

Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536813014141/hy2626sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536813014141/hy2626Isup2.hkl |
CCDC reference: 954400
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean
(C-C) = 0.006 Å
- R factor = 0.032
- wR factor = 0.083
- Data-to-parameter ratio = 23.4
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C4
Alert level C PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C7 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C10 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C13 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C16 PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 139
Alert level G PLAT005_ALERT_5_G No _iucr_refine_instructions_details in the CIF ? PLAT154_ALERT_1_G The su's on the Cell Angles are Equal .......... 0.00200 Deg. PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 244
0 ALERT level A = Most likely a serious problem - resolve or explain 1 ALERT level B = A potentially serious problem, consider carefully 7 ALERT level C = Check. Ensure it is not caused by an omission or oversight 3 ALERT level G = General information/check it is not something unexpected 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
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%.
H atoms were placed in geometrically idealized positions and refined as riding atoms, with C—H = 0.98 (CH) and 0.96 (CH3) Å and with Uiso(H) = 1.2(1.5 for methyl)Ueq(C).
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).
![]() | Fig. 1. The molecular structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. |
[Ru(C6H14O2PS2)3] | Z = 2 |
Mr = 740.92 | F(000) = 766 |
Triclinic, P1 | Dx = 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 |
Bruker APEXII CCD diffractometer | 7478 independent reflections |
Radiation source: fine-focus sealed tube | 6083 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
ϕ and ω scans | θmax = 27.2°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.877, Tmax = 0.910 | k = −13→12 |
11411 measured reflections | l = −24→17 |
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(Fo2) + (0.0341P)2 + 0.2818P] where P = (Fo2 + 2Fc2)/3 |
7478 reflections | (Δ/σ)max = 0.001 |
319 parameters | Δρmax = 0.47 e Å−3 |
0 restraints | Δρmin = −0.32 e Å−3 |
[Ru(C6H14O2PS2)3] | γ = 82.175 (2)° |
Mr = 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)° |
Bruker APEXII CCD diffractometer | 7478 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 6083 reflections with I > 2σ(I) |
Tmin = 0.877, Tmax = 0.910 | Rint = 0.022 |
11411 measured reflections |
R[F2 > 2σ(F2)] = 0.032 | 0 restraints |
wR(F2) = 0.083 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.47 e Å−3 |
7478 reflections | Δρmin = −0.32 e Å−3 |
319 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
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* |
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) |
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] |
Mr | 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) |
Tmin, Tmax | 0.877, 0.910 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11411, 7478, 6083 |
Rint | 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 |
Δρmax, Δρmin (e Å−3) | 0.47, −0.32 |
Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
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) |
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 RuIII atom displays a distorted octahedral RuS6 coordination geometry. Each of dithiophosphate ligands binds to the RuIII 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).