Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802016768/lh6000sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802016768/lh6000Isup2.hkl |
CCDC reference: 198312
A mixture of Ru3(CO)12 (0.100 g, 0.156 mmol) and HC≡CSiiPr3 (0.056 g, 0.156 mmol) in toluene (15 cm3) was heated with stirring at 358 K for 2.5 h. After removing the solvent in vacuo, the residue was crystallized from hexane at 253 K giving yellow crystals of [Ru3(CO)9(µ-H)(µ3-C2SiiPr3)] (0.090 g, 78.2% yield). Anal. Calcd. for C20H22O9SiRu3 (Found) C, 32.56 (32.79); H, 3.01 (2.81) %. IR (toluene, cm-1) ν(CO): 2095 (m), 2067 (versus), 2050 (versus), 2018 (versus), 1984 (m). 1H NMR (CDCl3): δ= 1.17 [s, 21H, iPr], -20.83 [s, 1H, H]. FAB+ (m/z): 737 (M+), 711–485 (M+-nCO, n= 1–9).
All H atoms atoms were located in difference Fourier maps, and refined by using a riding-model approximation with an isotropic displacement parameter fixed at 20% higher than those of the carbons atoms to which they are connected. The hydride H was refined independently with an isotropic displacement parameter. Owing to the geometry of the Stoe IPDS diffractometer which has only one circle (φ rotation), the coverage of the data is usually not complete and only around 90%. To obtain a better coverage, we would need to recollect data with the crystal mounted in a different orientation.
Acetylide compounds are being widely studied because of the versatile coordination modes of the unsaturated fragments which act as metalloligands (Ara et al., 1995). Researchers are also interested in cluster chemistry containing C2R groups regarding their implications in the syntheses of organic molecules that take place on metal surfaces (Chi et al., 1997). More recently the acetylide derivatives have been used as precursors to synthesize polymetallic compounds bearing unsaturated polycarbon chains (Alcalde et al., 2001). Herein we report the structure of the new compound [Ru3(CO)9(µ-H)(µ3-C2SiiPr3)], (I). The ν(CO) pattern in the carbonyl region as well as the 1H NMR resonance for hydride observed in the spectra are in agreement with data reported on analogous compounds (Sappa et al., 1972; Edwards et al., 1995).
The title compound consists of a triangular ruthenium cluster (see Fig. 1). The Ru—Ru distances [Ru1—Ru3 2.8010 (9), Ru1—Ru2 2.7907 (13) and Ru2—Ru3 2.7957 (11) Å] are similar to those reported for other compounds of this type. [Ru3(CO)9(µ-H)(µ3-C2R)] [R= H [2.792 (1), 2.803 (1), 2.810 (1) Å (Bruce et al., 1999); tBu [2.790 (2), 2.795 (2), 2.796 (2) Å (Gervasio & Ferraris, 1973)]. The three ruthenium atoms in all of these compounds form an almost equilateral triangle. In (I) the acetylide ligand is σ-bonded to one Ru atom [Ru2—C1 1.958 (2) Å] and π-bonded to the other two Ru atoms [Ru3—C1 2.215 (2), Ru1—C1 2.206 (2), Ru3—C2 2.302 (3) and Ru1—C2 2.322 (2) Å]. The acetylide group is acting as 5 e- donor, the C1—C2 distance [1.299 (3) Å] being comparable to that in other acetylide clusters [Ru3(CO)9(µ-H)(µ3-C2R)][R= H [1.28 (1) Å (Bruce et al., 1999)]; t Bu [1.29 (3) Å (Gervasio & Ferraris, 1973)]. The hydride is unsymmetrically located between atoms Ru1 and Ru3 giving Ru—H distances of 1.81 (3) and 1.77 (3) Å (see Table 1.). Three terminal CO ligands around each metal atom complete the structure.
Data collection: IPDS Software (Stoe, 1996); cell refinement: IPDS Software; data reduction: X-RED (Stoe, 1996); program(s) used to solve structure: SIR92 (Altomare et al., 1994) in WjnGX (Farrugia, 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997) in WinGX; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) in WinGX; software used to prepare material for publication: SHELXL97 in WinGX.
[Ru3(C11H22Si)(CO)9] | Z = 2 |
Mr = 737.68 | F(000) = 720 |
Triclinic, P1 | Dx = 1.91 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 9.3592 (13) Å | Cell parameters from 5000 reflections |
b = 11.8691 (18) Å | θ = 1.5–26.0° |
c = 12.6669 (17) Å | µ = 1.83 mm−1 |
α = 79.393 (17)° | T = 160 K |
β = 87.314 (17)° | Parallelepiped, orange yellow |
γ = 68.106 (16)° | 0.4 × 0.35 × 0.2 mm |
V = 1282.9 (3) Å3 |
Stoe IPDS diffractometer | 4456 reflections with I > 2σ(I) |
φ scans | Rint = 0.028 |
Absorption correction: multi-scan (Blessing, 1995) | θmax = 26.0°, θmin = 3.5° |
Tmin = 0.342, Tmax = 0.463 | h = −11→11 |
12223 measured reflections | k = −14→14 |
4546 independent reflections | l = −15→15 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.020 | w = 1/[σ2(Fo2) + (0.0241P)2 + 1.1678P] where P = Fo2 + 2Fc2)/3 |
wR(F2) = 0.054 | (Δ/σ)max = 0.002 |
S = 1.13 | Δρmax = 0.37 e Å−3 |
4546 reflections | Δρmin = −0.40 e Å−3 |
320 parameters |
[Ru3(C11H22Si)(CO)9] | γ = 68.106 (16)° |
Mr = 737.68 | V = 1282.9 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 9.3592 (13) Å | Mo Kα radiation |
b = 11.8691 (18) Å | µ = 1.83 mm−1 |
c = 12.6669 (17) Å | T = 160 K |
α = 79.393 (17)° | 0.4 × 0.35 × 0.2 mm |
β = 87.314 (17)° |
Stoe IPDS diffractometer | 4546 independent reflections |
Absorption correction: multi-scan (Blessing, 1995) | 4456 reflections with I > 2σ(I) |
Tmin = 0.342, Tmax = 0.463 | Rint = 0.028 |
12223 measured reflections |
R[F2 > 2σ(F2)] = 0.020 | 0 restraints |
wR(F2) = 0.054 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.13 | Δρmax = 0.37 e Å−3 |
4546 reflections | Δρmin = −0.40 e Å−3 |
320 parameters |
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. The structure has been refined by means of least-squares procedures on a F2 with the aid of the program SHELXL97 include in the softwares package WinGX version 1.63. The Atomic Scattering Factors were taken from International tables for X-Ray Crystallography. All non-H atoms atoms were anisotropically refined, and in the last cycles of refinement a weighting scheme was used, where weights are calculated from the following formula: w=1/[σ2(Fo2)+(aP)2+bP] where P=(Fo2+2Fc2)/3. 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 > 2σ(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 | −0.01078 (2) | 0.413152 (16) | 0.768929 (14) | 0.01971 (6) | |
Ru2 | −0.28060 (2) | 0.398048 (17) | 0.862315 (15) | 0.02237 (7) | |
Ru3 | −0.21596 (2) | 0.359488 (17) | 0.651244 (14) | 0.02084 (6) | |
Si | 0.16340 (8) | 0.07630 (6) | 0.72245 (5) | 0.02073 (13) | |
O11 | 0.2856 (2) | 0.41617 (18) | 0.65700 (18) | 0.0401 (5) | |
O12 | 0.1373 (2) | 0.3607 (2) | 0.99054 (15) | 0.0382 (5) | |
O13 | −0.1529 (3) | 0.68922 (17) | 0.76664 (16) | 0.0380 (5) | |
O21 | −0.2070 (3) | 0.3935 (2) | 1.09514 (16) | 0.0452 (5) | |
O22 | −0.5022 (3) | 0.66766 (19) | 0.8205 (2) | 0.0540 (6) | |
O23 | −0.5285 (3) | 0.2895 (2) | 0.9097 (2) | 0.0521 (6) | |
O31 | −0.4866 (3) | 0.59904 (19) | 0.57837 (18) | 0.0452 (5) | |
O32 | −0.4142 (2) | 0.20480 (19) | 0.66898 (18) | 0.0411 (5) | |
O33 | −0.1131 (3) | 0.31402 (19) | 0.42391 (15) | 0.0427 (5) | |
C1 | −0.1073 (3) | 0.2676 (2) | 0.81170 (18) | 0.0208 (5) | |
C2 | 0.0007 (3) | 0.2202 (2) | 0.74666 (18) | 0.0213 (5) | |
C11 | 0.1760 (3) | 0.4113 (2) | 0.6951 (2) | 0.0263 (5) | |
C12 | 0.0838 (3) | 0.3788 (2) | 0.9076 (2) | 0.0272 (5) | |
C13 | −0.0983 (3) | 0.5855 (2) | 0.7707 (2) | 0.0276 (5) | |
C21 | −0.2354 (3) | 0.3958 (3) | 1.0083 (2) | 0.0319 (6) | |
C22 | −0.4205 (3) | 0.5675 (2) | 0.8384 (2) | 0.0328 (6) | |
C23 | −0.4381 (3) | 0.3318 (3) | 0.8918 (2) | 0.0316 (6) | |
C31 | −0.3876 (3) | 0.5089 (3) | 0.6066 (2) | 0.0316 (6) | |
C32 | −0.3404 (3) | 0.2627 (2) | 0.6612 (2) | 0.0281 (5) | |
C33 | −0.1444 (3) | 0.3286 (2) | 0.5091 (2) | 0.0289 (5) | |
C111 | 0.0943 (3) | −0.0558 (2) | 0.7632 (2) | 0.0284 (5) | |
C112 | −0.0271 (4) | −0.0500 (3) | 0.6838 (3) | 0.0409 (7) | |
H11A | 0.0148 | −0.0488 | 0.6114 | 0.061* | |
H11B | −0.1186 | 0.025 | 0.6846 | 0.061* | |
H11C | −0.0554 | −0.1226 | 0.7044 | 0.061* | |
C113 | 0.0315 (5) | −0.0669 (3) | 0.8769 (3) | 0.0521 (9) | |
H11D | 0.114 | −0.0839 | 0.9294 | 0.078* | |
H11E | −0.0069 | −0.1345 | 0.8898 | 0.078* | |
H11F | −0.0527 | 0.0106 | 0.8843 | 0.078* | |
C121 | 0.2029 (3) | 0.0890 (2) | 0.5744 (2) | 0.0276 (5) | |
C122 | 0.3113 (4) | −0.0341 (3) | 0.5440 (2) | 0.0379 (6) | |
H12A | 0.2709 | −0.0988 | 0.5715 | 0.057* | |
H12B | 0.4141 | −0.0568 | 0.5754 | 0.057* | |
H12C | 0.3177 | −0.0249 | 0.4656 | 0.057* | |
C123 | 0.2591 (3) | 0.1926 (3) | 0.5275 (2) | 0.0330 (6) | |
H12D | 0.1826 | 0.2718 | 0.5397 | 0.05* | |
H12E | 0.2735 | 0.1947 | 0.4501 | 0.05* | |
H12F | 0.3572 | 0.178 | 0.5624 | 0.05* | |
C131 | 0.3292 (3) | 0.0706 (2) | 0.8053 (2) | 0.0262 (5) | |
C132 | 0.4866 (3) | −0.0285 (3) | 0.7879 (3) | 0.0386 (6) | |
H13A | 0.5124 | −0.016 | 0.7119 | 0.058* | |
H13B | 0.4816 | −0.1106 | 0.8092 | 0.058* | |
H13C | 0.5658 | −0.0218 | 0.8316 | 0.058* | |
C133 | 0.2958 (4) | 0.0618 (3) | 0.9252 (2) | 0.0382 (6) | |
H13D | 0.1889 | 0.1151 | 0.9349 | 0.057* | |
H13E | 0.3655 | 0.0886 | 0.9605 | 0.057* | |
H13F | 0.3116 | −0.0238 | 0.9572 | 0.057* | |
H1 | 0.191 (4) | −0.133 (3) | 0.763 (2) | 0.034 (8)* | |
H2 | 0.112 (4) | 0.101 (3) | 0.545 (2) | 0.023 (7)* | |
H3 | 0.333 (3) | 0.146 (3) | 0.781 (2) | 0.026 (7)* | |
H | −0.115 (4) | 0.461 (3) | 0.642 (2) | 0.039 (8)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.01952 (11) | 0.01985 (10) | 0.02139 (10) | −0.00883 (8) | 0.00124 (8) | −0.00463 (7) |
Ru2 | 0.02044 (11) | 0.02240 (10) | 0.02557 (11) | −0.00843 (9) | 0.00541 (8) | −0.00762 (8) |
Ru3 | 0.01886 (11) | 0.02105 (10) | 0.02192 (10) | −0.00610 (8) | −0.00201 (8) | −0.00433 (7) |
Si | 0.0194 (3) | 0.0198 (3) | 0.0222 (3) | −0.0061 (3) | 0.0008 (3) | −0.0047 (2) |
O11 | 0.0273 (11) | 0.0357 (10) | 0.0544 (12) | −0.0124 (9) | 0.0105 (10) | −0.0023 (9) |
O12 | 0.0383 (12) | 0.0487 (12) | 0.0280 (10) | −0.0153 (10) | −0.0091 (9) | −0.0074 (8) |
O13 | 0.0490 (13) | 0.0228 (9) | 0.0407 (11) | −0.0121 (9) | 0.0034 (10) | −0.0057 (8) |
O21 | 0.0530 (14) | 0.0619 (14) | 0.0308 (11) | −0.0298 (12) | 0.0070 (10) | −0.0162 (10) |
O22 | 0.0444 (14) | 0.0289 (11) | 0.0783 (17) | −0.0036 (10) | 0.0116 (13) | −0.0079 (11) |
O23 | 0.0430 (13) | 0.0613 (14) | 0.0668 (15) | −0.0352 (13) | 0.0151 (12) | −0.0171 (12) |
O31 | 0.0365 (13) | 0.0331 (11) | 0.0518 (12) | 0.0043 (10) | −0.0142 (11) | −0.0065 (9) |
O32 | 0.0307 (11) | 0.0401 (11) | 0.0608 (13) | −0.0194 (10) | 0.0012 (10) | −0.0160 (10) |
O33 | 0.0519 (14) | 0.0418 (11) | 0.0237 (10) | −0.0049 (10) | 0.0005 (9) | −0.0063 (8) |
C1 | 0.0215 (12) | 0.0194 (10) | 0.0228 (11) | −0.0100 (10) | −0.0017 (10) | −0.0015 (9) |
C2 | 0.0225 (12) | 0.0200 (11) | 0.0222 (11) | −0.0094 (10) | −0.0007 (10) | −0.0025 (9) |
C11 | 0.0259 (14) | 0.0203 (11) | 0.0304 (12) | −0.0067 (10) | −0.0008 (11) | −0.0025 (9) |
C12 | 0.0249 (13) | 0.0254 (12) | 0.0324 (13) | −0.0097 (11) | 0.0016 (11) | −0.0069 (10) |
C13 | 0.0322 (14) | 0.0289 (13) | 0.0255 (12) | −0.0154 (12) | 0.0047 (11) | −0.0064 (10) |
C21 | 0.0312 (15) | 0.0354 (14) | 0.0340 (14) | −0.0162 (12) | 0.0111 (12) | −0.0120 (11) |
C22 | 0.0285 (15) | 0.0282 (13) | 0.0403 (14) | −0.0086 (12) | 0.0088 (12) | −0.0090 (11) |
C23 | 0.0272 (14) | 0.0347 (14) | 0.0343 (13) | −0.0121 (12) | 0.0054 (12) | −0.0094 (11) |
C31 | 0.0313 (15) | 0.0318 (14) | 0.0328 (13) | −0.0107 (13) | −0.0032 (12) | −0.0098 (11) |
C32 | 0.0213 (13) | 0.0277 (12) | 0.0316 (13) | −0.0036 (11) | −0.0046 (11) | −0.0066 (10) |
C33 | 0.0284 (14) | 0.0256 (12) | 0.0297 (13) | −0.0068 (11) | −0.0035 (11) | −0.0035 (10) |
C111 | 0.0290 (14) | 0.0209 (11) | 0.0338 (13) | −0.0087 (11) | 0.0013 (11) | −0.0028 (10) |
C112 | 0.0391 (17) | 0.0367 (15) | 0.0532 (17) | −0.0202 (14) | −0.0076 (14) | −0.0079 (13) |
C113 | 0.080 (3) | 0.0470 (18) | 0.0448 (17) | −0.0416 (19) | 0.0207 (17) | −0.0104 (14) |
C121 | 0.0243 (14) | 0.0346 (13) | 0.0262 (12) | −0.0107 (12) | 0.0038 (11) | −0.0123 (10) |
C122 | 0.0333 (16) | 0.0401 (15) | 0.0379 (15) | −0.0064 (13) | 0.0069 (13) | −0.0184 (12) |
C123 | 0.0327 (15) | 0.0424 (15) | 0.0231 (12) | −0.0146 (13) | 0.0036 (11) | −0.0031 (11) |
C131 | 0.0255 (14) | 0.0233 (12) | 0.0282 (12) | −0.0079 (11) | −0.0029 (11) | −0.0019 (10) |
C132 | 0.0257 (15) | 0.0396 (15) | 0.0474 (16) | −0.0071 (13) | −0.0025 (13) | −0.0102 (13) |
C133 | 0.0384 (17) | 0.0458 (16) | 0.0283 (13) | −0.0124 (14) | −0.0061 (12) | −0.0067 (12) |
Ru1—C13 | 1.903 (3) | O32—C32 | 1.132 (3) |
Ru1—C12 | 1.910 (3) | O33—C33 | 1.132 (3) |
Ru1—C11 | 1.938 (3) | C1—C2 | 1.299 (3) |
Ru1—C1 | 2.206 (2) | C111—C112 | 1.526 (4) |
Ru1—C2 | 2.322 (2) | C111—C113 | 1.531 (4) |
Ru1—Ru2 | 2.7907 (5) | C111—H1 | 1.01 (3) |
Ru1—Ru3 | 2.8010 (5) | C112—H11A | 0.98 |
Ru1—H | 1.81 (3) | C112—H11B | 0.98 |
Ru2—C23 | 1.907 (3) | C112—H11C | 0.98 |
Ru2—C21 | 1.909 (3) | C113—H11D | 0.98 |
Ru2—C22 | 1.924 (3) | C113—H11E | 0.98 |
Ru2—C1 | 1.958 (2) | C113—H11F | 0.98 |
Ru2—Ru3 | 2.7957 (5) | C121—C123 | 1.526 (4) |
Ru3—C32 | 1.904 (3) | C121—C122 | 1.541 (4) |
Ru3—C31 | 1.907 (3) | C121—H2 | 0.89 (3) |
Ru3—C33 | 1.942 (3) | C122—H12A | 0.98 |
Ru3—C1 | 2.215 (2) | C122—H12B | 0.98 |
Ru3—C2 | 2.302 (3) | C122—H12C | 0.98 |
Ru3—H | 1.77 (3) | C123—H12D | 0.98 |
Si—C2 | 1.881 (3) | C123—H12E | 0.98 |
Si—C121 | 1.884 (3) | C123—H12F | 0.98 |
Si—C131 | 1.887 (3) | C131—C133 | 1.529 (4) |
Si—C111 | 1.890 (3) | C131—C132 | 1.541 (4) |
O11—C11 | 1.129 (3) | C131—H3 | 0.91 (3) |
O12—C12 | 1.135 (3) | C132—H13A | 0.98 |
O13—C13 | 1.135 (3) | C132—H13B | 0.98 |
O21—C21 | 1.137 (4) | C132—H13C | 0.98 |
O22—C22 | 1.135 (4) | C133—H13D | 0.98 |
O23—C23 | 1.130 (3) | C133—H13E | 0.98 |
O31—C31 | 1.132 (3) | C133—H13F | 0.98 |
C13—Ru1—C12 | 91.98 (11) | C131—Si—C111 | 115.77 (12) |
C13—Ru1—C11 | 97.34 (10) | C2—C1—Ru2 | 156.06 (19) |
C12—Ru1—C11 | 92.96 (11) | C2—C1—Ru1 | 78.27 (14) |
C13—Ru1—C1 | 131.25 (10) | Ru2—C1—Ru1 | 83.93 (9) |
C12—Ru1—C1 | 93.10 (9) | C2—C1—Ru3 | 77.04 (15) |
C11—Ru1—C1 | 130.70 (9) | Ru2—C1—Ru3 | 83.90 (9) |
C13—Ru1—C2 | 158.26 (10) | Ru1—C1—Ru3 | 78.63 (8) |
C12—Ru1—C2 | 102.52 (9) | C1—C2—Si | 145.28 (19) |
C11—Ru1—C2 | 97.98 (9) | C1—C2—Ru3 | 69.62 (15) |
C1—Ru1—C2 | 33.21 (9) | Si—C2—Ru3 | 135.36 (12) |
C13—Ru1—Ru2 | 87.27 (8) | C1—C2—Ru1 | 68.52 (13) |
C12—Ru1—Ru2 | 90.70 (8) | Si—C2—Ru1 | 133.19 (12) |
C11—Ru1—Ru2 | 174.00 (7) | Ru3—C2—Ru1 | 74.57 (7) |
C1—Ru1—Ru2 | 44.24 (6) | O11—C11—Ru1 | 174.7 (2) |
C2—Ru1—Ru2 | 76.57 (6) | O12—C12—Ru1 | 178.4 (2) |
C13—Ru1—Ru3 | 106.84 (8) | O13—C13—Ru1 | 176.6 (2) |
C12—Ru1—Ru3 | 143.33 (7) | O21—C21—Ru2 | 179.3 (3) |
C11—Ru1—Ru3 | 114.73 (8) | O22—C22—Ru2 | 177.5 (3) |
C1—Ru1—Ru3 | 50.82 (6) | O23—C23—Ru2 | 178.2 (3) |
C2—Ru1—Ru3 | 52.40 (6) | O31—C31—Ru3 | 177.9 (3) |
Ru2—Ru1—Ru3 | 60.00 (1) | O32—C32—Ru3 | 178.9 (2) |
C13—Ru1—H | 82.3 (10) | O33—C33—Ru3 | 175.2 (2) |
C12—Ru1—H | 173.8 (10) | C112—C111—C113 | 108.9 (3) |
C11—Ru1—H | 90.2 (10) | C112—C111—Si | 111.45 (19) |
C1—Ru1—H | 88.8 (10) | C113—C111—Si | 114.93 (18) |
C2—Ru1—H | 82.3 (10) | C112—C111—H1 | 110.9 (17) |
Ru2—Ru1—H | 86.6 (10) | C113—C111—H1 | 106.2 (17) |
Ru3—Ru1—H | 38.0 (10) | Si—C111—H1 | 104.3 (17) |
C23—Ru2—C21 | 96.49 (11) | C111—C112—H11A | 109.5 |
C23—Ru2—C22 | 94.79 (12) | C111—C112—H11B | 109.5 |
C21—Ru2—C22 | 94.22 (12) | H11A—C112—H11B | 109.5 |
C23—Ru2—C1 | 105.17 (11) | C111—C112—H11C | 109.5 |
C21—Ru2—C1 | 107.35 (11) | H11A—C112—H11C | 109.5 |
C22—Ru2—C1 | 148.34 (10) | H11B—C112—H11C | 109.5 |
C23—Ru2—Ru1 | 155.30 (8) | C111—C113—H11D | 109.5 |
C21—Ru2—Ru1 | 99.28 (8) | C111—C113—H11E | 109.5 |
C22—Ru2—Ru1 | 102.83 (8) | H11D—C113—H11E | 109.5 |
C1—Ru2—Ru1 | 51.83 (7) | C111—C113—H11F | 109.5 |
C23—Ru2—Ru3 | 99.77 (8) | H11D—C113—H11F | 109.5 |
C21—Ru2—Ru3 | 156.55 (9) | H11E—C113—H11F | 109.5 |
C22—Ru2—Ru3 | 101.10 (8) | C123—C121—C122 | 110.4 (2) |
C1—Ru2—Ru3 | 51.97 (7) | C123—C121—Si | 114.58 (17) |
Ru1—Ru2—Ru3 | 60.184 (11) | C122—C121—Si | 112.9 (2) |
C32—Ru3—C31 | 92.18 (12) | C123—C121—H2 | 111.4 (18) |
C32—Ru3—C33 | 93.73 (11) | C122—C121—H2 | 103.5 (18) |
C31—Ru3—C33 | 97.38 (11) | Si—C121—H2 | 103.3 (17) |
C32—Ru3—C1 | 92.66 (10) | C121—C122—H12A | 109.5 |
C31—Ru3—C1 | 131.43 (10) | C121—C122—H12B | 109.5 |
C33—Ru3—C1 | 130.41 (10) | H12A—C122—H12B | 109.5 |
C32—Ru3—C2 | 100.62 (10) | C121—C122—H12C | 109.5 |
C31—Ru3—C2 | 159.80 (9) | H12A—C122—H12C | 109.5 |
C33—Ru3—C2 | 97.31 (10) | H12B—C122—H12C | 109.5 |
C1—Ru3—C2 | 33.35 (8) | C121—C123—H12D | 109.5 |
C32—Ru3—Ru2 | 91.37 (8) | C121—C123—H12E | 109.5 |
C31—Ru3—Ru2 | 87.46 (8) | H12D—C123—H12E | 109.5 |
C33—Ru3—Ru2 | 172.82 (8) | C121—C123—H12F | 109.5 |
C1—Ru3—Ru2 | 44.13 (6) | H12D—C123—H12F | 109.5 |
C2—Ru3—Ru2 | 76.76 (6) | H12E—C123—H12F | 109.5 |
C32—Ru3—Ru1 | 142.85 (8) | C133—C131—C132 | 110.1 (2) |
C31—Ru3—Ru1 | 108.03 (8) | C133—C131—Si | 112.84 (19) |
C33—Ru3—Ru1 | 113.41 (8) | C132—C131—Si | 115.44 (18) |
C1—Ru3—Ru1 | 50.56 (6) | C133—C131—H3 | 107.0 (18) |
C2—Ru3—Ru1 | 53.03 (6) | C132—C131—H3 | 108.8 (19) |
Ru2—Ru3—Ru1 | 59.82 (2) | Si—C131—H3 | 102.0 (19) |
C32—Ru3—H | 175.0 (11) | C131—C132—H13A | 109.5 |
C31—Ru3—H | 83.0 (11) | C131—C132—H13B | 109.5 |
C33—Ru3—H | 88.2 (10) | H13A—C132—H13B | 109.5 |
C1—Ru3—H | 89.6 (10) | C131—C132—H13C | 109.5 |
C2—Ru3—H | 83.7 (11) | H13A—C132—H13C | 109.5 |
Ru1—H—Ru3 | 102.2 (16) | H13B—C132—H13C | 109.5 |
Ru2—Ru3—H | 87.2 (10) | C131—C133—H13D | 109.5 |
Ru1—Ru3—H | 39.1 (10) | C131—C133—H13E | 109.5 |
C2—Si—C121 | 109.32 (11) | H13D—C133—H13E | 109.5 |
C2—Si—C131 | 103.97 (11) | C131—C133—H13F | 109.5 |
C121—Si—C131 | 113.07 (12) | H13D—C133—H13F | 109.5 |
C2—Si—C111 | 106.81 (11) | H13E—C133—H13F | 109.5 |
C121—Si—C111 | 107.56 (11) |
Experimental details
Crystal data | |
Chemical formula | [Ru3(C11H22Si)(CO)9] |
Mr | 737.68 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 160 |
a, b, c (Å) | 9.3592 (13), 11.8691 (18), 12.6669 (17) |
α, β, γ (°) | 79.393 (17), 87.314 (17), 68.106 (16) |
V (Å3) | 1282.9 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.83 |
Crystal size (mm) | 0.4 × 0.35 × 0.2 |
Data collection | |
Diffractometer | Stoe IPDS |
Absorption correction | Multi-scan (Blessing, 1995) |
Tmin, Tmax | 0.342, 0.463 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12223, 4546, 4456 |
Rint | 0.028 |
(sin θ/λ)max (Å−1) | 0.618 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.020, 0.054, 1.13 |
No. of reflections | 4546 |
No. of parameters | 320 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.37, −0.40 |
Computer programs: IPDS Software (Stoe, 1996), IPDS Software, X-RED (Stoe, 1996), SIR92 (Altomare et al., 1994) in WjnGX (Farrugia, 1999), SHELXL97 (Sheldrick, 1997) in WinGX, ORTEP-3 for Windows (Farrugia, 1997) in WinGX, SHELXL97 in WinGX.
Ru1—C1 | 2.206 (2) | Ru2—Ru3 | 2.7957 (5) |
Ru1—C2 | 2.322 (2) | Ru3—C1 | 2.215 (2) |
Ru1—Ru2 | 2.7907 (5) | Ru3—C2 | 2.302 (3) |
Ru1—Ru3 | 2.8010 (5) | Ru3—H | 1.77 (3) |
Ru1—H | 1.81 (3) | Si—C2 | 1.881 (3) |
Ru2—C1 | 1.958 (2) | C1—C2 | 1.299 (3) |
Ru2—Ru1—Ru3 | 60.00 (1) | C2—C1—Ru2 | 156.06 (19) |
Ru1—Ru2—Ru3 | 60.184 (11) | Ru1—C1—Ru3 | 78.63 (8) |
Ru2—Ru3—Ru1 | 59.82 (2) | C1—C2—Si | 145.28 (19) |
Ru1—H—Ru3 | 102.2 (16) | Ru3—C2—Ru1 | 74.57 (7) |
Acetylide compounds are being widely studied because of the versatile coordination modes of the unsaturated fragments which act as metalloligands (Ara et al., 1995). Researchers are also interested in cluster chemistry containing C2R groups regarding their implications in the syntheses of organic molecules that take place on metal surfaces (Chi et al., 1997). More recently the acetylide derivatives have been used as precursors to synthesize polymetallic compounds bearing unsaturated polycarbon chains (Alcalde et al., 2001). Herein we report the structure of the new compound [Ru3(CO)9(µ-H)(µ3-C2SiiPr3)], (I). The ν(CO) pattern in the carbonyl region as well as the 1H NMR resonance for hydride observed in the spectra are in agreement with data reported on analogous compounds (Sappa et al., 1972; Edwards et al., 1995).
The title compound consists of a triangular ruthenium cluster (see Fig. 1). The Ru—Ru distances [Ru1—Ru3 2.8010 (9), Ru1—Ru2 2.7907 (13) and Ru2—Ru3 2.7957 (11) Å] are similar to those reported for other compounds of this type. [Ru3(CO)9(µ-H)(µ3-C2R)] [R= H [2.792 (1), 2.803 (1), 2.810 (1) Å (Bruce et al., 1999); tBu [2.790 (2), 2.795 (2), 2.796 (2) Å (Gervasio & Ferraris, 1973)]. The three ruthenium atoms in all of these compounds form an almost equilateral triangle. In (I) the acetylide ligand is σ-bonded to one Ru atom [Ru2—C1 1.958 (2) Å] and π-bonded to the other two Ru atoms [Ru3—C1 2.215 (2), Ru1—C1 2.206 (2), Ru3—C2 2.302 (3) and Ru1—C2 2.322 (2) Å]. The acetylide group is acting as 5 e- donor, the C1—C2 distance [1.299 (3) Å] being comparable to that in other acetylide clusters [Ru3(CO)9(µ-H)(µ3-C2R)][R= H [1.28 (1) Å (Bruce et al., 1999)]; t Bu [1.29 (3) Å (Gervasio & Ferraris, 1973)]. The hydride is unsymmetrically located between atoms Ru1 and Ru3 giving Ru—H distances of 1.81 (3) and 1.77 (3) Å (see Table 1.). Three terminal CO ligands around each metal atom complete the structure.