



Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536809049940/sj2681sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536809049940/sj2681Isup2.hkl |
CCDC reference: 766661
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean
(C-C) = 0.007 Å
- R factor = 0.049
- wR factor = 0.096
- Data-to-parameter ratio = 24.8
checkCIF/PLATON results
No syntax errors found
Alert level C SHFSU01_ALERT_2_C Test not performed. _refine_ls_shift/su_max and _refine_ls_shift/esd_max not present. Absolute value of the parameter shift to su ratio given 0.001 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.06 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru1 -- C44 .. 5.25 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru2 -- C47 .. 6.76 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru2 -- C49 .. 6.11 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru3 -- C50 .. 5.49 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C24 PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 96.00 A 3 PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 1 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 14 PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 1 PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 20 Ang. PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 65
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 13 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
All manipulations were performed under a dry oxygen-free dinitrogen atmosphere using standard Schlenk techniques, all solvents were dried over sodium and distilled from sodium benzophenone ketyl under nitrogen. Tris(4-methylphenyl)phosphine (Maybridge) was used as received and µ-bis(diphenylarsino)methanedecacarbonyltriruthenium(0) (Bruce et al., 1983) was prepared by a previously reported procedure. The title compound was obtained by refluxing equimolar quantities of Ru3(CO)10(µ-Ph2AsCH2AsPh2) (105.5 mg, 0.1 mmol) and tris(4-methylphenyl)phosphine (30.4 mg, 0.1 mmol) in hexane under a nitrogen atmosphere. Crystals suitable for X-ray diffraction were grown by slow solvent / solvent diffusion of CH3OH into CH2Cl2.
All hydrogen atoms were positioned geometrically and refined using a riding model with C—H = 0.93–0.97 Å and Uiso(H) = 1.2 or 1.5 Ueq(C). A rotating group model was used for the methyl groups.
Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).
[Ru3(C25H22As2)(C21H21P)(CO)9] | F(000) = 2632 |
Mr = 1331.91 | Dx = 1.652 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9940 reflections |
a = 16.2585 (2) Å | θ = 2.3–26.0° |
b = 16.9247 (2) Å | µ = 2.15 mm−1 |
c = 19.6900 (2) Å | T = 296 K |
β = 98.680 (1)° | Plate, red |
V = 5356.05 (11) Å3 | 0.21 × 0.21 × 0.03 mm |
Z = 4 |
Bruker SMART APEXII CCD area-detector diffractometer | 15703 independent reflections |
Radiation source: fine-focus sealed tube | 9536 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.063 |
ϕ and ω scans | θmax = 30.1°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2005) | h = −22→22 |
Tmin = 0.665, Tmax = 0.933 | k = −18→23 |
63277 measured reflections | l = −27→27 |
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)] = 0.049 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.096 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0397P)2] where P = (Fo2 + 2Fc2)/3 |
15703 reflections | (Δ/σ)max < 0.001 |
634 parameters | Δρmax = 0.60 e Å−3 |
0 restraints | Δρmin = −0.41 e Å−3 |
[Ru3(C25H22As2)(C21H21P)(CO)9] | V = 5356.05 (11) Å3 |
Mr = 1331.91 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 16.2585 (2) Å | µ = 2.15 mm−1 |
b = 16.9247 (2) Å | T = 296 K |
c = 19.6900 (2) Å | 0.21 × 0.21 × 0.03 mm |
β = 98.680 (1)° |
Bruker SMART APEXII CCD area-detector diffractometer | 15703 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2005) | 9536 reflections with I > 2σ(I) |
Tmin = 0.665, Tmax = 0.933 | Rint = 0.063 |
63277 measured reflections |
R[F2 > 2σ(F2)] = 0.049 | 0 restraints |
wR(F2) = 0.096 | H-atom parameters constrained |
S = 1.00 | Δρmax = 0.60 e Å−3 |
15703 reflections | Δρmin = −0.41 e Å−3 |
634 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. 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. |
x | y | z | Uiso*/Ueq | ||
Ru1 | 0.234430 (18) | 0.082258 (18) | 0.290394 (17) | 0.03903 (8) | |
Ru2 | 0.095682 (17) | 0.005658 (17) | 0.211088 (16) | 0.03574 (8) | |
Ru3 | 0.250620 (18) | −0.075182 (17) | 0.238649 (17) | 0.03759 (8) | |
As1 | 0.16874 (2) | 0.21116 (2) | 0.26830 (2) | 0.03705 (10) | |
As2 | −0.00352 (2) | 0.11309 (2) | 0.21734 (2) | 0.03700 (10) | |
P1 | 0.38304 (6) | −0.13329 (6) | 0.26418 (5) | 0.0402 (2) | |
O1 | 0.3348 (2) | 0.10979 (19) | 0.17289 (18) | 0.0784 (10) | |
O2 | 0.3831 (2) | 0.1220 (2) | 0.3968 (2) | 0.0934 (12) | |
O3 | 0.1375 (2) | 0.05987 (18) | 0.41083 (17) | 0.0741 (10) | |
O4 | 0.0457 (2) | −0.08636 (18) | 0.33265 (19) | 0.0782 (11) | |
O5 | −0.0027 (2) | −0.1159 (2) | 0.1199 (2) | 0.0924 (12) | |
O6 | 0.1513 (2) | 0.09138 (18) | 0.08889 (17) | 0.0699 (9) | |
O7 | 0.2824 (2) | −0.0409 (2) | 0.09116 (17) | 0.0756 (10) | |
O8 | 0.1550 (2) | −0.22473 (19) | 0.19949 (19) | 0.0814 (11) | |
O9 | 0.2461 (2) | −0.08632 (17) | 0.39289 (17) | 0.0697 (9) | |
C1 | 0.1912 (2) | 0.2681 (2) | 0.1877 (2) | 0.0445 (10) | |
C2 | 0.2732 (3) | 0.2890 (3) | 0.1858 (3) | 0.0652 (13) | |
H2A | 0.3141 | 0.2753 | 0.2221 | 0.078* | |
C3 | 0.2948 (4) | 0.3300 (3) | 0.1304 (3) | 0.0791 (16) | |
H3A | 0.3500 | 0.3436 | 0.1296 | 0.095* | |
C4 | 0.2357 (4) | 0.3504 (3) | 0.0775 (3) | 0.0845 (18) | |
H4A | 0.2504 | 0.3785 | 0.0406 | 0.101* | |
C5 | 0.1538 (4) | 0.3297 (3) | 0.0780 (3) | 0.0817 (16) | |
H5A | 0.1132 | 0.3430 | 0.0412 | 0.098* | |
C6 | 0.1326 (3) | 0.2889 (3) | 0.1338 (2) | 0.0616 (12) | |
H6A | 0.0773 | 0.2755 | 0.1345 | 0.074* | |
C7 | 0.1927 (2) | 0.2926 (2) | 0.3382 (2) | 0.0405 (9) | |
C8 | 0.2062 (3) | 0.2709 (2) | 0.4064 (2) | 0.0538 (11) | |
H8A | 0.2058 | 0.2176 | 0.4177 | 0.065* | |
C9 | 0.2204 (3) | 0.3265 (3) | 0.4583 (2) | 0.0671 (14) | |
H9A | 0.2289 | 0.3107 | 0.5041 | 0.081* | |
C10 | 0.2217 (3) | 0.4046 (3) | 0.4418 (3) | 0.0668 (14) | |
H10A | 0.2314 | 0.4425 | 0.4763 | 0.080* | |
C11 | 0.2086 (3) | 0.4272 (3) | 0.3744 (3) | 0.0675 (14) | |
H11A | 0.2099 | 0.4806 | 0.3634 | 0.081* | |
C12 | 0.1936 (3) | 0.3718 (2) | 0.3225 (2) | 0.0578 (12) | |
H12A | 0.1841 | 0.3881 | 0.2769 | 0.069* | |
C13 | 0.0474 (2) | 0.2089 (2) | 0.2622 (2) | 0.0416 (9) | |
H13A | 0.0243 | 0.2548 | 0.2367 | 0.050* | |
H13B | 0.0330 | 0.2123 | 0.3082 | 0.050* | |
C14 | −0.0632 (2) | 0.1517 (2) | 0.1305 (2) | 0.0448 (10) | |
C15 | −0.0724 (3) | 0.1023 (3) | 0.0737 (3) | 0.0661 (13) | |
H15A | −0.0508 | 0.0513 | 0.0779 | 0.079* | |
C16 | −0.1131 (4) | 0.1278 (4) | 0.0115 (3) | 0.0925 (19) | |
H16A | −0.1193 | 0.0936 | −0.0259 | 0.111* | |
C17 | −0.1448 (4) | 0.2033 (4) | 0.0036 (3) | 0.0920 (19) | |
H17A | −0.1715 | 0.2206 | −0.0390 | 0.110* | |
C18 | −0.1363 (3) | 0.2525 (3) | 0.0599 (3) | 0.0763 (15) | |
H18A | −0.1572 | 0.3037 | 0.0554 | 0.092* | |
C19 | −0.0973 (3) | 0.2266 (3) | 0.1227 (2) | 0.0560 (11) | |
H19A | −0.0937 | 0.2599 | 0.1605 | 0.067* | |
C20 | −0.0938 (2) | 0.0935 (2) | 0.2700 (2) | 0.0501 (11) | |
C21 | −0.1754 (3) | 0.0953 (3) | 0.2391 (3) | 0.0676 (14) | |
H21A | −0.1886 | 0.1111 | 0.1935 | 0.081* | |
C22 | −0.2379 (3) | 0.0736 (4) | 0.2756 (4) | 0.095 (2) | |
H22A | −0.2931 | 0.0742 | 0.2545 | 0.114* | |
C23 | −0.2189 (4) | 0.0514 (4) | 0.3419 (4) | 0.113 (3) | |
H23A | −0.2612 | 0.0352 | 0.3657 | 0.136* | |
C24 | −0.1385 (4) | 0.0523 (4) | 0.3747 (4) | 0.123 (3) | |
H24A | −0.1261 | 0.0390 | 0.4209 | 0.148* | |
C25 | −0.0748 (3) | 0.0737 (3) | 0.3370 (3) | 0.0853 (18) | |
H25A | −0.0197 | 0.0743 | 0.3583 | 0.102* | |
C26 | 0.3884 (2) | −0.2298 (2) | 0.3075 (2) | 0.0416 (9) | |
C27 | 0.3279 (2) | −0.2538 (2) | 0.3465 (2) | 0.0529 (11) | |
H27A | 0.2810 | −0.2226 | 0.3474 | 0.064* | |
C28 | 0.3370 (3) | −0.3233 (2) | 0.3841 (2) | 0.0581 (12) | |
H28A | 0.2967 | −0.3370 | 0.4108 | 0.070* | |
C29 | 0.4040 (3) | −0.3724 (2) | 0.3827 (2) | 0.0545 (11) | |
C30 | 0.4632 (3) | −0.3498 (2) | 0.3433 (2) | 0.0584 (12) | |
H30A | 0.5088 | −0.3825 | 0.3412 | 0.070* | |
C31 | 0.4564 (3) | −0.2794 (2) | 0.3066 (2) | 0.0520 (11) | |
H31A | 0.4979 | −0.2652 | 0.2812 | 0.062* | |
C32 | 0.4366 (2) | −0.1552 (2) | 0.1903 (2) | 0.0434 (9) | |
C33 | 0.3920 (3) | −0.1915 (2) | 0.1337 (2) | 0.0546 (11) | |
H33A | 0.3360 | −0.2028 | 0.1333 | 0.066* | |
C34 | 0.4297 (3) | −0.2114 (3) | 0.0773 (2) | 0.0644 (13) | |
H34A | 0.3983 | −0.2353 | 0.0394 | 0.077* | |
C35 | 0.5131 (3) | −0.1962 (3) | 0.0764 (2) | 0.0579 (12) | |
C36 | 0.5573 (3) | −0.1617 (3) | 0.1335 (2) | 0.0596 (12) | |
H36A | 0.6138 | −0.1519 | 0.1344 | 0.072* | |
C37 | 0.5202 (2) | −0.1409 (2) | 0.1898 (2) | 0.0533 (11) | |
H37A | 0.5519 | −0.1171 | 0.2276 | 0.064* | |
C38 | 0.4591 (2) | −0.0747 (2) | 0.3211 (2) | 0.0416 (9) | |
C39 | 0.4872 (3) | −0.0032 (2) | 0.2982 (2) | 0.0546 (11) | |
H39A | 0.4691 | 0.0130 | 0.2533 | 0.065* | |
C40 | 0.5415 (3) | 0.0441 (3) | 0.3412 (3) | 0.0585 (12) | |
H40A | 0.5603 | 0.0911 | 0.3244 | 0.070* | |
C41 | 0.5683 (3) | 0.0229 (3) | 0.4083 (2) | 0.0578 (12) | |
C42 | 0.5398 (3) | −0.0477 (3) | 0.4309 (2) | 0.0592 (12) | |
H42A | 0.5572 | −0.0635 | 0.4760 | 0.071* | |
C43 | 0.4858 (2) | −0.0957 (2) | 0.3878 (2) | 0.0491 (11) | |
H43A | 0.4675 | −0.1429 | 0.4045 | 0.059* | |
C44 | 0.2951 (3) | 0.0928 (2) | 0.2144 (2) | 0.0522 (11) | |
C45 | 0.3291 (3) | 0.1071 (3) | 0.3549 (3) | 0.0582 (12) | |
C46 | 0.1713 (3) | 0.0653 (2) | 0.3637 (2) | 0.0518 (11) | |
C47 | 0.0670 (2) | −0.0503 (2) | 0.2894 (2) | 0.0499 (11) | |
C48 | 0.0325 (2) | −0.0683 (3) | 0.1537 (2) | 0.0525 (11) | |
C49 | 0.1344 (2) | 0.0597 (2) | 0.1357 (2) | 0.0475 (10) | |
C50 | 0.2690 (3) | −0.0515 (2) | 0.1462 (2) | 0.0494 (10) | |
C51 | 0.1925 (2) | −0.1692 (3) | 0.2141 (2) | 0.0505 (11) | |
C52 | 0.2446 (3) | −0.0733 (2) | 0.3344 (2) | 0.0505 (11) | |
C53 | 0.4136 (3) | −0.4481 (3) | 0.4251 (3) | 0.0830 (16) | |
H53A | 0.4712 | −0.4558 | 0.4433 | 0.124* | |
H53B | 0.3940 | −0.4921 | 0.3964 | 0.124* | |
H53C | 0.3818 | −0.4439 | 0.4622 | 0.124* | |
C54 | 0.5545 (3) | −0.2172 (3) | 0.0149 (2) | 0.0850 (18) | |
H54A | 0.6021 | −0.2500 | 0.0294 | 0.127* | |
H54B | 0.5718 | −0.1698 | −0.0056 | 0.127* | |
H54C | 0.5157 | −0.2452 | −0.0182 | 0.127* | |
C55 | 0.6253 (3) | 0.0748 (3) | 0.4567 (3) | 0.095 (2) | |
H55A | 0.6557 | 0.1092 | 0.4307 | 0.142* | |
H55B | 0.6635 | 0.0424 | 0.4865 | 0.142* | |
H55C | 0.5928 | 0.1059 | 0.4837 | 0.142* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.03420 (15) | 0.03399 (18) | 0.04736 (19) | −0.00229 (13) | 0.00114 (15) | −0.00603 (15) |
Ru2 | 0.02854 (13) | 0.03101 (17) | 0.04748 (18) | −0.00082 (12) | 0.00511 (13) | −0.00357 (14) |
Ru3 | 0.03213 (15) | 0.03246 (17) | 0.04644 (19) | 0.00260 (12) | 0.00032 (14) | −0.00174 (14) |
As1 | 0.0377 (2) | 0.0325 (2) | 0.0409 (2) | −0.00439 (16) | 0.00575 (18) | −0.00314 (17) |
As2 | 0.03049 (18) | 0.0332 (2) | 0.0480 (2) | 0.00017 (16) | 0.00820 (18) | −0.00228 (18) |
P1 | 0.0329 (5) | 0.0406 (6) | 0.0455 (6) | 0.0030 (4) | 0.0012 (5) | 0.0006 (5) |
O1 | 0.072 (2) | 0.079 (2) | 0.093 (3) | −0.0106 (18) | 0.041 (2) | −0.008 (2) |
O2 | 0.070 (2) | 0.104 (3) | 0.093 (3) | 0.004 (2) | −0.031 (2) | −0.038 (2) |
O3 | 0.093 (3) | 0.068 (2) | 0.066 (2) | −0.0084 (18) | 0.028 (2) | −0.0057 (17) |
O4 | 0.085 (2) | 0.064 (2) | 0.091 (3) | −0.0072 (18) | 0.031 (2) | 0.0289 (19) |
O5 | 0.074 (2) | 0.076 (3) | 0.120 (3) | −0.017 (2) | −0.006 (2) | −0.046 (2) |
O6 | 0.074 (2) | 0.075 (2) | 0.064 (2) | 0.0058 (17) | 0.0215 (19) | 0.0193 (18) |
O7 | 0.097 (3) | 0.076 (2) | 0.057 (2) | 0.0244 (19) | 0.020 (2) | 0.0140 (18) |
O8 | 0.079 (2) | 0.048 (2) | 0.109 (3) | −0.0221 (18) | −0.014 (2) | −0.005 (2) |
O9 | 0.099 (3) | 0.056 (2) | 0.053 (2) | 0.0103 (17) | 0.008 (2) | 0.0068 (16) |
C1 | 0.050 (2) | 0.033 (2) | 0.051 (3) | −0.0051 (18) | 0.012 (2) | −0.0029 (19) |
C2 | 0.060 (3) | 0.072 (3) | 0.065 (3) | −0.016 (2) | 0.014 (3) | 0.006 (3) |
C3 | 0.086 (4) | 0.078 (4) | 0.079 (4) | −0.027 (3) | 0.034 (4) | 0.002 (3) |
C4 | 0.122 (5) | 0.074 (4) | 0.065 (4) | −0.022 (4) | 0.039 (4) | 0.007 (3) |
C5 | 0.114 (5) | 0.069 (4) | 0.059 (3) | 0.005 (3) | 0.001 (3) | 0.017 (3) |
C6 | 0.060 (3) | 0.062 (3) | 0.062 (3) | −0.001 (2) | 0.007 (3) | 0.011 (3) |
C7 | 0.043 (2) | 0.032 (2) | 0.045 (2) | −0.0035 (17) | 0.0051 (19) | −0.0045 (18) |
C8 | 0.076 (3) | 0.035 (2) | 0.049 (3) | −0.006 (2) | 0.006 (2) | −0.005 (2) |
C9 | 0.104 (4) | 0.054 (3) | 0.044 (3) | −0.008 (3) | 0.014 (3) | −0.012 (2) |
C10 | 0.088 (4) | 0.055 (3) | 0.060 (3) | −0.014 (3) | 0.016 (3) | −0.023 (3) |
C11 | 0.099 (4) | 0.037 (3) | 0.067 (3) | −0.011 (2) | 0.016 (3) | −0.007 (2) |
C12 | 0.079 (3) | 0.040 (3) | 0.054 (3) | −0.003 (2) | 0.007 (3) | −0.004 (2) |
C13 | 0.0393 (19) | 0.039 (2) | 0.047 (2) | 0.0029 (16) | 0.0079 (19) | −0.0054 (18) |
C14 | 0.0347 (19) | 0.050 (3) | 0.049 (2) | 0.0002 (18) | 0.0025 (19) | −0.001 (2) |
C15 | 0.061 (3) | 0.070 (3) | 0.062 (3) | 0.019 (2) | −0.009 (3) | −0.016 (3) |
C16 | 0.090 (4) | 0.123 (5) | 0.057 (3) | 0.032 (4) | −0.014 (3) | −0.028 (4) |
C17 | 0.092 (4) | 0.116 (5) | 0.062 (4) | 0.035 (4) | −0.006 (3) | 0.006 (4) |
C18 | 0.074 (3) | 0.071 (4) | 0.076 (4) | 0.020 (3) | −0.013 (3) | 0.010 (3) |
C19 | 0.055 (3) | 0.048 (3) | 0.062 (3) | 0.008 (2) | −0.002 (2) | −0.006 (2) |
C20 | 0.044 (2) | 0.041 (2) | 0.070 (3) | 0.0045 (18) | 0.023 (2) | 0.004 (2) |
C21 | 0.042 (2) | 0.067 (3) | 0.097 (4) | −0.006 (2) | 0.024 (3) | −0.005 (3) |
C22 | 0.047 (3) | 0.115 (5) | 0.128 (6) | −0.013 (3) | 0.029 (4) | −0.005 (4) |
C23 | 0.088 (5) | 0.119 (5) | 0.151 (7) | 0.018 (4) | 0.077 (5) | 0.040 (5) |
C24 | 0.099 (5) | 0.164 (7) | 0.120 (6) | 0.044 (5) | 0.060 (5) | 0.069 (5) |
C25 | 0.057 (3) | 0.122 (5) | 0.082 (4) | 0.021 (3) | 0.027 (3) | 0.033 (3) |
C26 | 0.040 (2) | 0.034 (2) | 0.048 (2) | 0.0044 (16) | −0.0027 (19) | −0.0037 (18) |
C27 | 0.039 (2) | 0.044 (3) | 0.074 (3) | 0.0042 (19) | 0.004 (2) | 0.010 (2) |
C28 | 0.047 (2) | 0.046 (3) | 0.079 (3) | −0.004 (2) | 0.004 (2) | 0.012 (2) |
C29 | 0.058 (3) | 0.036 (2) | 0.064 (3) | −0.004 (2) | −0.010 (2) | 0.001 (2) |
C30 | 0.059 (3) | 0.046 (3) | 0.066 (3) | 0.022 (2) | −0.002 (2) | −0.003 (2) |
C31 | 0.049 (2) | 0.053 (3) | 0.054 (3) | 0.010 (2) | 0.008 (2) | 0.000 (2) |
C32 | 0.044 (2) | 0.042 (2) | 0.042 (2) | 0.0084 (18) | 0.0006 (19) | 0.0015 (19) |
C33 | 0.048 (2) | 0.054 (3) | 0.060 (3) | 0.008 (2) | 0.000 (2) | −0.005 (2) |
C34 | 0.073 (3) | 0.061 (3) | 0.056 (3) | 0.015 (2) | −0.002 (3) | −0.011 (2) |
C35 | 0.066 (3) | 0.059 (3) | 0.049 (3) | 0.023 (2) | 0.007 (2) | 0.007 (2) |
C36 | 0.050 (2) | 0.073 (3) | 0.056 (3) | 0.012 (2) | 0.009 (2) | 0.004 (3) |
C37 | 0.045 (2) | 0.063 (3) | 0.050 (3) | 0.006 (2) | 0.002 (2) | −0.001 (2) |
C38 | 0.0327 (18) | 0.044 (2) | 0.049 (2) | 0.0033 (16) | 0.0085 (18) | −0.0028 (19) |
C39 | 0.046 (2) | 0.056 (3) | 0.059 (3) | −0.008 (2) | 0.002 (2) | 0.000 (2) |
C40 | 0.044 (2) | 0.057 (3) | 0.076 (3) | −0.014 (2) | 0.013 (2) | −0.010 (3) |
C41 | 0.041 (2) | 0.074 (3) | 0.061 (3) | 0.000 (2) | 0.012 (2) | −0.024 (3) |
C42 | 0.058 (3) | 0.073 (3) | 0.045 (3) | 0.007 (2) | 0.002 (2) | −0.012 (2) |
C43 | 0.050 (2) | 0.053 (3) | 0.046 (2) | 0.005 (2) | 0.012 (2) | −0.002 (2) |
C44 | 0.043 (2) | 0.049 (3) | 0.063 (3) | −0.0051 (19) | 0.003 (2) | −0.013 (2) |
C45 | 0.047 (2) | 0.057 (3) | 0.067 (3) | 0.002 (2) | −0.003 (2) | −0.016 (2) |
C46 | 0.058 (3) | 0.040 (3) | 0.056 (3) | −0.0021 (19) | 0.005 (2) | −0.004 (2) |
C47 | 0.042 (2) | 0.038 (2) | 0.070 (3) | 0.0010 (18) | 0.008 (2) | 0.000 (2) |
C48 | 0.040 (2) | 0.047 (3) | 0.069 (3) | 0.0006 (19) | 0.005 (2) | −0.010 (2) |
C49 | 0.040 (2) | 0.046 (3) | 0.057 (3) | 0.0082 (18) | 0.006 (2) | −0.005 (2) |
C50 | 0.047 (2) | 0.042 (2) | 0.056 (3) | 0.0095 (19) | −0.001 (2) | −0.002 (2) |
C51 | 0.042 (2) | 0.043 (3) | 0.064 (3) | 0.0014 (19) | −0.003 (2) | 0.004 (2) |
C52 | 0.050 (2) | 0.049 (3) | 0.052 (3) | 0.0040 (19) | 0.005 (2) | −0.005 (2) |
C53 | 0.092 (4) | 0.047 (3) | 0.104 (4) | −0.001 (3) | −0.003 (4) | 0.017 (3) |
C54 | 0.103 (4) | 0.103 (4) | 0.052 (3) | 0.046 (3) | 0.020 (3) | 0.009 (3) |
C55 | 0.073 (4) | 0.121 (5) | 0.092 (4) | −0.037 (3) | 0.017 (3) | −0.057 (4) |
Ru1—C45 | 1.890 (5) | C16—C17 | 1.378 (7) |
Ru1—C46 | 1.915 (4) | C16—H16A | 0.9300 |
Ru1—C44 | 1.922 (4) | C17—C18 | 1.378 (7) |
Ru1—As1 | 2.4391 (5) | C17—H17A | 0.9300 |
Ru1—Ru2 | 2.8539 (4) | C18—C19 | 1.373 (6) |
Ru1—Ru3 | 2.8790 (4) | C18—H18A | 0.9300 |
Ru2—C48 | 1.884 (5) | C19—H19A | 0.9300 |
Ru2—C47 | 1.925 (4) | C20—C25 | 1.352 (7) |
Ru2—C49 | 1.929 (4) | C20—C21 | 1.374 (6) |
Ru2—As2 | 2.4460 (4) | C21—C22 | 1.380 (6) |
Ru2—Ru3 | 2.8460 (4) | C21—H21A | 0.9300 |
Ru3—C51 | 1.876 (5) | C22—C23 | 1.348 (9) |
Ru3—C52 | 1.904 (4) | C22—H22A | 0.9300 |
Ru3—C50 | 1.931 (5) | C23—C24 | 1.368 (10) |
Ru3—P1 | 2.3513 (10) | C23—H23A | 0.9300 |
As1—C1 | 1.938 (4) | C24—C25 | 1.410 (7) |
As1—C7 | 1.946 (4) | C24—H24A | 0.9300 |
As1—C13 | 1.958 (3) | C25—H25A | 0.9300 |
As2—C14 | 1.947 (4) | C26—C31 | 1.390 (5) |
As2—C20 | 1.948 (3) | C26—C27 | 1.397 (5) |
As2—C13 | 1.968 (4) | C27—C28 | 1.386 (5) |
P1—C38 | 1.831 (4) | C27—H27A | 0.9300 |
P1—C26 | 1.839 (4) | C28—C29 | 1.374 (6) |
P1—C32 | 1.842 (4) | C28—H28A | 0.9300 |
O1—C44 | 1.151 (5) | C29—C30 | 1.379 (6) |
O2—C45 | 1.138 (5) | C29—C53 | 1.523 (6) |
O3—C46 | 1.151 (4) | C30—C31 | 1.389 (5) |
O4—C47 | 1.144 (5) | C30—H30A | 0.9300 |
O5—C48 | 1.141 (5) | C31—H31A | 0.9300 |
O6—C49 | 1.135 (5) | C32—C33 | 1.379 (6) |
O7—C50 | 1.151 (5) | C32—C37 | 1.382 (5) |
O8—C51 | 1.134 (5) | C33—C34 | 1.389 (6) |
O9—C52 | 1.168 (5) | C33—H33A | 0.9300 |
C1—C6 | 1.362 (6) | C34—C35 | 1.383 (6) |
C1—C2 | 1.385 (5) | C34—H34A | 0.9300 |
C2—C3 | 1.381 (6) | C35—C36 | 1.370 (6) |
C2—H2A | 0.9300 | C35—C54 | 1.514 (6) |
C3—C4 | 1.350 (7) | C36—C37 | 1.385 (5) |
C3—H3A | 0.9300 | C36—H36A | 0.9300 |
C4—C5 | 1.379 (8) | C37—H37A | 0.9300 |
C4—H4A | 0.9300 | C38—C43 | 1.366 (5) |
C5—C6 | 1.384 (6) | C38—C39 | 1.392 (5) |
C5—H5A | 0.9300 | C39—C40 | 1.383 (6) |
C6—H6A | 0.9300 | C39—H39A | 0.9300 |
C7—C12 | 1.376 (5) | C40—C41 | 1.374 (6) |
C7—C8 | 1.376 (5) | C40—H40A | 0.9300 |
C8—C9 | 1.383 (6) | C41—C42 | 1.379 (6) |
C8—H8A | 0.9300 | C41—C55 | 1.508 (6) |
C9—C10 | 1.363 (6) | C42—C43 | 1.388 (6) |
C9—H9A | 0.9300 | C42—H42A | 0.9300 |
C10—C11 | 1.366 (6) | C43—H43A | 0.9300 |
C10—H10A | 0.9300 | C53—H53A | 0.9600 |
C11—C12 | 1.381 (6) | C53—H53B | 0.9600 |
C11—H11A | 0.9300 | C53—H53C | 0.9600 |
C12—H12A | 0.9300 | C54—H54A | 0.9600 |
C13—H13A | 0.9700 | C54—H54B | 0.9600 |
C13—H13B | 0.9700 | C54—H54C | 0.9600 |
C14—C19 | 1.382 (5) | C55—H55A | 0.9600 |
C14—C15 | 1.386 (6) | C55—H55B | 0.9600 |
C15—C16 | 1.372 (7) | C55—H55C | 0.9600 |
C15—H15A | 0.9300 | ||
C45—Ru1—C46 | 90.09 (19) | C15—C16—C17 | 121.0 (5) |
C45—Ru1—C44 | 92.37 (18) | C15—C16—H16A | 119.5 |
C46—Ru1—C44 | 176.30 (17) | C17—C16—H16A | 119.5 |
C45—Ru1—As1 | 102.18 (14) | C16—C17—C18 | 118.7 (5) |
C46—Ru1—As1 | 89.88 (12) | C16—C17—H17A | 120.7 |
C44—Ru1—As1 | 92.30 (12) | C18—C17—H17A | 120.7 |
C45—Ru1—Ru2 | 164.91 (15) | C19—C18—C17 | 120.5 (5) |
C46—Ru1—Ru2 | 82.81 (13) | C19—C18—H18A | 119.8 |
C44—Ru1—Ru2 | 94.15 (13) | C17—C18—H18A | 119.8 |
As1—Ru1—Ru2 | 91.150 (15) | C18—C19—C14 | 121.2 (4) |
C45—Ru1—Ru3 | 109.60 (13) | C18—C19—H19A | 119.4 |
C46—Ru1—Ru3 | 102.50 (12) | C14—C19—H19A | 119.4 |
C44—Ru1—Ru3 | 74.06 (12) | C25—C20—C21 | 120.1 (4) |
As1—Ru1—Ru3 | 145.659 (18) | C25—C20—As2 | 118.8 (3) |
Ru2—Ru1—Ru3 | 59.526 (10) | C21—C20—As2 | 121.0 (4) |
C48—Ru2—C47 | 88.73 (18) | C20—C21—C22 | 120.1 (5) |
C48—Ru2—C49 | 93.74 (18) | C20—C21—H21A | 120.0 |
C47—Ru2—C49 | 174.99 (17) | C22—C21—H21A | 120.0 |
C48—Ru2—As2 | 102.71 (12) | C23—C22—C21 | 120.0 (6) |
C47—Ru2—As2 | 94.85 (11) | C23—C22—H22A | 120.0 |
C49—Ru2—As2 | 88.86 (11) | C21—C22—H22A | 120.0 |
C48—Ru2—Ru3 | 100.48 (12) | C22—C23—C24 | 121.1 (5) |
C47—Ru2—Ru3 | 85.69 (12) | C22—C23—H23A | 119.5 |
C49—Ru2—Ru3 | 89.58 (11) | C24—C23—H23A | 119.5 |
As2—Ru2—Ru3 | 156.811 (17) | C23—C24—C25 | 118.7 (6) |
C48—Ru2—Ru1 | 160.83 (12) | C23—C24—H24A | 120.6 |
C47—Ru2—Ru1 | 92.99 (13) | C25—C24—H24A | 120.6 |
C49—Ru2—Ru1 | 83.26 (13) | C20—C25—C24 | 120.0 (5) |
As2—Ru2—Ru1 | 96.175 (14) | C20—C25—H25A | 120.0 |
Ru3—Ru2—Ru1 | 60.675 (11) | C24—C25—H25A | 120.0 |
C51—Ru3—C52 | 99.79 (18) | C31—C26—C27 | 117.3 (4) |
C51—Ru3—C50 | 94.40 (18) | C31—C26—P1 | 120.9 (3) |
C52—Ru3—C50 | 165.73 (17) | C27—C26—P1 | 121.6 (3) |
C51—Ru3—P1 | 96.29 (12) | C28—C27—C26 | 120.9 (4) |
C52—Ru3—P1 | 88.70 (13) | C28—C27—H27A | 119.6 |
C50—Ru3—P1 | 91.23 (12) | C26—C27—H27A | 119.6 |
C51—Ru3—Ru2 | 87.81 (12) | C29—C28—C27 | 121.6 (4) |
C52—Ru3—Ru2 | 90.27 (12) | C29—C28—H28A | 119.2 |
C50—Ru3—Ru2 | 88.79 (12) | C27—C28—H28A | 119.2 |
P1—Ru3—Ru2 | 175.88 (3) | C28—C29—C30 | 117.8 (4) |
C51—Ru3—Ru1 | 143.77 (12) | C28—C29—C53 | 120.9 (4) |
C52—Ru3—Ru1 | 67.23 (12) | C30—C29—C53 | 121.2 (4) |
C50—Ru3—Ru1 | 100.20 (12) | C29—C30—C31 | 121.5 (4) |
P1—Ru3—Ru1 | 116.18 (3) | C29—C30—H30A | 119.2 |
Ru2—Ru3—Ru1 | 59.798 (10) | C31—C30—H30A | 119.2 |
C1—As1—C7 | 100.67 (16) | C30—C31—C26 | 120.8 (4) |
C1—As1—C13 | 105.80 (17) | C30—C31—H31A | 119.6 |
C7—As1—C13 | 98.57 (15) | C26—C31—H31A | 119.6 |
C1—As1—Ru1 | 117.32 (11) | C33—C32—C37 | 118.0 (4) |
C7—As1—Ru1 | 118.18 (12) | C33—C32—P1 | 118.3 (3) |
C13—As1—Ru1 | 113.78 (11) | C37—C32—P1 | 123.6 (3) |
C14—As2—C20 | 102.02 (17) | C32—C33—C34 | 120.9 (4) |
C14—As2—C13 | 103.76 (17) | C32—C33—H33A | 119.6 |
C20—As2—C13 | 101.59 (16) | C34—C33—H33A | 119.6 |
C14—As2—Ru2 | 116.77 (11) | C35—C34—C33 | 121.1 (5) |
C20—As2—Ru2 | 117.12 (12) | C35—C34—H34A | 119.4 |
C13—As2—Ru2 | 113.51 (11) | C33—C34—H34A | 119.4 |
C38—P1—C26 | 102.54 (18) | C36—C35—C34 | 117.6 (4) |
C38—P1—C32 | 103.69 (17) | C36—C35—C54 | 121.1 (4) |
C26—P1—C32 | 101.05 (16) | C34—C35—C54 | 121.4 (5) |
C38—P1—Ru3 | 114.60 (12) | C35—C36—C37 | 121.8 (4) |
C26—P1—Ru3 | 116.66 (12) | C35—C36—H36A | 119.1 |
C32—P1—Ru3 | 116.26 (13) | C37—C36—H36A | 119.1 |
C6—C1—C2 | 118.4 (4) | C32—C37—C36 | 120.6 (4) |
C6—C1—As1 | 124.8 (3) | C32—C37—H37A | 119.7 |
C2—C1—As1 | 116.8 (3) | C36—C37—H37A | 119.7 |
C3—C2—C1 | 120.7 (5) | C43—C38—C39 | 117.8 (4) |
C3—C2—H2A | 119.7 | C43—C38—P1 | 122.3 (3) |
C1—C2—H2A | 119.7 | C39—C38—P1 | 119.8 (3) |
C4—C3—C2 | 120.1 (5) | C40—C39—C38 | 121.0 (4) |
C4—C3—H3A | 120.0 | C40—C39—H39A | 119.5 |
C2—C3—H3A | 120.0 | C38—C39—H39A | 119.5 |
C3—C4—C5 | 120.4 (5) | C41—C40—C39 | 121.1 (4) |
C3—C4—H4A | 119.8 | C41—C40—H40A | 119.4 |
C5—C4—H4A | 119.8 | C39—C40—H40A | 119.4 |
C4—C5—C6 | 119.2 (6) | C40—C41—C42 | 117.6 (4) |
C4—C5—H5A | 120.4 | C40—C41—C55 | 122.0 (5) |
C6—C5—H5A | 120.4 | C42—C41—C55 | 120.3 (5) |
C1—C6—C5 | 121.3 (5) | C41—C42—C43 | 121.4 (4) |
C1—C6—H6A | 119.4 | C41—C42—H42A | 119.3 |
C5—C6—H6A | 119.4 | C43—C42—H42A | 119.3 |
C12—C7—C8 | 118.3 (4) | C38—C43—C42 | 121.0 (4) |
C12—C7—As1 | 122.6 (3) | C38—C43—H43A | 119.5 |
C8—C7—As1 | 119.1 (3) | C42—C43—H43A | 119.5 |
C7—C8—C9 | 121.6 (4) | O1—C44—Ru1 | 170.0 (4) |
C7—C8—H8A | 119.2 | O2—C45—Ru1 | 175.8 (4) |
C9—C8—H8A | 119.2 | O3—C46—Ru1 | 174.2 (4) |
C10—C9—C8 | 119.3 (4) | O4—C47—Ru2 | 175.0 (4) |
C10—C9—H9A | 120.4 | O5—C48—Ru2 | 176.5 (4) |
C8—C9—H9A | 120.4 | O6—C49—Ru2 | 174.9 (4) |
C9—C10—C11 | 119.9 (4) | O7—C50—Ru3 | 176.5 (4) |
C9—C10—H10A | 120.1 | O8—C51—Ru3 | 177.7 (4) |
C11—C10—H10A | 120.1 | O9—C52—Ru3 | 167.5 (4) |
C10—C11—C12 | 120.9 (4) | C29—C53—H53A | 109.5 |
C10—C11—H11A | 119.6 | C29—C53—H53B | 109.5 |
C12—C11—H11A | 119.6 | H53A—C53—H53B | 109.5 |
C7—C12—C11 | 120.0 (4) | C29—C53—H53C | 109.5 |
C7—C12—H12A | 120.0 | H53A—C53—H53C | 109.5 |
C11—C12—H12A | 120.0 | H53B—C53—H53C | 109.5 |
As1—C13—As2 | 113.29 (16) | C35—C54—H54A | 109.5 |
As1—C13—H13A | 108.9 | C35—C54—H54B | 109.5 |
As2—C13—H13A | 108.9 | H54A—C54—H54B | 109.5 |
As1—C13—H13B | 108.9 | C35—C54—H54C | 109.5 |
As2—C13—H13B | 108.9 | H54A—C54—H54C | 109.5 |
H13A—C13—H13B | 107.7 | H54B—C54—H54C | 109.5 |
C19—C14—C15 | 118.0 (4) | C41—C55—H55A | 109.5 |
C19—C14—As2 | 123.0 (3) | C41—C55—H55B | 109.5 |
C15—C14—As2 | 119.0 (3) | H55A—C55—H55B | 109.5 |
C16—C15—C14 | 120.6 (5) | C41—C55—H55C | 109.5 |
C16—C15—H15A | 119.7 | H55A—C55—H55C | 109.5 |
C14—C15—H15A | 119.7 | H55B—C55—H55C | 109.5 |
C45—Ru1—Ru2—C48 | −58.0 (6) | Ru1—As1—C1—C2 | −62.2 (3) |
C46—Ru1—Ru2—C48 | −120.5 (4) | C6—C1—C2—C3 | 0.0 (7) |
C44—Ru1—Ru2—C48 | 57.4 (4) | As1—C1—C2—C3 | −179.6 (4) |
As1—Ru1—Ru2—C48 | 149.8 (4) | C1—C2—C3—C4 | 0.2 (8) |
Ru3—Ru1—Ru2—C48 | −11.4 (4) | C2—C3—C4—C5 | −0.7 (9) |
C45—Ru1—Ru2—C47 | 36.8 (5) | C3—C4—C5—C6 | 1.0 (8) |
C46—Ru1—Ru2—C47 | −25.75 (17) | C2—C1—C6—C5 | 0.3 (7) |
C44—Ru1—Ru2—C47 | 152.12 (17) | As1—C1—C6—C5 | 180.0 (4) |
As1—Ru1—Ru2—C47 | −115.48 (11) | C4—C5—C6—C1 | −0.8 (8) |
Ru3—Ru1—Ru2—C47 | 83.36 (11) | C1—As1—C7—C12 | 20.0 (4) |
C45—Ru1—Ru2—C49 | −139.9 (5) | C13—As1—C7—C12 | −88.0 (3) |
C46—Ru1—Ru2—C49 | 157.58 (16) | Ru1—As1—C7—C12 | 149.1 (3) |
C44—Ru1—Ru2—C49 | −24.55 (17) | C1—As1—C7—C8 | −162.4 (3) |
As1—Ru1—Ru2—C49 | 67.84 (11) | C13—As1—C7—C8 | 89.6 (3) |
Ru3—Ru1—Ru2—C49 | −93.32 (11) | Ru1—As1—C7—C8 | −33.3 (4) |
C45—Ru1—Ru2—As2 | 132.0 (5) | C12—C7—C8—C9 | 0.1 (6) |
C46—Ru1—Ru2—As2 | 69.46 (12) | As1—C7—C8—C9 | −177.5 (3) |
C44—Ru1—Ru2—As2 | −112.67 (12) | C7—C8—C9—C10 | −0.6 (7) |
As1—Ru1—Ru2—As2 | −20.274 (16) | C8—C9—C10—C11 | 0.3 (8) |
Ru3—Ru1—Ru2—As2 | 178.567 (15) | C9—C10—C11—C12 | 0.4 (8) |
C45—Ru1—Ru2—Ru3 | −46.6 (5) | C8—C7—C12—C11 | 0.6 (6) |
C46—Ru1—Ru2—Ru3 | −109.10 (12) | As1—C7—C12—C11 | 178.2 (3) |
C44—Ru1—Ru2—Ru3 | 68.77 (12) | C10—C11—C12—C7 | −0.9 (7) |
As1—Ru1—Ru2—Ru3 | 161.159 (15) | C1—As1—C13—As2 | 93.4 (2) |
C48—Ru2—Ru3—C51 | −20.78 (19) | C7—As1—C13—As2 | −162.9 (2) |
C47—Ru2—Ru3—C51 | 67.13 (18) | Ru1—As1—C13—As2 | −36.8 (2) |
C49—Ru2—Ru3—C51 | −114.50 (18) | C14—As2—C13—As1 | −110.8 (2) |
As2—Ru2—Ru3—C51 | 159.38 (14) | C20—As2—C13—As1 | 143.6 (2) |
Ru1—Ru2—Ru3—C51 | 163.00 (13) | Ru2—As2—C13—As1 | 16.9 (2) |
C48—Ru2—Ru3—C52 | −120.56 (19) | C20—As2—C14—C19 | 74.5 (3) |
C47—Ru2—Ru3—C52 | −32.66 (18) | C13—As2—C14—C19 | −30.8 (3) |
C49—Ru2—Ru3—C52 | 145.72 (18) | Ru2—As2—C14—C19 | −156.5 (3) |
As2—Ru2—Ru3—C52 | 59.59 (13) | C20—As2—C14—C15 | −105.4 (3) |
Ru1—Ru2—Ru3—C52 | 63.21 (13) | C13—As2—C14—C15 | 149.3 (3) |
C48—Ru2—Ru3—C50 | 73.68 (18) | Ru2—As2—C14—C15 | 23.6 (4) |
C47—Ru2—Ru3—C50 | 161.58 (18) | C19—C14—C15—C16 | 1.0 (7) |
C49—Ru2—Ru3—C50 | −20.05 (18) | As2—C14—C15—C16 | −179.1 (4) |
As2—Ru2—Ru3—C50 | −106.17 (13) | C14—C15—C16—C17 | 0.8 (8) |
Ru1—Ru2—Ru3—C50 | −102.55 (12) | C15—C16—C17—C18 | −1.2 (9) |
C48—Ru2—Ru3—Ru1 | 176.22 (13) | C16—C17—C18—C19 | −0.3 (9) |
C47—Ru2—Ru3—Ru1 | −95.87 (13) | C17—C18—C19—C14 | 2.2 (8) |
C49—Ru2—Ru3—Ru1 | 82.50 (12) | C15—C14—C19—C18 | −2.5 (6) |
As2—Ru2—Ru3—Ru1 | −3.62 (4) | As2—C14—C19—C18 | 177.6 (3) |
C45—Ru1—Ru3—C51 | 138.8 (3) | C14—As2—C20—C25 | −172.9 (4) |
C46—Ru1—Ru3—C51 | 44.2 (3) | C13—As2—C20—C25 | −66.0 (4) |
C44—Ru1—Ru3—C51 | −134.4 (3) | Ru2—As2—C20—C25 | 58.3 (4) |
As1—Ru1—Ru3—C51 | −64.5 (2) | C14—As2—C20—C21 | 10.7 (4) |
Ru2—Ru1—Ru3—C51 | −29.6 (2) | C13—As2—C20—C21 | 117.7 (4) |
C45—Ru1—Ru3—C52 | 63.9 (2) | Ru2—As2—C20—C21 | −118.1 (3) |
C46—Ru1—Ru3—C52 | −30.7 (2) | C25—C20—C21—C22 | −2.8 (7) |
C44—Ru1—Ru3—C52 | 150.7 (2) | As2—C20—C21—C22 | 173.5 (4) |
As1—Ru1—Ru3—C52 | −139.41 (14) | C20—C21—C22—C23 | 0.7 (9) |
Ru2—Ru1—Ru3—C52 | −104.50 (14) | C21—C22—C23—C24 | 2.0 (11) |
C45—Ru1—Ru3—C50 | −109.03 (19) | C22—C23—C24—C25 | −2.6 (11) |
C46—Ru1—Ru3—C50 | 156.34 (19) | C21—C20—C25—C24 | 2.2 (8) |
C44—Ru1—Ru3—C50 | −22.24 (18) | As2—C20—C25—C24 | −174.2 (5) |
As1—Ru1—Ru3—C50 | 47.64 (13) | C23—C24—C25—C20 | 0.5 (10) |
Ru2—Ru1—Ru3—C50 | 82.55 (13) | C38—P1—C26—C31 | −73.2 (4) |
C45—Ru1—Ru3—P1 | −12.55 (15) | C32—P1—C26—C31 | 33.7 (4) |
C46—Ru1—Ru3—P1 | −107.18 (14) | Ru3—P1—C26—C31 | 160.7 (3) |
C44—Ru1—Ru3—P1 | 74.23 (14) | C38—P1—C26—C27 | 102.0 (4) |
As1—Ru1—Ru3—P1 | 144.11 (4) | C32—P1—C26—C27 | −151.1 (3) |
Ru2—Ru1—Ru3—P1 | 179.02 (3) | Ru3—P1—C26—C27 | −24.1 (4) |
C45—Ru1—Ru3—Ru2 | 168.42 (15) | C31—C26—C27—C28 | 1.5 (6) |
C46—Ru1—Ru3—Ru2 | 73.79 (14) | P1—C26—C27—C28 | −173.9 (4) |
C44—Ru1—Ru3—Ru2 | −104.80 (14) | C26—C27—C28—C29 | −2.1 (7) |
As1—Ru1—Ru3—Ru2 | −34.91 (2) | C27—C28—C29—C30 | 1.0 (7) |
C45—Ru1—As1—C1 | 97.1 (2) | C27—C28—C29—C53 | 179.1 (4) |
C46—Ru1—As1—C1 | −172.78 (19) | C28—C29—C30—C31 | 0.7 (7) |
C44—Ru1—As1—C1 | 4.23 (19) | C53—C29—C30—C31 | −177.4 (4) |
Ru2—Ru1—As1—C1 | −89.97 (14) | C29—C30—C31—C26 | −1.2 (7) |
Ru3—Ru1—As1—C1 | −60.41 (14) | C27—C26—C31—C30 | 0.1 (6) |
C45—Ru1—As1—C7 | −23.72 (18) | P1—C26—C31—C30 | 175.5 (3) |
C46—Ru1—As1—C7 | 66.35 (18) | C38—P1—C32—C33 | −172.6 (3) |
C44—Ru1—As1—C7 | −116.65 (17) | C26—P1—C32—C33 | 81.4 (3) |
Ru2—Ru1—As1—C7 | 149.15 (11) | Ru3—P1—C32—C33 | −45.9 (4) |
Ru3—Ru1—As1—C7 | 178.72 (11) | C38—P1—C32—C37 | 10.7 (4) |
C45—Ru1—As1—C13 | −138.62 (18) | C26—P1—C32—C37 | −95.3 (4) |
C46—Ru1—As1—C13 | −48.55 (18) | Ru3—P1—C32—C37 | 137.4 (3) |
C44—Ru1—As1—C13 | 128.46 (18) | C37—C32—C33—C34 | −1.4 (6) |
Ru2—Ru1—As1—C13 | 34.26 (12) | P1—C32—C33—C34 | −178.3 (3) |
Ru3—Ru1—As1—C13 | 63.83 (13) | C32—C33—C34—C35 | 0.7 (7) |
C48—Ru2—As2—C14 | −50.20 (18) | C33—C34—C35—C36 | 0.7 (7) |
C47—Ru2—As2—C14 | −139.99 (18) | C33—C34—C35—C54 | −179.6 (4) |
C49—Ru2—As2—C14 | 43.38 (18) | C34—C35—C36—C37 | −1.3 (7) |
Ru3—Ru2—As2—C14 | 129.64 (13) | C54—C35—C36—C37 | 179.0 (4) |
Ru1—Ru2—As2—C14 | 126.47 (12) | C33—C32—C37—C36 | 0.8 (6) |
C48—Ru2—As2—C20 | 71.2 (2) | P1—C32—C37—C36 | 177.5 (3) |
C47—Ru2—As2—C20 | −18.6 (2) | C35—C36—C37—C32 | 0.6 (7) |
C49—Ru2—As2—C20 | 164.7 (2) | C26—P1—C38—C43 | −19.2 (3) |
Ru3—Ru2—As2—C20 | −108.99 (16) | C32—P1—C38—C43 | −124.1 (3) |
Ru1—Ru2—As2—C20 | −112.17 (16) | Ru3—P1—C38—C43 | 108.2 (3) |
C48—Ru2—As2—C13 | −170.87 (18) | C26—P1—C38—C39 | 165.4 (3) |
C47—Ru2—As2—C13 | 99.34 (18) | C32—P1—C38—C39 | 60.5 (3) |
C49—Ru2—As2—C13 | −77.29 (17) | Ru3—P1—C38—C39 | −67.3 (3) |
Ru3—Ru2—As2—C13 | 8.97 (13) | C43—C38—C39—C40 | 1.3 (6) |
Ru1—Ru2—As2—C13 | 5.80 (12) | P1—C38—C39—C40 | 176.9 (3) |
C51—Ru3—P1—C38 | −158.16 (19) | C38—C39—C40—C41 | −1.3 (6) |
C52—Ru3—P1—C38 | −58.46 (18) | C39—C40—C41—C42 | 0.8 (6) |
C50—Ru3—P1—C38 | 107.27 (18) | C39—C40—C41—C55 | −177.9 (4) |
Ru1—Ru3—P1—C38 | 5.28 (14) | C40—C41—C42—C43 | −0.2 (6) |
C51—Ru3—P1—C26 | −38.36 (19) | C55—C41—C42—C43 | 178.5 (4) |
C52—Ru3—P1—C26 | 61.34 (19) | C39—C38—C43—C42 | −0.7 (5) |
C50—Ru3—P1—C26 | −132.93 (19) | P1—C38—C43—C42 | −176.2 (3) |
Ru1—Ru3—P1—C26 | 125.07 (14) | C41—C42—C43—C38 | 0.2 (6) |
C51—Ru3—P1—C32 | 80.77 (19) | C45—Ru1—C44—O1 | −52 (2) |
C52—Ru3—P1—C32 | −179.52 (19) | As1—Ru1—C44—O1 | 50 (2) |
C50—Ru3—P1—C32 | −13.79 (19) | Ru2—Ru1—C44—O1 | 141 (2) |
Ru1—Ru3—P1—C32 | −115.79 (14) | Ru3—Ru1—C44—O1 | −162 (2) |
C7—As1—C1—C6 | −112.1 (4) | C51—Ru3—C52—O9 | 49.9 (18) |
C13—As1—C1—C6 | −9.9 (4) | C50—Ru3—C52—O9 | −136.1 (16) |
Ru1—As1—C1—C6 | 118.2 (3) | P1—Ru3—C52—O9 | −46.3 (18) |
C7—As1—C1—C2 | 67.5 (3) | Ru2—Ru3—C52—O9 | 137.7 (18) |
C13—As1—C1—C2 | 169.7 (3) | Ru1—Ru3—C52—O9 | −165.5 (19) |
D—H···A | D—H | H···A | D···A | D—H···A |
C27—H27A···O9 | 0.93 | 2.57 | 3.317 (5) | 138 |
C54—H54A···O2i | 0.96 | 2.60 | 3.306 (6) | 131 |
Symmetry code: (i) −x+1, y−1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Ru3(C25H22As2)(C21H21P)(CO)9] |
Mr | 1331.91 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 296 |
a, b, c (Å) | 16.2585 (2), 16.9247 (2), 19.6900 (2) |
β (°) | 98.680 (1) |
V (Å3) | 5356.05 (11) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.15 |
Crystal size (mm) | 0.21 × 0.21 × 0.03 |
Data collection | |
Diffractometer | Bruker SMART APEXII CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2005) |
Tmin, Tmax | 0.665, 0.933 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 63277, 15703, 9536 |
Rint | 0.063 |
(sin θ/λ)max (Å−1) | 0.706 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.049, 0.096, 1.00 |
No. of reflections | 15703 |
No. of parameters | 634 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.60, −0.41 |
Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).
D—H···A | D—H | H···A | D···A | D—H···A |
C27—H27A···O9 | 0.9300 | 2.5700 | 3.317 (5) | 138.00 |
C54—H54A···O2i | 0.9600 | 2.6000 | 3.306 (6) | 131.00 |
Symmetry code: (i) −x+1, y−1/2, −z+1/2. |
Triangulo-triruthenium clusters are known for their interesting structural variations and related catalytic activity. A large number of substituted derivatives, Ru3(CO)12-nLn (L= group 15 ligand) have been reported (Bruce et al., 1985, 1988a,b). As part of our study on the substitution of transition metal-carbonyl clusters with mixed-ligand complexes, we have published several structures of triangulo-triruthenium-carbonyl clusters containing mixed P/As and P/Sb ligands (Shawkataly et al., 1998, 2004, 2009). Herein we report the synthesis and structure of Ru3(C21H21P)(C25H22As2)(CO)9.
The bond lengths and angles of title compound (Fig. 1) are comparable to those in related structures (Shawkataly et al., 2009). The bis(diphenylarsino)methane ligand bridges the Ru1—Ru2 bond and the monodentate phosphine ligand bonds to the Ru3 atom. Both the phosphine and arsine ligands are equatorial with respect to the Ru3 triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three phosphine substituted phenyl rings make dihedral angles (C26–C31/C32–C37, C26–C31/C38–C43 and C32–C37/C38–C43) of 86.89 (19), 82.1 (2) and 63.0 (2)° with each other respectively. The dihedral angles between the two phenyl rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 73.8 (2) and 82.2 (3)° for the two diphenylarsino groups respectively.
An intramolecular C27—H27A···O9 hydrogen bond stabilizes the molecular structure. In the crystal packing (Fig. 2), the molecules are linked together into chains via intermolecular C54—H54A···O2 hydrogen bonds along the b axis.