å. This edge is bridged symmetrically by a μ₂-S(CH₃) group, and the other side of the metal triangle is capped by a (C≡CSiMe₃) group in which one acetylenic C atom σ-bonds to Ru2 while the acetylenic triple bond is π-bound to Ru1 and Ru3, adopting a bonding mode perpendicular to the long Ru1⋯Ru3 edge. The nine carbonyl ligands are terminal and essentially linear, three being bound to each Ru centre. Overall, the cluster has an electron count of 50, consistent with the observed open triangular metal framework.

Figure 1
The molecular structure of (I)

, showing the atom-numbering scheme (50% probability displacement ellipsoids).

Experimental

Powdered Ru₃(CO)₁₂ (0.102 g, 0.16 mmol) and Me₃SC≡CSiMe₃ (0.085 g, 0.75 mmol) were dissolved in hexane (20 ml) and the mixture refluxed for 3 h, after which a second portion of Me₃SC≡CSiMe₃ [0.090 g, 0.79 mmol, in hexane (5 ml)] was added. The mixture was further refluxed for 1 h and subsequently cooled. Upon solvent removal, the crude product was purified by preparative thin layer chromatography using hexane as an eluent. The title compound was obtained from the yellow band with the highest R_f value after that of Ru₃(CO)₁₂. The product was recrystallized from a 1:1 mixture of CH₂Cl₂/hexane to give yellow block crystals.

Crystal data

[Ru₃(CH₃S)(C₅H₉Si)(CO)₉]
M_r = 699.61
Triclinic, $[P \overline 1]$
a = 9.0510 (1) Å
b = 9.6680 (1) Å
c = 14.5830 (2) Å
α = 76.319 (1)°
β = 88.116 (1)°
γ = 64.933 (10)°
V = 1119.81 (10) Å³
Z = 2
D_x = 2.075 Mg m⁻³
Mo Kα radiation
μ = 2.19 mm⁻¹
T = 150 (2) K
Block, yellow
0.4 × 0.35 × 0.35 mm

Data collection

Bruker–Nonius KappaCCD diffractometer
ω and φ scans
Absorption correction: multi-scan (SORTAV; Blessing, 1995 ) T_min = 0.393, T_max = 0.466
25218 measured reflections
7649 independent reflections
7024 reflections with I > 2σ(I)
R_int = 0.034
θ_max = 32.0°

Refinement

Refinement on F²
R[F² > 2σ(F²)] = 0.025
wR(F²) = 0.060
S = 1.06
7649 reflections
263 parameters
H-atom parameters constrained
w = 1/[σ²(F_o²) + (0.0244P)² + 0.728P] where P = (F_o² + 2F_c²)/3
(Δ/σ)_max < 0.001
Δρ_max = 1.16 e Å⁻³
Δρ_min = −1.05 e Å⁻³
Extinction correction: SHELXL97
Extinction coefficient: 0.0125 (5)

The methyl H atoms were constrained as riding atoms with C—H = 0.98 Å and U_iso(H) = 1.5U_eq(C). The highest residual electron-density peak is 1.81 Å from O8 and the deepest hole is 0.69 Å from Ru2.

Data collection: COLLECT (Nonius, 2000 ); cell refinement: SCALEPACK (Otwinowski & Minor, 1997 ); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: DIRDIF99 (Beurskens et al., 1999 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536806038451/bm2005sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536806038451/bm2005Isup2.hkl

Computing details top

Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: DIRDIF99 (Beurskens et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Nonacarbonyl(µ₂-methanethiolato)(µ₃-trimethylsilylacetylene)triruthenium top

Crystal data top

[Ru₃(CH₃S)(C₅H₉Si)(CO)₉]	Z = 2
M_r = 699.61	F(000) = 672
Triclinic, P1	D_x = 2.075 Mg m⁻³
a = 9.0510 (1) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.6680 (1) Å	Cell parameters from 16094 reflections
c = 14.5830 (2) Å	θ = 2.9–32.0°
α = 76.319 (1)°	µ = 2.19 mm⁻¹
β = 88.116 (1)°	T = 150 K
γ = 64.933 (10)°	Block, yellow
V = 1119.81 (10) Å³	0.4 × 0.35 × 0.35 mm

Data collection top

Bruker–Nonius KappaCCD diffractometer	7649 independent reflections
Radiation source: fine-focus sealed tube	7024 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.034
ω and φ scans	θ_max = 32.0°, θ_min = 3.7°
Absorption correction: multi-scan (SORTAV; Blessing, 1995)	h = −13→13
T_min = 0.393, T_max = 0.466	k = −13→14
25218 measured reflections	l = −18→21

Refinement top

Refinement on F²	H-atom parameters constrained
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0244P)² + 0.728P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.025	(Δ/σ)_max < 0.001
wR(F²) = 0.060	Δρ_max = 1.16 e Å⁻³
S = 1.06	Δρ_min = −1.05 e Å⁻³
7649 reflections	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
263 parameters	Extinction coefficient: 0.0125 (5)
0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ru1	0.141581 (16)	0.205411 (16)	0.227713 (10)	0.01705 (4)
Ru2	0.159195 (16)	0.453982 (16)	0.290179 (10)	0.01715 (4)
Ru3	0.448076 (16)	0.317260 (16)	0.199009 (10)	0.01684 (4)
S1	0.25288 (5)	0.31333 (5)	0.09168 (3)	0.01993 (9)
C1	0.1589 (3)	0.0279 (2)	0.18020 (17)	0.0293 (4)
O1	0.1615 (2)	−0.0723 (2)	0.15244 (17)	0.0508 (5)
C2	0.0595 (2)	0.1353 (3)	0.34375 (15)	0.0276 (4)
O2	0.0129 (2)	0.0942 (3)	0.41279 (13)	0.0482 (5)
C3	−0.0712 (2)	0.3528 (2)	0.17291 (14)	0.0231 (4)
O3	−0.19797 (18)	0.4410 (2)	0.13891 (12)	0.0337 (3)
C4	−0.0089 (2)	0.4664 (2)	0.37529 (14)	0.0242 (4)
O4	−0.1040 (2)	0.4682 (2)	0.42852 (12)	0.0357 (4)
C5	0.0312 (2)	0.6309 (2)	0.18696 (16)	0.0266 (4)
O5	−0.0381 (2)	0.7301 (2)	0.12321 (14)	0.0446 (4)
C6	0.2378 (3)	0.5724 (3)	0.34570 (16)	0.0303 (4)
O6	0.2833 (3)	0.6430 (3)	0.37957 (17)	0.0549 (5)
C7	0.4168 (2)	0.5173 (2)	0.12179 (14)	0.0250 (4)
O7	0.3990 (2)	0.63528 (19)	0.07424 (13)	0.0396 (4)
C8	0.5770 (2)	0.3371 (2)	0.29268 (14)	0.0241 (4)
O8	0.6535 (2)	0.3509 (2)	0.34671 (12)	0.0375 (4)
C9	0.6388 (2)	0.1860 (2)	0.14350 (15)	0.0256 (4)
O9	0.7511 (2)	0.1104 (2)	0.11253 (13)	0.0401 (4)
C10	0.3184 (2)	0.2342 (2)	0.31745 (12)	0.0175 (3)
C11	0.4126 (2)	0.1028 (2)	0.29716 (13)	0.0191 (3)
Si1	0.56728 (6)	−0.10449 (6)	0.34213 (4)	0.02014 (10)
C12	0.4938 (3)	−0.1902 (2)	0.45160 (15)	0.0297 (4)
H12A	0.39	−0.1916	0.4362	0.045*
H12B	0.4776	−0.1261	0.4973	0.045*
H12C	0.5751	−0.298	0.4791	0.045*
C13	0.5906 (3)	−0.2166 (3)	0.25057 (15)	0.0301 (4)
H13A	0.6295	−0.1691	0.1937	0.045*
H13B	0.4846	−0.2133	0.2346	0.045*
H13C	0.6698	−0.3263	0.2753	0.045*
C14	0.7655 (3)	−0.1011 (3)	0.37012 (18)	0.0315 (4)
H14A	0.8032	−0.0555	0.312	0.047*
H14B	0.8473	−0.2088	0.3972	0.047*
H14C	0.75	−0.0372	0.4158	0.047*
C15	0.3635 (3)	0.1569 (3)	0.03268 (15)	0.0291 (4)
H15A	0.4101	0.1976	−0.023	0.044*
H15B	0.2882	0.1186	0.0129	0.044*
H15C	0.4517	0.0701	0.0764	0.044*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ru1	0.01543 (7)	0.01754 (7)	0.01896 (7)	−0.00819 (5)	−0.00003 (5)	−0.00350 (5)
Ru2	0.01528 (7)	0.01648 (7)	0.01918 (7)	−0.00573 (5)	0.00145 (5)	−0.00554 (5)
Ru3	0.01455 (7)	0.01741 (7)	0.01837 (7)	−0.00731 (5)	0.00219 (5)	−0.00329 (5)
S1	0.01897 (19)	0.0221 (2)	0.01693 (19)	−0.00742 (16)	0.00085 (15)	−0.00414 (16)
C1	0.0244 (9)	0.0260 (9)	0.0399 (11)	−0.0116 (8)	−0.0015 (8)	−0.0101 (9)
O1	0.0462 (11)	0.0392 (10)	0.0787 (15)	−0.0200 (9)	−0.0014 (10)	−0.0313 (10)
C2	0.0233 (9)	0.0300 (10)	0.0288 (10)	−0.0148 (8)	−0.0014 (7)	0.0007 (8)
O2	0.0468 (11)	0.0593 (12)	0.0359 (9)	−0.0307 (10)	0.0059 (8)	0.0081 (9)
C3	0.0189 (8)	0.0283 (9)	0.0235 (9)	−0.0128 (7)	0.0019 (6)	−0.0039 (7)
O3	0.0192 (7)	0.0381 (8)	0.0364 (8)	−0.0102 (6)	−0.0032 (6)	0.0009 (7)
C4	0.0207 (8)	0.0258 (9)	0.0255 (9)	−0.0077 (7)	0.0019 (7)	−0.0095 (7)
O4	0.0290 (8)	0.0464 (9)	0.0348 (8)	−0.0164 (7)	0.0126 (6)	−0.0162 (7)
C5	0.0220 (9)	0.0210 (8)	0.0333 (10)	−0.0071 (7)	−0.0009 (7)	−0.0040 (8)
O5	0.0387 (9)	0.0337 (9)	0.0475 (11)	−0.0109 (7)	−0.0130 (8)	0.0083 (8)
C6	0.0296 (10)	0.0312 (10)	0.0357 (11)	−0.0158 (9)	0.0053 (8)	−0.0137 (9)
O6	0.0630 (13)	0.0619 (13)	0.0666 (14)	−0.0417 (11)	0.0061 (11)	−0.0354 (11)
C7	0.0245 (9)	0.0243 (9)	0.0263 (9)	−0.0115 (7)	0.0053 (7)	−0.0049 (7)
O7	0.0458 (10)	0.0270 (8)	0.0415 (9)	−0.0175 (7)	0.0066 (8)	0.0030 (7)
C8	0.0210 (8)	0.0273 (9)	0.0261 (9)	−0.0135 (7)	0.0032 (7)	−0.0046 (7)
O8	0.0346 (8)	0.0512 (10)	0.0356 (9)	−0.0262 (8)	−0.0031 (7)	−0.0110 (8)
C9	0.0205 (8)	0.0265 (9)	0.0275 (9)	−0.0091 (7)	0.0034 (7)	−0.0047 (8)
O9	0.0277 (8)	0.0397 (9)	0.0416 (9)	−0.0041 (7)	0.0112 (7)	−0.0109 (8)
C10	0.0158 (7)	0.0193 (8)	0.0173 (7)	−0.0086 (6)	0.0005 (6)	−0.0023 (6)
C11	0.0182 (7)	0.0191 (8)	0.0196 (8)	−0.0088 (6)	−0.0004 (6)	−0.0021 (6)
Si1	0.0199 (2)	0.0164 (2)	0.0215 (2)	−0.00547 (18)	−0.00286 (18)	−0.00376 (18)
C12	0.0411 (12)	0.0239 (9)	0.0232 (9)	−0.0155 (9)	−0.0030 (8)	−0.0004 (8)
C13	0.0287 (10)	0.0260 (10)	0.0289 (10)	−0.0022 (8)	−0.0029 (8)	−0.0123 (8)
C14	0.0220 (9)	0.0253 (9)	0.0429 (12)	−0.0066 (8)	−0.0088 (8)	−0.0058 (9)
C15	0.0292 (10)	0.0347 (11)	0.0242 (9)	−0.0104 (8)	0.0043 (7)	−0.0154 (8)

Geometric parameters (Å, º) top

Ru1—C1	1.944 (2)	C5—O5	1.133 (3)
Ru1—C2	1.917 (2)	C6—O6	1.136 (3)
Ru1—C3	1.9014 (19)	C7—O7	1.134 (2)
Ru1—C10	2.2451 (17)	C8—O8	1.132 (2)
Ru1—C11	2.3775 (18)	C9—O9	1.126 (3)
Ru1—S1	2.4122 (5)	C10—C11	1.293 (2)
Ru1—Ru2	2.8285 (2)	C11—Si1	1.8619 (18)
Ru2—C4	1.914 (2)	Si1—C12	1.857 (2)
Ru2—C5	1.937 (2)	Si1—C13	1.864 (2)
Ru2—C6	1.908 (2)	Si1—C14	1.869 (2)
Ru2—C10	1.9474 (18)	C12—H12A	0.98
Ru2—Ru3	2.8329 (2)	C12—H12B	0.98
Ru3—C7	1.902 (2)	C12—H12C	0.98
Ru3—C8	1.919 (2)	C13—H13A	0.98
Ru3—C9	1.946 (2)	C13—H13B	0.98
Ru3—C10	2.2390 (17)	C13—H13C	0.98
Ru3—C11	2.3628 (18)	C14—H14A	0.98
Ru3—S1	2.4165 (5)	C14—H14B	0.98
S1—C15	1.818 (2)	C14—H14C	0.98
C1—O1	1.126 (3)	C15—H15A	0.98
C2—O2	1.129 (3)	C15—H15B	0.98
C3—O3	1.139 (2)	C15—H15C	0.98
C4—O4	1.137 (2)

C3—Ru1—C2	92.71 (8)	S1—Ru3—Ru2	80.780 (11)
C3—Ru1—C1	98.86 (9)	C15—S1—Ru1	107.75 (8)
C2—Ru1—C1	92.78 (10)	C15—S1—Ru3	107.46 (7)
C3—Ru1—C10	129.73 (7)	Ru1—S1—Ru3	88.197 (15)
C2—Ru1—C10	86.71 (8)	O1—C1—Ru1	176.9 (2)
C1—Ru1—C10	131.40 (8)	O2—C2—Ru1	179.0 (2)
C3—Ru1—C11	160.31 (7)	O3—C3—Ru1	179.09 (18)
C2—Ru1—C11	93.47 (7)	O4—C4—Ru2	177.03 (19)
C1—Ru1—C11	99.49 (8)	O5—C5—Ru2	176.2 (2)
C10—Ru1—C11	32.34 (6)	O6—C6—Ru2	179.2 (2)
C3—Ru1—S1	88.47 (6)	O7—C7—Ru3	178.62 (19)
C2—Ru1—S1	172.95 (7)	O8—C8—Ru3	178.75 (19)
C1—Ru1—S1	93.91 (7)	O9—C9—Ru3	178.6 (2)
C10—Ru1—S1	87.19 (5)	C11—C10—Ru2	155.62 (15)
C11—Ru1—S1	83.23 (4)	C11—C10—Ru3	79.02 (11)
C3—Ru1—Ru2	86.63 (6)	Ru2—C10—Ru3	84.87 (6)
C2—Ru1—Ru2	92.18 (7)	C11—C10—Ru1	79.47 (11)
C1—Ru1—Ru2	172.42 (6)	Ru2—C10—Ru1	84.54 (6)
C10—Ru1—Ru2	43.26 (4)	Ru3—C10—Ru1	97.07 (7)
C11—Ru1—Ru2	74.48 (4)	C10—C11—Si1	146.86 (15)
S1—Ru1—Ru2	80.943 (12)	C10—C11—Ru3	68.47 (11)
C6—Ru2—C4	94.63 (9)	Si1—C11—Ru3	128.62 (9)
C6—Ru2—C5	94.29 (9)	C10—C11—Ru1	68.19 (11)
C4—Ru2—C5	98.92 (9)	Si1—C11—Ru1	130.61 (9)
C6—Ru2—C10	110.12 (8)	Ru3—C11—Ru1	90.29 (6)
C4—Ru2—C10	106.94 (8)	C12—Si1—C11	107.21 (9)
C5—Ru2—C10	142.30 (8)	C12—Si1—C13	111.17 (10)
C6—Ru2—Ru1	162.17 (7)	C11—Si1—C13	109.82 (9)
C4—Ru2—Ru1	93.48 (6)	C12—Si1—C14	110.06 (11)
C5—Ru2—Ru1	100.11 (6)	C11—Si1—C14	108.08 (9)
C10—Ru2—Ru1	52.20 (5)	C13—Si1—C14	110.40 (11)
C6—Ru2—Ru3	94.61 (7)	Si1—C12—H12A	109.5
C4—Ru2—Ru3	158.83 (6)	Si1—C12—H12B	109.5
C5—Ru2—Ru3	99.34 (6)	H12A—C12—H12B	109.5
C10—Ru2—Ru3	51.92 (5)	Si1—C12—H12C	109.5
Ru1—Ru2—Ru3	72.818 (5)	H12A—C12—H12C	109.5
C7—Ru3—C8	90.71 (9)	H12B—C12—H12C	109.5
C7—Ru3—C9	98.61 (8)	Si1—C13—H13A	109.5
C8—Ru3—C9	93.40 (9)	Si1—C13—H13B	109.5
C7—Ru3—C10	134.79 (7)	H13A—C13—H13B	109.5
C8—Ru3—C10	87.66 (7)	Si1—C13—H13C	109.5
C9—Ru3—C10	126.60 (8)	H13A—C13—H13C	109.5
C7—Ru3—C11	165.05 (7)	H13B—C13—H13C	109.5
C8—Ru3—C11	95.49 (7)	Si1—C14—H14A	109.5
C9—Ru3—C11	94.59 (7)	Si1—C14—H14B	109.5
C10—Ru3—C11	32.51 (6)	H14A—C14—H14B	109.5
C7—Ru3—S1	88.51 (6)	Si1—C14—H14C	109.5
C8—Ru3—S1	171.98 (6)	H14A—C14—H14C	109.5
C9—Ru3—S1	94.61 (6)	H14B—C14—H14C	109.5
C10—Ru3—S1	87.23 (4)	S1—C15—H15A	109.5
C11—Ru3—S1	83.45 (4)	S1—C15—H15B	109.5
C7—Ru3—Ru2	91.72 (6)	H15A—C15—H15B	109.5
C8—Ru3—Ru2	91.27 (6)	S1—C15—H15C	109.5
C9—Ru3—Ru2	168.60 (6)	H15A—C15—H15C	109.5
C10—Ru3—Ru2	43.21 (4)	H15B—C15—H15C	109.5
C11—Ru3—Ru2	74.60 (4)

C3—Ru1—Ru2—C6	−176.4 (2)	C5—Ru2—C10—Ru1	−50.20 (14)
C2—Ru1—Ru2—C6	91.0 (2)	Ru3—Ru2—C10—Ru1	−97.63 (6)
C10—Ru1—Ru2—C6	8.1 (2)	C7—Ru3—C10—C11	167.28 (12)
C11—Ru1—Ru2—C6	−2.0 (2)	C8—Ru3—C10—C11	−104.04 (12)
S1—Ru1—Ru2—C6	−87.4 (2)	C9—Ru3—C10—C11	−11.53 (15)
C3—Ru1—Ru2—C4	66.65 (8)	S1—Ru3—C10—C11	82.15 (11)
C2—Ru1—Ru2—C4	−25.94 (9)	Ru2—Ru3—C10—C11	161.61 (14)
C10—Ru1—Ru2—C4	−108.80 (9)	C7—Ru3—C10—Ru2	5.67 (13)
C11—Ru1—Ru2—C4	−118.94 (7)	C8—Ru3—C10—Ru2	94.35 (8)
S1—Ru1—Ru2—C4	155.63 (6)	C9—Ru3—C10—Ru2	−173.15 (8)
C3—Ru1—Ru2—C5	−33.06 (8)	C11—Ru3—C10—Ru2	−161.61 (14)
C2—Ru1—Ru2—C5	−125.64 (9)	S1—Ru3—C10—Ru2	−79.47 (5)
C10—Ru1—Ru2—C5	151.49 (9)	C7—Ru3—C10—Ru1	89.50 (11)
C11—Ru1—Ru2—C5	141.36 (8)	C8—Ru3—C10—Ru1	178.18 (8)
S1—Ru1—Ru2—C5	55.92 (6)	C9—Ru3—C10—Ru1	−89.32 (10)
C3—Ru1—Ru2—C10	175.45 (9)	C11—Ru3—C10—Ru1	−77.78 (11)
C2—Ru1—Ru2—C10	82.86 (9)	S1—Ru3—C10—Ru1	4.36 (5)
C11—Ru1—Ru2—C10	−10.14 (8)	Ru2—Ru3—C10—Ru1	83.83 (6)
S1—Ru1—Ru2—C10	−95.57 (6)	C3—Ru1—C10—C11	−167.43 (12)
C3—Ru1—Ru2—Ru3	−129.80 (6)	C2—Ru1—C10—C11	101.79 (13)
C2—Ru1—Ru2—Ru3	137.62 (6)	C1—Ru1—C10—C11	10.98 (16)
C10—Ru1—Ru2—Ru3	54.75 (6)	S1—Ru1—C10—C11	−81.76 (11)
C11—Ru1—Ru2—Ru3	44.61 (4)	Ru2—Ru1—C10—C11	−161.51 (14)
S1—Ru1—Ru2—Ru3	−40.817 (11)	C3—Ru1—C10—Ru2	−5.91 (11)
C6—Ru2—Ru3—C7	−63.94 (10)	C2—Ru1—C10—Ru2	−96.70 (8)
C4—Ru2—Ru3—C7	−179.54 (17)	C1—Ru1—C10—Ru2	172.49 (9)
C5—Ru2—Ru3—C7	31.18 (9)	C11—Ru1—C10—Ru2	161.51 (14)
C10—Ru2—Ru3—C7	−175.98 (9)	S1—Ru1—C10—Ru2	79.75 (5)
Ru1—Ru2—Ru3—C7	128.96 (6)	C3—Ru1—C10—Ru3	−90.04 (10)
C6—Ru2—Ru3—C8	26.81 (9)	C2—Ru1—C10—Ru3	179.18 (8)
C4—Ru2—Ru3—C8	−88.79 (17)	C1—Ru1—C10—Ru3	88.37 (11)
C5—Ru2—Ru3—C8	121.94 (9)	C11—Ru1—C10—Ru3	77.39 (11)
C10—Ru2—Ru3—C8	−85.22 (9)	S1—Ru1—C10—Ru3	−4.37 (5)
Ru1—Ru2—Ru3—C8	−140.28 (6)	Ru2—Ru1—C10—Ru3	−84.12 (7)
C6—Ru2—Ru3—C9	141.0 (3)	Ru2—C10—C11—Si1	178.09 (18)
C4—Ru2—Ru3—C9	25.4 (4)	Ru3—C10—C11—Si1	128.5 (3)
C5—Ru2—Ru3—C9	−123.8 (3)	Ru1—C10—C11—Si1	−132.0 (3)
C10—Ru2—Ru3—C9	29.0 (3)	Ru2—C10—C11—Ru3	49.5 (3)
Ru1—Ru2—Ru3—C9	−26.1 (3)	Ru1—C10—C11—Ru3	99.42 (5)
C6—Ru2—Ru3—C10	112.04 (10)	Ru2—C10—C11—Ru1	−49.9 (3)
C4—Ru2—Ru3—C10	−3.56 (17)	Ru3—C10—C11—Ru1	−99.42 (5)
C5—Ru2—Ru3—C10	−152.84 (9)	C7—Ru3—C11—C10	−37.3 (3)
Ru1—Ru2—Ru3—C10	−55.06 (6)	C8—Ru3—C11—C10	76.86 (12)
C6—Ru2—Ru3—C11	122.16 (8)	C9—Ru3—C11—C10	170.73 (12)
C4—Ru2—Ru3—C11	6.56 (17)	S1—Ru3—C11—C10	−95.15 (11)
C5—Ru2—Ru3—C11	−142.71 (8)	Ru2—Ru3—C11—C10	−12.94 (10)
C10—Ru2—Ru3—C11	10.13 (8)	C7—Ru3—C11—Si1	175.9 (3)
Ru1—Ru2—Ru3—C11	−44.93 (4)	C8—Ru3—C11—Si1	−69.96 (12)
C6—Ru2—Ru3—S1	−152.15 (7)	C9—Ru3—C11—Si1	23.91 (13)
C4—Ru2—Ru3—S1	92.25 (16)	C10—Ru3—C11—Si1	−146.82 (19)
C5—Ru2—Ru3—S1	−57.03 (6)	S1—Ru3—C11—Si1	118.03 (11)
C10—Ru2—Ru3—S1	95.81 (6)	Ru2—Ru3—C11—Si1	−159.77 (12)
Ru1—Ru2—Ru3—S1	40.754 (12)	C7—Ru3—C11—Ru1	29.1 (3)
C3—Ru1—S1—C15	−118.31 (10)	C8—Ru3—C11—Ru1	143.20 (7)
C1—Ru1—S1—C15	−19.54 (10)	C9—Ru3—C11—Ru1	−122.93 (7)
C10—Ru1—S1—C15	111.78 (9)	C10—Ru3—C11—Ru1	66.34 (10)
C11—Ru1—S1—C15	79.57 (9)	S1—Ru3—C11—Ru1	−28.81 (4)
Ru2—Ru1—S1—C15	154.86 (7)	Ru2—Ru3—C11—Ru1	53.39 (4)
C3—Ru1—S1—Ru3	133.92 (6)	C3—Ru1—C11—C10	29.8 (3)
C1—Ru1—S1—Ru3	−127.30 (6)	C2—Ru1—C11—C10	−78.27 (13)
C10—Ru1—S1—Ru3	4.02 (5)	C1—Ru1—C11—C10	−171.67 (12)
C11—Ru1—S1—Ru3	−28.19 (4)	S1—Ru1—C11—C10	95.48 (11)
Ru2—Ru1—S1—Ru3	47.094 (10)	Ru2—Ru1—C11—C10	13.03 (10)
C7—Ru3—S1—C15	112.94 (10)	C3—Ru1—C11—Si1	177.46 (17)
C9—Ru3—S1—C15	14.42 (10)	C2—Ru1—C11—Si1	69.40 (13)
C10—Ru3—S1—C15	−112.08 (9)	C1—Ru1—C11—Si1	−24.01 (14)
C11—Ru3—S1—C15	−79.68 (9)	C10—Ru1—C11—Si1	147.66 (19)
Ru2—Ru3—S1—C15	−155.08 (8)	S1—Ru1—C11—Si1	−116.86 (12)
C7—Ru3—S1—Ru1	−139.01 (6)	Ru2—Ru1—C11—Si1	160.70 (12)
C9—Ru3—S1—Ru1	122.48 (6)	C3—Ru1—C11—Ru3	−36.8 (2)
C10—Ru3—S1—Ru1	−4.03 (5)	C2—Ru1—C11—Ru3	−144.86 (8)
C11—Ru3—S1—Ru1	28.37 (4)	C1—Ru1—C11—Ru3	121.73 (8)
Ru2—Ru3—S1—Ru1	−47.024 (10)	C10—Ru1—C11—Ru3	−66.60 (10)
C6—Ru2—C10—C11	−128.3 (3)	S1—Ru1—C11—Ru3	28.88 (4)
C4—Ru2—C10—C11	130.1 (3)	Ru2—Ru1—C11—Ru3	−53.56 (4)
C5—Ru2—C10—C11	−1.2 (4)	C10—C11—Si1—C12	44.6 (3)
Ru1—Ru2—C10—C11	49.0 (3)	Ru3—C11—Si1—C12	156.01 (11)
Ru3—Ru2—C10—C11	−48.6 (3)	Ru1—C11—Si1—C12	−70.09 (14)
C6—Ru2—C10—Ru3	−79.73 (9)	C10—C11—Si1—C13	165.5 (3)
C4—Ru2—C10—Ru3	178.66 (7)	Ru3—C11—Si1—C13	−83.09 (13)
C5—Ru2—C10—Ru3	47.43 (14)	Ru1—C11—Si1—C13	50.81 (15)
Ru1—Ru2—C10—Ru3	97.63 (6)	C10—C11—Si1—C14	−74.0 (3)
C6—Ru2—C10—Ru1	−177.36 (8)	Ru3—C11—Si1—C14	37.40 (15)
C4—Ru2—C10—Ru1	81.03 (8)	Ru1—C11—Si1—C14	171.30 (12)

Acknowledgements

We are grateful to the EPSRC for funding and to the Cambridge Crystallographic Data Centre for a studentship to HAS.

References

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Volume 62| Part 12| December 2006| Pages m3220-m3221

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