Octa­carbonyldi-μ2-hydrido-[μ3-(1,3,5-trimethyl­phen­yl)phosphinidene](tri­phenyl­phosphane)-triangulo-triruthenium

Kakizawa, T.

doi:10.1107/S1600536812039499

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 68| Part 10| October 2012| Page m1293

https://doi.org/10.1107/S1600536812039499

Open

access

Octacarbonyldi-μ₂-hydrido-[μ₃-(1,3,5-trimethylphenyl)phosphinidene](triphenylphosphane)-triangulo-triruthenium

Taeko Kakizawa ^a ^*

^aAcademic Support Center, Kogakuin University, 1-24-2 Nishi-shinjuku, Shinjuku-ku, Tokyo 163-8677, Japan
^*Correspondence e-mail: kt13385@ns.kogakuin.ac.jp

(Received 6 September 2012; accepted 17 September 2012; online 22 September 2012)

In the crystal structure of the title compound, [Ru₃(C₉H₁₁P)H₂(C₁₈H₁₅P)(CO)₈], the triangular Ru₃ unit is capped with one mesitylphosphinidene ligand. In the trigonal–pyramidal Ru₃P core, one Ru^II atom is coordinated by a triphenylphosphane ligand in a terminal fashion. Two hydride ligands bridge over two Ru—Ru bonds. These Ru—Ru bonds [2.9400 (4) and 2.9432 (4) Å] are slightly longer than the nonhydride-bridged Ru—Ru bond [2.8146 (4) Å]. The terminal triphenylphosphane ligand coordinates to the Ru^II atom, which is involved in two hydride bridges.

Related literature

For related literature, see: Kakizawa et al. (2006 ); Frediani et al. (1997 ).

Experimental

Crystal data

[Ru₃(C₉H₁₁P)H₂(C₁₈H₁₅P)(CO)₈]
M_r = 941.72
Triclinic, $[P \overline 1]$
a = 11.5954 (5) Å
b = 12.0870 (7) Å
c = 13.4304 (1) Å
α = 100.224 (2)°
β = 94.6231 (17)°
γ = 95.0167 (13)°
V = 1836.44 (13) Å³
Z = 2
Mo Kα radiation
μ = 1.35 mm⁻¹
T = 150 K
0.30 × 0.30 × 0.03 mm

Data collection

Rigaku R-AXIS RAPID imaging plate diffractometer
Absorption correction: integration (NUMABS; Higashi, 1999 ) T_min = 0.687, T_max = 0.961
17157 measured reflections
8304 independent reflections
7671 reflections with I > 2σ(I)
R_int = 0.035

Refinement

R[F² > 2σ(F²)] = 0.030
wR(F²) = 0.118
S = 1.23
8304 reflections
444 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.74 e Å⁻³
Δρ_min = −1.79 e Å⁻³

Table 1
Selected bond lengths (Å)

Ru1—P1	2.3351 (10)
Ru1—P2	2.3896 (9)
Ru2—P1	2.3143 (10)
Ru3—P1	2.3285 (9)

Data collection: PROCESS-AUTO (Rigaku, 1998 ); cell refinement: PROCESS-AUTO; data reduction: TEXSAN (Molecular Structure Corporation & Rigaku, 2000 ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536812039499/nc2293sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812039499/nc2293Isup2.hkl

checkCIF report

Comment top

Previously, we reported the crystal structure of a mesitylphosphinidene-capped triruthenium cluster having a terminal phosphane ligand [Ru₃(CO)₈(PH₂Mes)(µ-H)₂(µ₃-PMes)] (Kakizawa et al., 2006). Here we report an additional structure of this type of compound prepared by photo-irradiation of the toluene solution containing [Ru₃(CO)₉(µ-H)₂(µ₃-PMes)] (Kakizawa et al., 2006) and PPh₃. The geometry of the title compound is similar to those of the related clusters [Ru₃(CO)₈(PH₂Mes)(µ-H)₂(µ₃-PMes)] and [Ru₃(CO)₈(PPh₃)(µ-H)₂(µ₃-PPh)] (Frediani et al., 1997) (Fig. 1). In the trigonal pyramidal Ru₃P core, one Ru atom is co-ordinated by a terminal PPh₃ ligand. Two hydrido ligands bridge over the Ru(1)–Ru(2) and Ru(1)–Ru(3) bonds. These Ru–Ru bonds (Ru(1)–Ru(2) 2.9400 (4) Å and Ru(1)–Ru(3) 2.9432 (4) Å) are slightly longer than the Ru(2)–Ru(3) bond (2.8146 (4) Å), which has no bridging hydrogen. The existence of two bridging hydrogen atoms was confirmed by the ¹H NMR spectrum. A signal was observed at -18.32 ppm as a doublet of doublet owing to the coupling with the phosphorus atoms of the µ₃-PMes (J_PH = 9.0 Hz) and PPh₃ (J_PH = 15.0 Hz) ligands. The ³¹P NMR spectrum shows the signals of µ₃-PMes and PPh₃ ligands at a low field (231.3 ppm) and a moderately high field (34.7 ppm), respectively.

Related literature top

For related literature, see: Kakizawa et al. (2006); Frediani et al. (1997).

Experimental top

All reactions were performed under a dry nitrogen atmosphere or a high vacuum. Toluene and hexane were distilled from sodium-benzophenone ketyl just before use. A toluene solution (2 ml) of [Ru₃(CO)₉(µ-H)₂(µ₃-PMes)] (25 mg, 0.035 mmol) and PPh₃ (10 mg, 0.038 mmol) was photolysed for 3 h with a 450 W medium pressure Hg arc lamp with stirring at 6°C. During the photo-irradiation, the evolved CO in the reaction vessel was removed by freeze-pump-thaw cycles every 1 h. After the photolysis, the solvent was filtered and evaporated to dryness under a high vacuum. Recrystallization of the residue from hexane at -30°C gave the title compound (29 mg, 0.031 mmol, 88%) as yellow platelets.

Spectral data for the title compound: ¹H NMR (300 MHz, CD₂Cl₂): δ -18.32 (dd, 2H, J_PH = 9.0 Hz, J_PH = 15.0 Hz, µ-H), 2.32 (s, 3H, p-CH₃), 2.77 (s, 6H, o-CH₃), 7.04 (s, 2H, ArH), 7.43–7.47 (m, 15H, PPh). ³¹P NMR (121.5 MHz, CD₂Cl₂): δ 34.7 (dt, J_PP = 116.6 Hz, J_PH = 15.0 Hz, PPh₃), 231.3 (dt, J_PP = 116.6 Hz, J_PH = 9.0 Hz, PMes). IR νCO (KBr, cm^-1): 2071 (s), 2029 (vs), 2012 (s), 1988 (s), 1968 (s), 1965 (s). Anal. Calcd for C₃₅H₂₈O₈P₂Ru₃: C, 44.64; H 3.00. Found: C, 45.02; H, 3.29.

Structure description top

For related literature, see: Kakizawa et al. (2006); Frediani et al. (1997).

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: TEXSAN (Molecular Structure Corporation & Rigaku, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. A molecular structure of the title compound, with atom labels and 50% probability displacement ellipsoids for non-H atoms.

Octacarbonyldi-µ₂-hydrido-[µ₃-(1,3,5- trimethylphenyl)phosphinidene](triphenylphosphane)-triangulo- triruthenium top

Crystal data top

[Ru₃(C₉H₁₁P)H₂(C₁₈H₁₅P)(CO)₈]	Z = 2
M_r = 941.72	F(000) = 928
Triclinic, P1	D_x = 1.703 Mg m⁻³
a = 11.5954 (5) Å	Mo Kα radiation, λ = 0.71069 Å
b = 12.0870 (7) Å	Cell parameters from 17157 reflections
c = 13.4304 (1) Å	θ = 1.6–27.5°
α = 100.224 (2)°	µ = 1.35 mm⁻¹
β = 94.6231 (17)°	T = 150 K
γ = 95.0167 (13)°	Platelet, yellow
V = 1836.44 (13) Å³	0.30 × 0.30 × 0.03 mm

Data collection top

Rigaku R-AXIS RAPID imaging plate diffractometer	8304 independent reflections
Radiation source: rotation-anode X-ray tube	7671 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.035
ω scans	θ_max = 27.5°, θ_min = 1.6°
Absorption correction: integration (NUMABS; Higashi, 1999)	h = −15→15
T_min = 0.687, T_max = 0.961	k = −15→15
17157 measured reflections	l = −17→17

Refinement top

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)] = 0.030	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.118	H atoms treated by a mixture of independent and constrained refinement
S = 1.23	w = 1/[σ²(F_o²) + (0.0542P)² + 4.2474P] where P = (F_o² + 2F_c²)/3
8304 reflections	(Δ/σ)_max = 0.001
444 parameters	Δρ_max = 0.74 e Å⁻³
0 restraints	Δρ_min = −1.79 e Å⁻³

Crystal data top

[Ru₃(C₉H₁₁P)H₂(C₁₈H₁₅P)(CO)₈]	γ = 95.0167 (13)°
M_r = 941.72	V = 1836.44 (13) Å³
Triclinic, P1	Z = 2
a = 11.5954 (5) Å	Mo Kα radiation
b = 12.0870 (7) Å	µ = 1.35 mm⁻¹
c = 13.4304 (1) Å	T = 150 K
α = 100.224 (2)°	0.30 × 0.30 × 0.03 mm
β = 94.6231 (17)°

Data collection top

Rigaku R-AXIS RAPID imaging plate diffractometer	8304 independent reflections
Absorption correction: integration (NUMABS; Higashi, 1999)	7671 reflections with I > 2σ(I)
T_min = 0.687, T_max = 0.961	R_int = 0.035
17157 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.030	0 restraints
wR(F²) = 0.118	H atoms treated by a mixture of independent and constrained refinement
S = 1.23	Δρ_max = 0.74 e Å⁻³
8304 reflections	Δρ_min = −1.79 e Å⁻³
444 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.

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

	x	y	z	U_iso*/U_eq
Ru1	0.77644 (2)	−0.14550 (2)	0.79228 (2)	0.02048 (9)
Ru2	0.59156 (3)	−0.33293 (3)	0.77256 (2)	0.02512 (9)
H1	0.630 (5)	−0.189 (5)	0.822 (4)	0.043 (14)*
Ru3	0.69300 (3)	−0.29398 (2)	0.59681 (2)	0.02434 (9)
H2	0.716 (4)	−0.161 (4)	0.664 (4)	0.033 (12)*
P1	0.78483 (8)	−0.33959 (8)	0.74261 (7)	0.02228 (18)
P2	0.70618 (8)	0.03502 (8)	0.79537 (7)	0.02088 (18)
C1	0.8183 (3)	−0.1288 (3)	0.9340 (3)	0.0269 (7)
C2	0.9265 (4)	−0.0988 (3)	0.7631 (3)	0.0306 (8)
C3	0.4408 (4)	−0.2860 (4)	0.7289 (3)	0.0320 (8)
C4	0.5779 (4)	−0.3404 (4)	0.9132 (3)	0.0373 (9)
C5	0.5459 (4)	−0.4889 (4)	0.7237 (4)	0.0399 (10)
C6	0.5554 (4)	−0.2355 (4)	0.5397 (3)	0.0333 (9)
C7	0.6632 (4)	−0.4441 (4)	0.5244 (3)	0.0388 (10)
C8	0.8053 (4)	−0.2472 (3)	0.5106 (3)	0.0312 (8)
C9	0.8942 (3)	−0.4344 (3)	0.7652 (3)	0.0252 (7)
C10	0.8906 (4)	−0.4926 (3)	0.8485 (3)	0.0309 (8)
C11	0.9668 (4)	−0.5748 (4)	0.8567 (3)	0.0383 (10)
H3	0.9637	−0.6136	0.9121	0.046*
C12	1.0461 (5)	−0.6016 (4)	0.7874 (3)	0.0436 (12)
C13	1.0541 (4)	−0.5387 (4)	0.7105 (3)	0.0365 (10)
H4	1.1113	−0.5533	0.6645	0.044*
C14	0.9812 (4)	−0.4547 (3)	0.6983 (3)	0.0287 (8)
C15	0.8073 (4)	−0.4711 (4)	0.9287 (3)	0.0388 (10)
H5	0.7298	−0.5082	0.9015	0.058*
H6	0.8035	−0.3895	0.9485	0.058*
H7	0.8345	−0.5016	0.9883	0.058*
C16	1.1215 (7)	−0.6964 (6)	0.7961 (4)	0.070 (2)
H8	1.1234	−0.7125	0.8652	0.105*
H9	1.2006	−0.6737	0.7815	0.105*
H10	1.0891	−0.7643	0.7473	0.105*
C17	1.0015 (4)	−0.3878 (4)	0.6151 (4)	0.0399 (10)
H11	1.0771	−0.4012	0.5900	0.060*
H12	1.0008	−0.3071	0.6422	0.060*
H13	0.9398	−0.4118	0.5591	0.060*
C18	0.5479 (3)	0.0334 (3)	0.7800 (3)	0.0245 (7)
C19	0.4915 (4)	0.0726 (5)	0.7008 (4)	0.0465 (12)
H14	0.5344	0.0993	0.6509	0.056*
C20	0.3700 (5)	0.0723 (7)	0.6947 (5)	0.069 (2)
H15	0.3306	0.0990	0.6403	0.082*
C21	0.3075 (4)	0.0338 (5)	0.7670 (5)	0.0525 (13)
H16	0.2255	0.0356	0.7631	0.063*
C22	0.3638 (4)	−0.0074 (4)	0.8449 (4)	0.0392 (10)
H17	0.3205	−0.0349	0.8941	0.047*
C23	0.4834 (4)	−0.0085 (4)	0.8511 (3)	0.0315 (8)
H18	0.5218	−0.0380	0.9043	0.038*
C24	0.7488 (3)	0.1366 (3)	0.9136 (3)	0.0232 (7)
C25	0.6732 (4)	0.2097 (3)	0.9588 (3)	0.0291 (8)
H19	0.5957	0.2066	0.9288	0.035*
C26	0.7109 (4)	0.2871 (4)	1.0476 (3)	0.0328 (9)
H20	0.6588	0.3362	1.0782	0.039*
C27	0.8236 (4)	0.2928 (4)	1.0915 (3)	0.0347 (9)
H21	0.8484	0.3448	1.1529	0.042*
C28	0.9002 (4)	0.2232 (4)	1.0466 (3)	0.0343 (9)
H22	0.9783	0.2286	1.0759	0.041*
C29	0.8631 (4)	0.1449 (3)	0.9579 (3)	0.0300 (8)
H23	0.9160	0.0967	0.9273	0.036*
C30	0.7549 (3)	0.1124 (3)	0.6979 (3)	0.0267 (7)
C31	0.7476 (5)	0.2290 (4)	0.7098 (3)	0.0388 (10)
H24	0.7217	0.2689	0.7700	0.047*
C32	0.7785 (5)	0.2863 (4)	0.6328 (4)	0.0466 (12)
H25	0.7731	0.3653	0.6408	0.056*
C33	0.8165 (5)	0.2301 (5)	0.5459 (4)	0.0471 (12)
H26	0.8354	0.2698	0.4934	0.056*
C34	0.8274 (6)	0.1174 (5)	0.5346 (4)	0.0604 (16)
H27	0.8553	0.0788	0.4748	0.072*
C35	0.7975 (5)	0.0585 (4)	0.6113 (4)	0.0491 (13)
H28	0.8067	−0.0198	0.6035	0.059*
O1	0.8423 (3)	−0.1182 (3)	1.0195 (2)	0.0401 (7)
O2	1.0180 (3)	−0.0709 (3)	0.7446 (3)	0.0548 (10)
O3	0.3513 (3)	−0.2646 (3)	0.7010 (3)	0.0446 (8)
O4	0.5720 (3)	−0.3418 (4)	0.9975 (3)	0.0570 (10)
O5	0.5191 (4)	−0.5828 (3)	0.6956 (3)	0.0588 (10)
O6	0.4761 (3)	−0.2000 (3)	0.5072 (3)	0.0483 (9)
O7	0.6459 (4)	−0.5347 (3)	0.4812 (3)	0.0559 (10)
O8	0.8706 (3)	−0.2151 (3)	0.4616 (3)	0.0486 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ru1	0.02143 (15)	0.02131 (15)	0.01840 (14)	0.00346 (11)	0.00047 (10)	0.00297 (10)
Ru2	0.02299 (16)	0.02734 (16)	0.02496 (16)	0.00086 (12)	0.00005 (11)	0.00655 (11)
Ru3	0.02974 (17)	0.02460 (16)	0.01801 (14)	0.00426 (12)	−0.00216 (11)	0.00352 (11)
P1	0.0253 (5)	0.0222 (4)	0.0197 (4)	0.0046 (3)	0.0004 (3)	0.0047 (3)
P2	0.0216 (4)	0.0220 (4)	0.0188 (4)	0.0031 (3)	0.0011 (3)	0.0035 (3)
C1	0.0270 (18)	0.0274 (18)	0.0261 (18)	0.0083 (14)	0.0008 (14)	0.0028 (14)
C2	0.030 (2)	0.0299 (19)	0.0289 (19)	0.0016 (16)	0.0012 (15)	−0.0014 (15)
C3	0.030 (2)	0.035 (2)	0.0291 (19)	−0.0013 (16)	0.0006 (16)	0.0037 (16)
C4	0.030 (2)	0.050 (3)	0.036 (2)	0.0110 (19)	0.0062 (17)	0.0142 (19)
C5	0.038 (2)	0.043 (3)	0.040 (2)	0.0051 (19)	0.0022 (19)	0.0110 (19)
C6	0.040 (2)	0.033 (2)	0.0247 (18)	0.0009 (17)	−0.0045 (16)	0.0056 (16)
C7	0.051 (3)	0.039 (2)	0.027 (2)	0.012 (2)	−0.0044 (18)	0.0065 (17)
C8	0.041 (2)	0.031 (2)	0.0216 (17)	0.0076 (17)	0.0027 (16)	0.0046 (15)
C9	0.0301 (19)	0.0206 (16)	0.0244 (17)	0.0054 (14)	−0.0020 (14)	0.0034 (13)
C10	0.042 (2)	0.0249 (18)	0.0246 (18)	0.0067 (16)	−0.0060 (16)	0.0032 (14)
C11	0.054 (3)	0.032 (2)	0.030 (2)	0.0129 (19)	−0.0071 (19)	0.0073 (17)
C12	0.064 (3)	0.036 (2)	0.031 (2)	0.026 (2)	−0.006 (2)	−0.0003 (17)
C13	0.044 (2)	0.037 (2)	0.0274 (19)	0.0190 (19)	0.0018 (17)	−0.0020 (16)
C14	0.037 (2)	0.0245 (18)	0.0236 (17)	0.0073 (15)	−0.0010 (15)	0.0002 (14)
C15	0.045 (3)	0.048 (3)	0.029 (2)	0.010 (2)	0.0042 (18)	0.0197 (19)
C16	0.113 (6)	0.066 (4)	0.041 (3)	0.064 (4)	0.008 (3)	0.012 (3)
C17	0.048 (3)	0.040 (2)	0.040 (2)	0.021 (2)	0.019 (2)	0.0162 (19)
C18	0.0194 (16)	0.0239 (17)	0.0281 (18)	−0.0018 (13)	−0.0012 (13)	0.0028 (14)
C19	0.025 (2)	0.072 (3)	0.049 (3)	−0.003 (2)	−0.0046 (19)	0.033 (3)
C20	0.029 (3)	0.110 (5)	0.077 (4)	0.002 (3)	−0.012 (3)	0.056 (4)
C21	0.021 (2)	0.066 (3)	0.073 (4)	0.001 (2)	0.001 (2)	0.024 (3)
C22	0.034 (2)	0.034 (2)	0.053 (3)	0.0044 (17)	0.018 (2)	0.0102 (19)
C23	0.029 (2)	0.032 (2)	0.035 (2)	0.0086 (16)	0.0071 (16)	0.0093 (16)
C24	0.0261 (18)	0.0209 (16)	0.0208 (16)	0.0001 (13)	−0.0009 (13)	0.0014 (13)
C25	0.0280 (19)	0.0314 (19)	0.0278 (18)	0.0081 (15)	0.0026 (15)	0.0029 (15)
C26	0.030 (2)	0.035 (2)	0.0297 (19)	0.0040 (16)	0.0047 (16)	−0.0042 (16)
C27	0.043 (2)	0.033 (2)	0.0244 (18)	0.0028 (18)	−0.0016 (16)	−0.0029 (15)
C28	0.032 (2)	0.031 (2)	0.035 (2)	0.0014 (16)	−0.0101 (17)	−0.0008 (16)
C29	0.031 (2)	0.0296 (19)	0.0283 (19)	0.0087 (16)	−0.0010 (15)	0.0005 (15)
C30	0.0261 (18)	0.0313 (19)	0.0236 (17)	0.0028 (15)	0.0017 (14)	0.0083 (14)
C31	0.056 (3)	0.032 (2)	0.028 (2)	0.0008 (19)	0.0010 (19)	0.0073 (16)
C32	0.064 (3)	0.033 (2)	0.041 (3)	−0.011 (2)	−0.006 (2)	0.0131 (19)
C33	0.052 (3)	0.049 (3)	0.043 (3)	−0.010 (2)	0.007 (2)	0.024 (2)
C34	0.092 (5)	0.050 (3)	0.045 (3)	0.003 (3)	0.035 (3)	0.014 (2)
C35	0.075 (4)	0.036 (2)	0.043 (3)	0.008 (2)	0.030 (3)	0.012 (2)
O1	0.0461 (18)	0.0520 (19)	0.0218 (14)	0.0159 (15)	−0.0035 (12)	0.0036 (13)
O2	0.0340 (18)	0.058 (2)	0.072 (3)	−0.0023 (16)	0.0197 (17)	0.0072 (19)
O3	0.0323 (17)	0.058 (2)	0.0420 (18)	0.0115 (15)	−0.0036 (14)	0.0047 (15)
O4	0.051 (2)	0.094 (3)	0.0355 (18)	0.025 (2)	0.0134 (16)	0.0244 (19)
O5	0.067 (3)	0.0280 (18)	0.074 (3)	−0.0083 (17)	−0.001 (2)	0.0006 (17)
O6	0.0413 (19)	0.062 (2)	0.0462 (19)	0.0120 (16)	−0.0067 (15)	0.0231 (17)
O7	0.085 (3)	0.0313 (18)	0.0424 (19)	0.0049 (18)	−0.0144 (19)	−0.0064 (14)
O8	0.059 (2)	0.053 (2)	0.0390 (18)	0.0099 (17)	0.0203 (16)	0.0140 (16)

Geometric parameters (Å, º) top

Ru1—C2	1.875 (4)	C15—H5	0.9800
Ru1—C1	1.897 (4)	C15—H6	0.9800
Ru1—P1	2.3351 (10)	C15—H7	0.9800
Ru1—P2	2.3896 (9)	C16—H8	0.9800
Ru1—Ru2	2.9400 (4)	C16—H9	0.9800
Ru1—Ru3	2.9432 (4)	C16—H10	0.9800
Ru1—H1	1.83 (5)	C17—H11	0.9800
Ru1—H2	1.78 (5)	C17—H12	0.9800
Ru2—C5	1.896 (5)	C17—H13	0.9800
Ru2—C4	1.925 (4)	C18—C19	1.381 (6)
Ru2—C3	1.962 (4)	C18—C23	1.396 (6)
Ru2—P1	2.3143 (10)	C19—C20	1.404 (7)
Ru2—Ru3	2.8146 (4)	C19—H14	0.9500
Ru2—H1	1.75 (5)	C20—C21	1.378 (8)
Ru3—C7	1.889 (5)	C20—H15	0.9500
Ru3—C8	1.925 (4)	C21—C22	1.378 (7)
Ru3—C6	1.956 (4)	C21—H16	0.9500
Ru3—P1	2.3285 (9)	C22—C23	1.384 (6)
Ru3—H2	1.68 (5)	C22—H17	0.9500
P1—C9	1.825 (4)	C23—H18	0.9500
P2—C18	1.828 (4)	C24—C25	1.395 (5)
P2—C24	1.830 (4)	C24—C29	1.396 (5)
P2—C30	1.835 (4)	C25—C26	1.392 (6)
C1—O1	1.141 (5)	C25—H19	0.9500
C2—O2	1.145 (6)	C26—C27	1.380 (6)
C3—O3	1.141 (5)	C26—H20	0.9500
C4—O4	1.143 (6)	C27—C28	1.377 (6)
C5—O5	1.138 (6)	C27—H21	0.9500
C6—O6	1.137 (5)	C28—C29	1.396 (5)
C7—O7	1.136 (6)	C28—H22	0.9500
C8—O8	1.130 (5)	C29—H23	0.9500
C9—C14	1.414 (6)	C30—C35	1.379 (6)
C9—C10	1.423 (5)	C30—C31	1.401 (6)
C10—C11	1.399 (6)	C31—C32	1.395 (6)
C10—C15	1.508 (6)	C31—H24	0.9500
C11—C12	1.378 (7)	C32—C33	1.368 (8)
C11—H3	0.9500	C32—H25	0.9500
C12—C13	1.391 (7)	C33—C34	1.362 (8)
C12—C16	1.516 (6)	C33—H26	0.9500
C13—C14	1.399 (6)	C34—C35	1.400 (7)
C13—H4	0.9500	C34—H27	0.9500
C14—C17	1.513 (6)	C35—H28	0.9500

C2—Ru1—C1	94.36 (18)	C14—C9—C10	118.9 (4)
C2—Ru1—P1	97.08 (13)	C14—C9—P1	120.6 (3)
C1—Ru1—P1	100.02 (12)	C10—C9—P1	120.5 (3)
C2—Ru1—P2	94.85 (13)	C11—C10—C9	119.0 (4)
C1—Ru1—P2	97.22 (11)	C11—C10—C15	117.7 (4)
P1—Ru1—P2	158.17 (3)	C9—C10—C15	123.3 (4)
C2—Ru1—Ru2	146.84 (12)	C12—C11—C10	122.6 (4)
C1—Ru1—Ru2	97.77 (13)	C12—C11—H3	118.7
P1—Ru1—Ru2	50.46 (3)	C10—C11—H3	118.7
P2—Ru1—Ru2	113.94 (3)	C11—C12—C13	117.7 (4)
C2—Ru1—Ru3	99.08 (12)	C11—C12—C16	120.4 (5)
C1—Ru1—Ru3	148.99 (12)	C13—C12—C16	121.9 (5)
P1—Ru1—Ru3	50.77 (2)	C12—C13—C14	122.7 (4)
P2—Ru1—Ru3	109.25 (2)	C12—C13—H4	118.7
Ru2—Ru1—Ru3	57.162 (10)	C14—C13—H4	118.7
C2—Ru1—H1	179.1 (18)	C13—C14—C9	118.9 (4)
C1—Ru1—H1	85.1 (17)	C13—C14—C17	118.1 (4)
P1—Ru1—H1	83.7 (17)	C9—C14—C17	123.0 (4)
P2—Ru1—H1	84.6 (17)	C10—C15—H5	109.5
Ru2—Ru1—H1	34.0 (17)	C10—C15—H6	109.5
Ru3—Ru1—H1	81.7 (17)	H5—C15—H6	109.5
C2—Ru1—H2	93.6 (16)	C10—C15—H7	109.5
C1—Ru1—H2	171.7 (16)	H5—C15—H7	109.5
P1—Ru1—H2	81.5 (16)	H6—C15—H7	109.5
P2—Ru1—H2	79.6 (16)	C12—C16—H8	109.5
Ru2—Ru1—H2	76.8 (16)	C12—C16—H9	109.5
Ru3—Ru1—H2	30.9 (16)	H8—C16—H9	109.5
H1—Ru1—H2	87 (2)	C12—C16—H10	109.5
C5—Ru2—C4	95.1 (2)	H8—C16—H10	109.5
C5—Ru2—C3	94.16 (19)	H9—C16—H10	109.5
C4—Ru2—C3	102.67 (18)	C14—C17—H11	109.5
C5—Ru2—P1	95.85 (15)	C14—C17—H12	109.5
C4—Ru2—P1	108.53 (13)	H11—C17—H12	109.5
C3—Ru2—P1	146.14 (13)	C14—C17—H13	109.5
C5—Ru2—Ru3	95.59 (15)	H11—C17—H13	109.5
C4—Ru2—Ru3	159.50 (14)	H12—C17—H13	109.5
C3—Ru2—Ru3	93.97 (13)	C19—C18—C23	119.7 (4)
P1—Ru2—Ru3	52.91 (2)	C19—C18—P2	121.8 (3)
C5—Ru2—Ru1	146.41 (15)	C23—C18—P2	118.5 (3)
C4—Ru2—Ru1	100.92 (15)	C18—C19—C20	119.2 (5)
C3—Ru2—Ru1	110.60 (13)	C18—C19—H14	120.4
P1—Ru2—Ru1	51.09 (2)	C20—C19—H14	120.4
Ru3—Ru2—Ru1	61.476 (10)	C21—C20—C19	120.6 (5)
C5—Ru2—H1	177.5 (18)	C21—C20—H15	119.7
C4—Ru2—H1	82.7 (18)	C19—C20—H15	119.7
C3—Ru2—H1	85.2 (18)	C20—C21—C22	120.0 (4)
P1—Ru2—H1	86.0 (18)	C20—C21—H16	120.0
Ru3—Ru2—H1	86.9 (18)	C22—C21—H16	120.0
Ru1—Ru2—H1	35.7 (18)	C21—C22—C23	119.9 (4)
C7—Ru3—C8	95.2 (2)	C21—C22—H17	120.1
C7—Ru3—C6	97.59 (19)	C23—C22—H17	120.1
C8—Ru3—C6	99.74 (18)	C22—C23—C18	120.6 (4)
C7—Ru3—P1	95.81 (13)	C22—C23—H18	119.7
C8—Ru3—P1	110.90 (12)	C18—C23—H18	119.7
C6—Ru3—P1	145.14 (13)	C25—C24—C29	118.6 (3)
C7—Ru3—Ru2	96.28 (15)	C25—C24—P2	122.7 (3)
C8—Ru3—Ru2	160.67 (12)	C29—C24—P2	118.6 (3)
C6—Ru3—Ru2	94.07 (13)	C26—C25—C24	120.3 (4)
P1—Ru3—Ru2	52.45 (3)	C26—C25—H19	119.8
C7—Ru3—Ru1	146.42 (13)	C24—C25—H19	119.8
C8—Ru3—Ru1	101.19 (12)	C27—C26—C25	120.4 (4)
C6—Ru3—Ru1	108.09 (12)	C27—C26—H20	119.8
P1—Ru3—Ru1	50.97 (2)	C25—C26—H20	119.8
Ru2—Ru3—Ru1	61.362 (10)	C28—C27—C26	120.1 (4)
C7—Ru3—H2	178.1 (17)	C28—C27—H21	119.9
C8—Ru3—H2	86.7 (17)	C26—C27—H21	119.9
C6—Ru3—H2	81.8 (17)	C27—C28—C29	120.0 (4)
P1—Ru3—H2	83.7 (17)	C27—C28—H22	120.0
Ru2—Ru3—H2	82.0 (17)	C29—C28—H22	120.0
Ru1—Ru3—H2	32.9 (17)	C28—C29—C24	120.6 (4)
C9—P1—Ru2	134.38 (14)	C28—C29—H23	119.7
C9—P1—Ru3	133.92 (13)	C24—C29—H23	119.7
Ru2—P1—Ru3	74.63 (3)	C35—C30—C31	118.3 (4)
C9—P1—Ru1	133.56 (13)	C35—C30—P2	121.8 (3)
Ru2—P1—Ru1	78.45 (3)	C31—C30—P2	120.0 (3)
Ru3—P1—Ru1	78.26 (3)	C32—C31—C30	119.8 (4)
C18—P2—C24	103.24 (17)	C32—C31—H24	120.1
C18—P2—C30	103.62 (17)	C30—C31—H24	120.1
C24—P2—C30	102.91 (18)	C33—C32—C31	120.8 (5)
C18—P2—Ru1	115.27 (12)	C33—C32—H25	119.6
C24—P2—Ru1	114.53 (12)	C31—C32—H25	119.6
C30—P2—Ru1	115.62 (13)	C34—C33—C32	120.1 (4)
O1—C1—Ru1	179.2 (4)	C34—C33—H26	120.0
O2—C2—Ru1	179.5 (4)	C32—C33—H26	120.0
O3—C3—Ru2	176.3 (4)	C33—C34—C35	119.9 (5)
O4—C4—Ru2	177.9 (5)	C33—C34—H27	120.0
O5—C5—Ru2	179.1 (5)	C35—C34—H27	120.0
O6—C6—Ru3	179.0 (4)	C30—C35—C34	121.1 (5)
O7—C7—Ru3	179.5 (5)	C30—C35—H28	119.5
O8—C8—Ru3	177.0 (4)	C34—C35—H28	119.5

Experimental details

Crystal data
Chemical formula	[Ru₃(C₉H₁₁P)H₂(C₁₈H₁₅P)(CO)₈]
M_r	941.72
Crystal system, space group	Triclinic, P1
Temperature (K)	150
a, b, c (Å)	11.5954 (5), 12.0870 (7), 13.4304 (1)
α, β, γ (°)	100.224 (2), 94.6231 (17), 95.0167 (13)
V (Å³)	1836.44 (13)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.35
Crystal size (mm)	0.30 × 0.30 × 0.03

Data collection
Diffractometer	Rigaku R-AXIS RAPID imaging plate
Absorption correction	Integration (NUMABS; Higashi, 1999)
T_min, T_max	0.687, 0.961
No. of measured, independent and observed [I > 2σ(I)] reflections	17157, 8304, 7671
R_int	0.035
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.030, 0.118, 1.23
No. of reflections	8304
No. of parameters	444
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.74, −1.79

Computer programs: PROCESS-AUTO (Rigaku, 1998), TEXSAN (Molecular Structure Corporation & Rigaku, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997).

Selected geometric parameters (Å, º) top

Ru1—P1	2.3351 (10)	Ru3—P1	2.3285 (9)
Ru1—P2	2.3896 (9)	P1—C9	1.825 (4)
Ru1—Ru2	2.9400 (4)	P2—C18	1.828 (4)
Ru1—Ru3	2.9432 (4)	P2—C24	1.830 (4)
Ru2—P1	2.3143 (10)	P2—C30	1.835 (4)
Ru2—Ru3	2.8146 (4)

P1—Ru1—P2	158.17 (3)	Ru3—Ru2—Ru1	61.476 (10)
P1—Ru1—Ru2	50.46 (3)	P1—Ru3—Ru2	52.45 (3)
P2—Ru1—Ru2	113.94 (3)	P1—Ru3—Ru1	50.97 (2)
P1—Ru1—Ru3	50.77 (2)	Ru2—Ru3—Ru1	61.362 (10)
P2—Ru1—Ru3	109.25 (2)	Ru2—P1—Ru3	74.63 (3)
Ru2—Ru1—Ru3	57.162 (10)	Ru2—P1—Ru1	78.45 (3)
P1—Ru2—Ru3	52.91 (2)	Ru3—P1—Ru1	78.26 (3)
P1—Ru2—Ru1	51.09 (2)

Acknowledgements

This work was partially supported by a Grant-in-Aid for Young Scientists (B, 24790117) from the Ministry of Education, Culture, Sports, Science and Technology. The author thanks Dr H. Hashimoto and Professor H. Tobita for their useful assistance.

References

Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Frediani, P., Faggi, C., Papaleo, S., Salvini, A., Bianchi, M., Piacenti, F., Ianelli, S. & Nardelli, M. (1997). J. Organomet. Chem. 536–537, 123–138. CSD CrossRef Web of Science Google Scholar
Higashi, T. (1999). NUMABS. Rigaku Corporation, Tokyo, Japan. Google Scholar
Kakizawa, T., Hashimoto, H. & Tobita, H. (2006). J. Organomet. Chem. 691, 726–736. Web of Science CSD CrossRef CAS Google Scholar
Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan. Google Scholar
Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.