Tris(diisopropyl di­thio­phosphato-κ2S,S′)ruthenium(III)

Chao, G.-P.; Wu, X.; Shi, H.-T.; Chen, Q.; Zhang, Q.-F.

doi:10.1107/S1600536813014141

metal-organic compounds

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ISSN: 2056-9890

Volume 69| Part 6| June 2013| Page m341

doi:10.1107/S1600536813014141

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Tris(diisopropyl dithiophosphato-κ²S,S′)ruthenium(III)

Guo-Ping Chao,^a Xiuli Wu,^a Hua-Tian Shi,^b Qun Chen ^a and Qian-Feng Zhang ^b,^a ^*

^aDepartment of Applied Chemistry, School of Petrochemical Engineering, Changzhou University, Jiangsu 213164, People's Republic of China, and ^bInstitute of Molecular Engineering and Applied Chemsitry, Anhui University of Technology, Ma'anshan, Anhui 243002, People's Republic of China
^*Correspondence e-mail: zhangqf@ahut.edu.cn

(Received 6 May 2013; accepted 21 May 2013; online 25 May 2013)

In the title complex, [Ru(C₆H₁₄O₂PS₂)₃], the coordination environment of the Ru^III atom is distorted octahedral, defined by six S atoms from three S,S′-bidentate diisopropyl dithiophosphate ligands. The average Ru—S bond length is 2.41 (1) Å and the average S—Ru—S bite angle is 81.13 (19)°.

Related literature

For background to ruthenium complexes, see: Castillo-Villalón et al. (2008 ); Chianelli et al. (2009 ); David et al. (2005 ); Leung et al. (2000 ); Wu et al. (2009 ). For related structures, see: Jain et al. (2000 ); Liu et al. (2005 ).

Experimental

Crystal data

[Ru(C₆H₁₄O₂PS₂)₃]
M_r = 740.92
Triclinic, $[P \overline 1]$
a = 8.9676 (8) Å
b = 10.5073 (9) Å
c = 19.1085 (17) Å
α = 81.281 (2)°
β = 88.678 (2)°
γ = 82.175 (2)°
V = 1763.1 (3) Å³
Z = 2
Mo Kα radiation
μ = 0.96 mm⁻¹
T = 296 K
0.14 × 0.11 × 0.10 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.877, T_max = 0.910
11411 measured reflections
7478 independent reflections
6083 reflections with I > 2σ(I)
R_int = 0.022

Refinement

R[F² > 2σ(F²)] = 0.032
wR(F²) = 0.083
S = 1.02
7478 reflections
319 parameters
H-atom parameters constrained
Δρ_max = 0.47 e Å⁻³
Δρ_min = −0.32 e Å⁻³

Table 1
Selected bond lengths (Å)

Ru1—S1	2.4189 (7)
Ru1—S2	2.4037 (7)
Ru1—S3	2.3981 (7)
Ru1—S4	2.3988 (7)
Ru1—S5	2.4155 (7)
Ru1—S6	2.4199 (7)

Data collection: APEX2 (Bruker, 2007 ); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; 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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536813014141/hy2626sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536813014141/hy2626Isup2.hkl

checkCIF report

Comment top

In recent years there has been an increased interest in ruthenium complexes with sulfur-donor ligands, in part because of the high catalytic activity of RuS₂ unit in various hydrogenation processes (Castillo-Villalón et al., 2008; Chianelli et al., 2009). In the course of our continuous study on ruthenium complexes in a sulfur-rich coordination environment (Leung et al., 2000), we are interested in the homoleptic ruthenium complexes with thiolate ligands, which may be probably designed as processors for the binary RuS₂ nanoparticles (David et al., 2005). Although the ruthenium chemistry of dithio acidic ligands such as dithiocarbamate and dithiocarbonate has been the subject of continuous study, the corresponding ruthenium dithiophosphate chemistry has not been developed much (Wu et al., 2009). Here we report the crystal structure of the title compound, a homoleptic ruthenium complex.

The molecular structure of the title complex is depicted in Fig. 1. The complex is mononuclear and the Ru^III atom displays a distorted octahedral RuS₆ coordination geometry. Each of dithiophosphate ligands binds to the Ru^III atom in an S,S'-bidentate mode, forming a four-membered ring with an average S—Ru—S bite angle of 81.31 (2)°, which is comparable with those in [Ru{S₂P(OMe)₂}₃] [av. 81.54 (8)°] and [Ru{S₂P(OEt)₂}₃] [av. 81.84 (6)°] (Jain et al., 2000). Each four-membered RuS₂P ring is nonplanar and contains a pair of nearly equal Ru—S bonds (Table 1). The average Ru—S bond length of 2.4092 (7) Å in the title complex is compatible to those in [Ru{S₂P(OMe)₂}₃] [av. 2.413 (13) Å] and [Ru{S₂P(OEt)₂}₃] [av. 2.424 (3) Å] (Jain et al., 2000), but is obviously shorter than those in [Ru{S₂P(OEt)₂}₂(PPh₃)₂] [av. 2.4974 (11) Å] and [RuH(CO){S₂P(OEt)₂}(PPh₃)₂] [av. 2.5474 (12) Å] (Liu et al., 2005). The bond distances within the di-iso-proposaldithiophosphate ligands of the title complex agree well with those found in the analogous dimethyl- and diethyldithiophosphate complexes of ruthenium (Jain et al., 2000).

Related literature top

For background to ruthenium complexes, see: Castillo-Villalón et al. (2008); Chianelli et al. (2009); David et al. (2005); Leung et al. (2000); Wu et al. (2009). For related structures, see: Jain et al. (2000); Liu et al. (2005).

Experimental top

A mixture of RuCl₃.H₂O (209 mg, 0.80 mmol) and KS₂P(OⁱPr)₂ (606 mg, 2.40 mmol) was dissolved in 25 ml of methanol and then heated at reflux for 8 h. During this time the color of the reaction solution was changed from brown to bright red. The solvent was evaporated in vacuo and the residue was redissolved in dichloromethane and then filtered. The filtrate was dried and then recrystallized from diethyl ether/hexane. The red plate-shaped crystals of the title complex were obtained within a week. Yield: 260 mg, 44% (based on Ru). Analysis, calculated for C₁₈H₄₂O₆P₃RuS₆: C 29.18, H 5.71%; found: C 29.25, H 5.67%.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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).

Figures top

Fig. 1. The molecular structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level.

Tris(diisopropyl dithiophosphato-κ²S,S')ruthenium(III) top

Crystal data top

[Ru(C₆H₁₄O₂PS₂)₃]	Z = 2
M_r = 740.92	F(000) = 766
Triclinic, P1	D_x = 1.396 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.9676 (8) Å	Cell parameters from 2994 reflections
b = 10.5073 (9) Å	θ = 2.6–25.7°
c = 19.1085 (17) Å	µ = 0.96 mm⁻¹
α = 81.281 (2)°	T = 296 K
β = 88.678 (2)°	Block, red
γ = 82.175 (2)°	0.14 × 0.11 × 0.10 mm
V = 1763.1 (3) Å³

Data collection top

Bruker APEXII CCD diffractometer	7478 independent reflections
Radiation source: fine-focus sealed tube	6083 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.022
ϕ and ω scans	θ_max = 27.2°, θ_min = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→11
T_min = 0.877, T_max = 0.910	k = −13→12
11411 measured reflections	l = −24→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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.083	H-atom parameters constrained
S = 1.02	w = 1/[σ²(F_o²) + (0.0341P)² + 0.2818P] where P = (F_o² + 2F_c²)/3
7478 reflections	(Δ/σ)_max = 0.001
319 parameters	Δρ_max = 0.47 e Å⁻³
0 restraints	Δρ_min = −0.32 e Å⁻³

Crystal data top

[Ru(C₆H₁₄O₂PS₂)₃]	γ = 82.175 (2)°
M_r = 740.92	V = 1763.1 (3) Å³
Triclinic, P1	Z = 2
a = 8.9676 (8) Å	Mo Kα radiation
b = 10.5073 (9) Å	µ = 0.96 mm⁻¹
c = 19.1085 (17) Å	T = 296 K
α = 81.281 (2)°	0.14 × 0.11 × 0.10 mm
β = 88.678 (2)°

Data collection top

Bruker APEXII CCD diffractometer	7478 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	6083 reflections with I > 2σ(I)
T_min = 0.877, T_max = 0.910	R_int = 0.022
11411 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	0 restraints
wR(F²) = 0.083	H-atom parameters constrained
S = 1.02	Δρ_max = 0.47 e Å⁻³
7478 reflections	Δρ_min = −0.32 e Å⁻³
319 parameters

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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	0.73359 (2)	0.556490 (18)	0.733889 (10)	0.04029 (7)
S1	0.76352 (8)	0.32294 (7)	0.76690 (4)	0.05468 (17)
S2	0.94238 (8)	0.50082 (7)	0.65811 (4)	0.05370 (17)
S3	0.53460 (8)	0.54659 (6)	0.65399 (4)	0.05063 (16)
S4	0.70241 (8)	0.77884 (6)	0.67808 (4)	0.04961 (16)
S5	0.55622 (7)	0.59086 (7)	0.82845 (4)	0.05446 (17)
S6	0.90545 (7)	0.59914 (7)	0.82065 (4)	0.05280 (17)
P1	0.93826 (8)	0.31504 (7)	0.69980 (4)	0.05098 (17)
P2	0.53435 (7)	0.73678 (6)	0.62205 (3)	0.04477 (15)
P3	0.72941 (8)	0.61841 (7)	0.88599 (4)	0.05070 (17)
O1	1.0904 (2)	0.2439 (2)	0.73416 (11)	0.0644 (5)
O2	0.9293 (2)	0.2225 (2)	0.64323 (11)	0.0645 (5)
O3	0.5505 (2)	0.7768 (2)	0.54005 (9)	0.0563 (5)
O4	0.37794 (19)	0.82026 (18)	0.62947 (9)	0.0551 (5)
O5	0.7094 (2)	0.74961 (19)	0.91720 (10)	0.0644 (5)
O6	0.7469 (2)	0.5263 (2)	0.95902 (10)	0.0624 (5)
C1	1.1586 (4)	0.2919 (3)	0.79194 (19)	0.0748 (9)
H1	1.0995	0.3727	0.8019	0.090*
C2	1.3140 (5)	0.3157 (6)	0.7684 (3)	0.151 (2)
H2A	1.3645	0.2406	0.7505	0.226*
H2B	1.3691	0.3321	0.8078	0.226*
H2C	1.3080	0.3896	0.7318	0.226*
C3	1.1601 (5)	0.1891 (5)	0.8553 (2)	0.1150 (16)
H3A	1.0598	0.1685	0.8648	0.172*
H3B	1.1968	0.2201	0.8955	0.172*
H3C	1.2246	0.1126	0.8463	0.172*
C4	0.7981 (4)	0.2394 (3)	0.5962 (2)	0.0735 (9)
H4	0.7245	0.3110	0.6079	0.088*
C5	0.7314 (6)	0.1163 (5)	0.6098 (4)	0.167 (3)
H5A	0.8043	0.0460	0.5992	0.251*
H5B	0.6445	0.1231	0.5804	0.251*
H5C	0.7024	0.1001	0.6587	0.251*
C6	0.8515 (5)	0.2709 (6)	0.5218 (2)	0.149 (2)
H6A	0.9104	0.3414	0.5185	0.224*
H6B	0.7664	0.2956	0.4908	0.224*
H6C	0.9121	0.1960	0.5082	0.224*
C7	0.6915 (3)	0.7423 (3)	0.50207 (15)	0.0623 (8)
H7	0.7729	0.7080	0.5359	0.075*
C8	0.6647 (6)	0.6420 (5)	0.4587 (3)	0.1266 (18)
H8A	0.6194	0.5746	0.4875	0.190*
H8B	0.7588	0.6057	0.4402	0.190*
H8C	0.5987	0.6809	0.4202	0.190*
C9	0.7253 (5)	0.8642 (4)	0.4591 (3)	0.1215 (17)
H9A	0.6431	0.8988	0.4274	0.182*
H9B	0.8155	0.8469	0.4322	0.182*
H9C	0.7391	0.9261	0.4897	0.182*
C10	0.2862 (4)	0.8074 (3)	0.69364 (16)	0.0675 (8)
H10	0.3235	0.7271	0.7249	0.081*
C11	0.1293 (5)	0.8026 (6)	0.6708 (3)	0.141 (2)
H11A	0.0966	0.8784	0.6373	0.212*
H11B	0.0637	0.8000	0.7113	0.212*
H11C	0.1267	0.7262	0.6492	0.212*
C12	0.2940 (5)	0.9204 (5)	0.7298 (3)	0.1266 (18)
H12A	0.3974	0.9317	0.7349	0.190*
H12B	0.2481	0.9063	0.7757	0.190*
H12C	0.2417	0.9968	0.7023	0.190*
C13	0.6915 (4)	0.8748 (3)	0.87079 (19)	0.0766 (9)
H13	0.6763	0.8600	0.8222	0.092*
C14	0.8314 (6)	0.9343 (5)	0.8733 (3)	0.148 (2)
H14A	0.8432	0.9553	0.9199	0.222*
H14B	0.8255	1.0120	0.8393	0.222*
H14C	0.9160	0.8741	0.8625	0.222*
C15	0.5537 (5)	0.9537 (5)	0.8945 (3)	0.1347 (19)
H15A	0.4684	0.9083	0.8921	0.202*
H15B	0.5371	1.0360	0.8642	0.202*
H15C	0.5668	0.9676	0.9423	0.202*
C16	0.7732 (4)	0.3847 (3)	0.96155 (16)	0.0659 (8)
H16	0.7969	0.3654	0.9136	0.079*
C17	0.6338 (5)	0.3299 (5)	0.9858 (3)	0.1299 (18)
H17A	0.6092	0.3480	1.0328	0.195*
H17B	0.6492	0.2376	0.9861	0.195*
H17C	0.5527	0.3685	0.9544	0.195*
C18	0.9062 (5)	0.3339 (5)	1.0075 (3)	0.138 (2)
H18A	0.9910	0.3754	0.9893	0.207*
H18B	0.9292	0.2417	1.0081	0.207*
H18C	0.8843	0.3516	1.0547	0.207*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ru1	0.04333 (12)	0.03643 (11)	0.04021 (12)	−0.00469 (8)	0.00048 (8)	−0.00357 (8)
S1	0.0558 (4)	0.0391 (4)	0.0658 (4)	−0.0044 (3)	0.0055 (3)	0.0006 (3)
S2	0.0540 (4)	0.0504 (4)	0.0555 (4)	−0.0055 (3)	0.0117 (3)	−0.0071 (3)
S3	0.0542 (4)	0.0429 (4)	0.0563 (4)	−0.0088 (3)	−0.0084 (3)	−0.0091 (3)
S4	0.0585 (4)	0.0386 (3)	0.0517 (4)	−0.0116 (3)	−0.0064 (3)	−0.0013 (3)
S5	0.0491 (4)	0.0671 (5)	0.0463 (4)	−0.0058 (3)	0.0055 (3)	−0.0083 (3)
S6	0.0497 (4)	0.0619 (4)	0.0478 (4)	−0.0078 (3)	−0.0042 (3)	−0.0107 (3)
P1	0.0486 (4)	0.0443 (4)	0.0592 (4)	0.0025 (3)	−0.0037 (3)	−0.0123 (3)
P2	0.0481 (4)	0.0438 (4)	0.0402 (3)	−0.0021 (3)	−0.0014 (3)	−0.0030 (3)
P3	0.0603 (4)	0.0498 (4)	0.0400 (4)	−0.0007 (3)	−0.0017 (3)	−0.0061 (3)
O1	0.0550 (11)	0.0601 (13)	0.0764 (14)	0.0102 (9)	−0.0149 (10)	−0.0183 (10)
O2	0.0603 (11)	0.0594 (13)	0.0755 (14)	0.0092 (9)	−0.0128 (10)	−0.0292 (10)
O3	0.0535 (10)	0.0707 (13)	0.0399 (10)	0.0003 (9)	0.0003 (8)	−0.0008 (8)
O4	0.0541 (10)	0.0539 (11)	0.0507 (10)	0.0060 (8)	0.0039 (8)	0.0005 (8)
O5	0.0869 (14)	0.0532 (12)	0.0512 (11)	0.0021 (10)	−0.0025 (10)	−0.0116 (9)
O6	0.0852 (14)	0.0580 (12)	0.0409 (10)	−0.0009 (10)	−0.0023 (9)	−0.0052 (8)
C1	0.069 (2)	0.068 (2)	0.087 (2)	0.0054 (16)	−0.0263 (18)	−0.0192 (18)
C2	0.122 (4)	0.197 (6)	0.139 (5)	−0.095 (4)	−0.040 (3)	0.029 (4)
C3	0.108 (3)	0.148 (5)	0.082 (3)	−0.012 (3)	−0.015 (2)	0.002 (3)
C4	0.0653 (19)	0.062 (2)	0.095 (3)	0.0054 (15)	−0.0227 (18)	−0.0271 (18)
C5	0.167 (5)	0.085 (3)	0.257 (7)	−0.045 (3)	−0.107 (5)	−0.007 (4)
C6	0.118 (4)	0.250 (8)	0.081 (3)	−0.007 (4)	−0.022 (3)	−0.041 (4)
C7	0.0580 (16)	0.077 (2)	0.0490 (16)	0.0018 (15)	0.0072 (13)	−0.0101 (14)
C8	0.140 (4)	0.133 (4)	0.124 (4)	−0.028 (3)	0.050 (3)	−0.075 (3)
C9	0.122 (3)	0.104 (4)	0.126 (4)	−0.015 (3)	0.063 (3)	0.009 (3)
C10	0.076 (2)	0.0612 (19)	0.0558 (17)	0.0121 (16)	0.0166 (15)	0.0008 (14)
C11	0.100 (3)	0.206 (6)	0.143 (5)	−0.072 (4)	0.053 (3)	−0.068 (4)
C12	0.131 (4)	0.146 (5)	0.114 (4)	−0.004 (3)	0.020 (3)	−0.072 (3)
C13	0.103 (3)	0.0522 (19)	0.071 (2)	0.0045 (18)	−0.0121 (19)	−0.0085 (15)
C14	0.132 (4)	0.073 (3)	0.232 (7)	−0.026 (3)	−0.018 (4)	0.013 (4)
C15	0.142 (4)	0.085 (3)	0.163 (5)	0.037 (3)	0.005 (4)	−0.021 (3)
C16	0.083 (2)	0.0575 (19)	0.0513 (17)	0.0013 (16)	0.0020 (15)	0.0002 (13)
C17	0.126 (4)	0.092 (3)	0.163 (5)	−0.028 (3)	0.040 (3)	0.012 (3)
C18	0.164 (4)	0.082 (3)	0.155 (5)	0.013 (3)	−0.083 (4)	0.007 (3)

Geometric parameters (Å, º) top

Ru1—S1	2.4189 (7)	C6—H6A	0.9600
Ru1—S2	2.4037 (7)	C6—H6B	0.9600
Ru1—S3	2.3981 (7)	C6—H6C	0.9600
Ru1—S4	2.3988 (7)	C7—C9	1.477 (5)
Ru1—S5	2.4155 (7)	C7—C8	1.483 (5)
Ru1—S6	2.4199 (7)	C7—H7	0.9800
S1—P1	2.0027 (10)	C8—H8A	0.9600
S2—P1	1.9983 (10)	C8—H8B	0.9600
S3—P2	1.9988 (9)	C8—H8C	0.9600
S4—P2	2.0030 (9)	C9—H9A	0.9600
S5—P3	2.0007 (10)	C9—H9B	0.9600
S6—P3	1.9976 (10)	C9—H9C	0.9600
P1—O2	1.570 (2)	C10—C12	1.471 (5)
P1—O1	1.5706 (19)	C10—C11	1.493 (5)
P2—O4	1.5653 (18)	C10—H10	0.9800
P2—O3	1.5681 (18)	C11—H11A	0.9600
P3—O5	1.570 (2)	C11—H11B	0.9600
P3—O6	1.5709 (19)	C11—H11C	0.9600
O1—C1	1.459 (4)	C12—H12A	0.9600
O2—C4	1.472 (4)	C12—H12B	0.9600
O3—C7	1.473 (3)	C12—H12C	0.9600
O4—C10	1.460 (3)	C13—C14	1.480 (5)
O5—C13	1.462 (4)	C13—C15	1.493 (5)
O6—C16	1.468 (4)	C13—H13	0.9800
C1—C3	1.494 (5)	C14—H14A	0.9600
C1—C2	1.496 (5)	C14—H14B	0.9600
C1—H1	0.9800	C14—H14C	0.9600
C2—H2A	0.9600	C15—H15A	0.9600
C2—H2B	0.9600	C15—H15B	0.9600
C2—H2C	0.9600	C15—H15C	0.9600
C3—H3A	0.9600	C16—C17	1.483 (5)
C3—H3B	0.9600	C16—C18	1.487 (5)
C3—H3C	0.9600	C16—H16	0.9800
C4—C5	1.483 (5)	C17—H17A	0.9600
C4—C6	1.494 (5)	C17—H17B	0.9600
C4—H4	0.9800	C17—H17C	0.9600
C5—H5A	0.9600	C18—H18A	0.9600
C5—H5B	0.9600	C18—H18B	0.9600
C5—H5C	0.9600	C18—H18C	0.9600

S3—Ru1—S4	81.50 (2)	H6A—C6—H6B	109.5
S3—Ru1—S2	98.00 (3)	C4—C6—H6C	109.5
S4—Ru1—S2	91.82 (2)	H6A—C6—H6C	109.5
S3—Ru1—S5	91.52 (3)	H6B—C6—H6C	109.5
S4—Ru1—S5	95.44 (3)	O3—C7—C9	105.9 (3)
S2—Ru1—S5	168.80 (3)	O3—C7—C8	107.4 (3)
S3—Ru1—S1	90.71 (3)	C9—C7—C8	113.0 (4)
S4—Ru1—S1	168.84 (3)	O3—C7—H7	110.1
S2—Ru1—S1	81.31 (2)	C9—C7—H7	110.1
S5—Ru1—S1	92.73 (3)	C8—C7—H7	110.1
S3—Ru1—S6	169.79 (2)	C7—C8—H8A	109.5
S4—Ru1—S6	92.10 (2)	C7—C8—H8B	109.5
S2—Ru1—S6	90.11 (3)	H8A—C8—H8B	109.5
S5—Ru1—S6	81.12 (3)	C7—C8—H8C	109.5
S1—Ru1—S6	96.67 (3)	H8A—C8—H8C	109.5
P1—S1—Ru1	87.31 (3)	H8B—C8—H8C	109.5
P1—S2—Ru1	87.83 (3)	C7—C9—H9A	109.5
P2—S3—Ru1	87.78 (3)	C7—C9—H9B	109.5
P2—S4—Ru1	87.67 (3)	H9A—C9—H9B	109.5
P3—S5—Ru1	87.61 (3)	C7—C9—H9C	109.5
P3—S6—Ru1	87.56 (3)	H9A—C9—H9C	109.5
O2—P1—O1	96.41 (11)	H9B—C9—H9C	109.5
O2—P1—S2	113.86 (9)	O4—C10—C12	108.7 (3)
O1—P1—S2	114.71 (9)	O4—C10—C11	106.8 (3)
O2—P1—S1	114.42 (9)	C12—C10—C11	111.2 (4)
O1—P1—S1	114.49 (9)	O4—C10—H10	110.0
S2—P1—S1	103.50 (4)	C12—C10—H10	110.0
O4—P2—O3	96.25 (10)	C11—C10—H10	110.0
O4—P2—S3	113.93 (8)	C10—C11—H11A	109.5
O3—P2—S3	114.89 (9)	C10—C11—H11B	109.5
O4—P2—S4	115.64 (8)	H11A—C11—H11B	109.5
O3—P2—S4	113.79 (8)	C10—C11—H11C	109.5
S3—P2—S4	102.97 (4)	H11A—C11—H11C	109.5
O5—P3—O6	96.44 (11)	H11B—C11—H11C	109.5
O5—P3—S6	113.64 (9)	C10—C12—H12A	109.5
O6—P3—S6	114.96 (9)	C10—C12—H12B	109.5
O5—P3—S5	115.12 (9)	H12A—C12—H12B	109.5
O6—P3—S5	113.51 (9)	C10—C12—H12C	109.5
S6—P3—S5	103.70 (4)	H12A—C12—H12C	109.5
C1—O1—P1	121.08 (19)	H12B—C12—H12C	109.5
C4—O2—P1	120.73 (18)	O5—C13—C14	108.5 (3)
C7—O3—P2	122.02 (16)	O5—C13—C15	107.3 (3)
C10—O4—P2	123.28 (17)	C14—C13—C15	114.4 (4)
C13—O5—P3	121.11 (19)	O5—C13—H13	108.8
C16—O6—P3	120.41 (17)	C14—C13—H13	108.8
O1—C1—C3	107.1 (3)	C15—C13—H13	108.8
O1—C1—C2	106.9 (3)	C13—C14—H14A	109.5
C3—C1—C2	112.1 (3)	C13—C14—H14B	109.5
O1—C1—H1	110.2	H14A—C14—H14B	109.5
C3—C1—H1	110.2	C13—C14—H14C	109.5
C2—C1—H1	110.2	H14A—C14—H14C	109.5
C1—C2—H2A	109.5	H14B—C14—H14C	109.5
C1—C2—H2B	109.5	C13—C15—H15A	109.5
H2A—C2—H2B	109.5	C13—C15—H15B	109.5
C1—C2—H2C	109.5	H15A—C15—H15B	109.5
H2A—C2—H2C	109.5	C13—C15—H15C	109.5
H2B—C2—H2C	109.5	H15A—C15—H15C	109.5
C1—C3—H3A	109.5	H15B—C15—H15C	109.5
C1—C3—H3B	109.5	O6—C16—C17	109.1 (3)
H3A—C3—H3B	109.5	O6—C16—C18	107.7 (3)
C1—C3—H3C	109.5	C17—C16—C18	114.2 (3)
H3A—C3—H3C	109.5	O6—C16—H16	108.6
H3B—C3—H3C	109.5	C17—C16—H16	108.6
O2—C4—C5	106.5 (3)	C18—C16—H16	108.6
O2—C4—C6	107.9 (3)	C16—C17—H17A	109.5
C5—C4—C6	113.4 (4)	C16—C17—H17B	109.5
O2—C4—H4	109.6	H17A—C17—H17B	109.5
C5—C4—H4	109.6	C16—C17—H17C	109.5
C6—C4—H4	109.6	H17A—C17—H17C	109.5
C4—C5—H5A	109.5	H17B—C17—H17C	109.5
C4—C5—H5B	109.5	C16—C18—H18A	109.5
H5A—C5—H5B	109.5	C16—C18—H18B	109.5
C4—C5—H5C	109.5	H18A—C18—H18B	109.5
H5A—C5—H5C	109.5	C16—C18—H18C	109.5
H5B—C5—H5C	109.5	H18A—C18—H18C	109.5
C4—C6—H6A	109.5	H18B—C18—H18C	109.5
C4—C6—H6B	109.5

Experimental details

Crystal data
Chemical formula	[Ru(C₆H₁₄O₂PS₂)₃]
M_r	740.92
Crystal system, space group	Triclinic, P1
Temperature (K)	296
a, b, c (Å)	8.9676 (8), 10.5073 (9), 19.1085 (17)
α, β, γ (°)	81.281 (2), 88.678 (2), 82.175 (2)
V (Å³)	1763.1 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.96
Crystal size (mm)	0.14 × 0.11 × 0.10

Data collection
Diffractometer	Bruker APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.877, 0.910
No. of measured, independent and observed [I > 2σ(I)] reflections	11411, 7478, 6083
R_int	0.022
(sin θ/λ)_max (Å⁻¹)	0.643

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.083, 1.02
No. of reflections	7478
No. of parameters	319
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.47, −0.32

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Ru1—S1	2.4189 (7)	Ru1—S4	2.3988 (7)
Ru1—S2	2.4037 (7)	Ru1—S5	2.4155 (7)
Ru1—S3	2.3981 (7)	Ru1—S6	2.4199 (7)

Acknowledgements

This project was supported by the Natural Science Foundation of China (grant No. 20771003).

References

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