[μ-Bis(diphenyl­arsino)methane-1:2κ2As:As′][bis­(4-methoxy­phen­yl)phenyl­phosphine-3κP]-nona­carbonyl-1κ3C,2κ3C,3κ3C-triangulo-tri­ruthenium(0) dichloro­methane 0.15-solvate

Shawkataly, O. bin; Khan, I.A.; Yeap, C.S.; Fun, H.-K.

doi:10.1107/S1600536810001194

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 66| Part 2| February 2010| Pages m225-m226

https://doi.org/10.1107/S1600536810001194

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[μ-Bis(diphenylarsino)methane-1:2κ²As:As′][bis(4-methoxyphenyl)phenylphosphine-3κP]-nonacarbonyl-1κ³C,2κ³C,3κ³C-triangulo-triruthenium(0) dichloromethane 0.15-solvate

Omar bin Shawkataly,^a ^*‡ Imthyaz Ahmed Khan,^a Chin Sing Yeap ^b § and Hoong-Kun Fun ^b ¶

^aChemical Sciences Programme, School of Distance Education, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia, and ^bX-ray Crystallography Unit, School of Physics, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia
^*Correspondence e-mail: omarsa@usm.my

(Received 30 December 2009; accepted 10 January 2010; online 30 January 2010)

The asymmetric unit of the title triangulo-triruthenium compound, [Ru₃(C₂₅H₂₂As₂)(C₂₀H₁₉O₂P)(CO)₉]·0.15CH₂Cl₂, contains one molecule of the triangulo-triruthenium complex and one partially occupied dichloromethane solvent molecule. The dichloromethane solvent lies across a crystallographic inversion center leading to the molecule being disordered over two positions of equal occupancy. The bis(diphenylarsino)methane ligand bridges an Ru—Ru bond and the monodentate arsine ligand bonds to the third Ru atom. Both the arsine ligands are equatorial with respect to the Ru₃ triangle. In addition, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three phosphorus-bound benzene rings make dihedral angles of 72.7 (3), 80.9 (3) and 70.8 (2)° with each other. The dihedral angles between the two benzene rings are 79.9 (3) and 81.5 (2)° for the two diphenylarsino groups.

Related literature

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985 , 1988a ,b ). For related structures, see: Shawkataly et al. (1998 , 2004 , 2009 ). For the synthesis of μ-bis(diphenylarsino)methanedecacarbonyltriruthenium(0), see: Bruce et al. (1983 ).

Experimental

Crystal data

[Ru₃(C₂₅H₂₂As₂)(C₂₀H₁₉O₂P)(CO)₉]·0.15CH₂Cl₂
M_r = 1362.63
Monoclinic, P 2₁ /c
a = 13.3723 (4) Å
b = 16.9461 (6) Å
c = 25.0956 (8) Å
β = 93.293 (2)°
V = 5677.5 (3) Å³
Z = 4
Mo Kα radiation
μ = 2.04 mm⁻¹
T = 296 K
0.31 × 0.21 × 0.16 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2005 ) T_min = 0.571, T_max = 0.741
67215 measured reflections
16557 independent reflections
10503 reflections with I > 2σ(I)
R_int = 0.041

Refinement

R[F² > 2σ(F²)] = 0.039
wR(F²) = 0.121
S = 1.02
16557 reflections
654 parameters
3 restraints
H-atom parameters constrained
Δρ_max = 1.00 e Å⁻³
Δρ_min = −0.38 e Å⁻³

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810001194/tk2608sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810001194/tk2608Isup2.hkl

checkCIF report

Comment top

Triangulo-triruthenium clusters are known for their interesting structural variations and related catalytic activity. A large number of substituted derivatives, Ru₃(CO)_12-nL_n (L = group 15 ligand) have been reported (Bruce et al., 1988a,b; Bruce et al., 1985). 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 title compound.

The asymmetric unit consists of one molecule of the triangulo-triruthenium complex and a 15% partially occupied molecule of dichloromethyl solvent (Fig. 1). The dichloromethyl solvent lies across a crystallographic inversion center leading to the molecule being disordered over two positions of equal occupancy. The bond lengths and angles of title compound are comparable to those found in related structure (Shawkataly et al., 2009). The bis(diphenylarsino)methane ligand bridges the Ru1—Ru2 bond and the monodentate arsine ligand bonds to the Ru3 atom. Both the 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 benzene rings make dihedral angles (C26–C31/C32–C37, C26–C31/C38–C43 and C32–C37/C38–C43) of 72.7 (3), 80.9 (3) and 70.8 (2)° with each other respectively. The dihedral angles between the two benzene rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 79.9 (3) and 81.5 (2)° for the two diphenylarsino groups respectively. In the crystal structure, the molecules are stacked along the b axis (Fig. 2).

Related literature top

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985, 1988a,b). For related structures, see: Shawkataly et al. (1998, 2004, 2009). For the synthesis of µ-bis(diphenylarsino)methanedecacarbonyltriruthenium(0), see: Bruce et al. (1983).

Experimental top

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. Bis(4-methoxyphenyl)phenylphosphine (Maybridge) was used as received and µ-bis(diphenylarsino)methanedecacarbonyltriruthenium(0) was prepared by reported procedures (Bruce et al., 1983). The title compound was obtained by refluxing equimolar quantities of Ru₃(CO)₁₀(µ-Ph₂AsCH₂AsPh₂) (105.5 mg, 0.1 mmol) and bis(4-methoxyphenyl)phenylphosphine (32.23 mg, 0.1 mmol) in hexane under nitrogen atmosphere. Crystals were grown by slow solvent / solvent diffusion of CH₃OH into CH₂Cl₂.

Structure description top

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985, 1988a,b). For related structures, see: Shawkataly et al. (1998, 2004, 2009). For the synthesis of µ-bis(diphenylarsino)methanedecacarbonyltriruthenium(0), see: Bruce et al. (1983).

Computing details top

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).

Figures top

	Fig. 1. The molecular structure of the title compound with 20% probability ellipsoids for non-H atoms.
	Fig. 2. The crystal packing of the title compound, viewed down the b axis, showing the molecules stacked along b axis. Hydrogen atoms not involved in the hydrogen-bonding (dashed lines) and the solvent molecules have been omitted for clarity.

[µ-Bis(diphenylarsino)methane-1:2κ²As:As'][bis(4- methoxyphenyl)phenylphosphine-3κP]nonacarbonyl- 1κ³C,2κ³C,3κ³C–triangulo-triruthenium(0) dichloromethane 0.15-solvate top

Crystal data top

[Ru₃(C₂₅H₂₂As₂)(C₂₀H₁₉O₂P)(CO)₉]·0.15CH₂Cl₂	F(000) = 2689
M_r = 1362.63	D_x = 1.594 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9029 reflections
a = 13.3723 (4) Å	θ = 2.5–27.7°
b = 16.9461 (6) Å	µ = 2.04 mm⁻¹
c = 25.0956 (8) Å	T = 296 K
β = 93.293 (2)°	Block, purple
V = 5677.5 (3) Å³	0.31 × 0.21 × 0.16 mm
Z = 4

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	16557 independent reflections
Radiation source: fine-focus sealed tube	10503 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.041
φ and ω scans	θ_max = 30.0°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2005)	h = −18→13
T_min = 0.571, T_max = 0.741	k = −23→23
67215 measured reflections	l = −35→35

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)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.121	H-atom parameters constrained
S = 1.02	w = 1/[σ²(F_o²) + (0.0631P)² + 0.2919P] where P = (F_o² + 2F_c²)/3
16557 reflections	(Δ/σ)_max = 0.001
654 parameters	Δρ_max = 1.00 e Å⁻³
3 restraints	Δρ_min = −0.38 e Å⁻³

Crystal data top

[Ru₃(C₂₅H₂₂As₂)(C₂₀H₁₉O₂P)(CO)₉]·0.15CH₂Cl₂	V = 5677.5 (3) Å³
M_r = 1362.63	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 13.3723 (4) Å	µ = 2.04 mm⁻¹
b = 16.9461 (6) Å	T = 296 K
c = 25.0956 (8) Å	0.31 × 0.21 × 0.16 mm
β = 93.293 (2)°

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	16557 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2005)	10503 reflections with I > 2σ(I)
T_min = 0.571, T_max = 0.741	R_int = 0.041
67215 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.039	3 restraints
wR(F²) = 0.121	H-atom parameters constrained
S = 1.02	Δρ_max = 1.00 e Å⁻³
16557 reflections	Δρ_min = −0.38 e Å⁻³
654 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	Occ. (<1)
Ru1	0.23500 (2)	0.681950 (18)	0.163442 (13)	0.03901 (9)
Ru2	0.04906 (2)	0.755091 (17)	0.183146 (11)	0.03391 (8)
Ru3	0.19523 (2)	0.842925 (18)	0.130875 (12)	0.03573 (8)
As1	0.16685 (3)	0.55179 (2)	0.182877 (16)	0.03808 (10)
As2	−0.01950 (3)	0.64684 (2)	0.233294 (14)	0.03357 (9)
P1	0.31142 (7)	0.91113 (6)	0.08118 (4)	0.0403 (2)
O1	0.2778 (3)	0.6974 (2)	0.28428 (14)	0.0720 (10)
O2	0.4536 (3)	0.6481 (3)	0.1507 (2)	0.130 (2)
O3	0.1941 (3)	0.6619 (2)	0.04285 (14)	0.0723 (10)
O4	−0.0261 (2)	0.6678 (2)	0.08212 (13)	0.0656 (9)
O5	−0.1248 (3)	0.8700 (2)	0.17369 (18)	0.0905 (13)
O6	0.1308 (3)	0.8404 (2)	0.28432 (14)	0.0721 (10)
O7	0.3531 (2)	0.84785 (18)	0.22408 (14)	0.0652 (9)
O8	0.0740 (2)	0.98639 (19)	0.15749 (14)	0.0685 (9)
O9	0.0639 (3)	0.8144 (2)	0.02844 (14)	0.0824 (11)
O10	0.6764 (3)	0.7311 (2)	0.02742 (18)	0.1004 (14)
O11	0.4740 (3)	1.2156 (2)	0.17242 (16)	0.0889 (12)
C1	0.2580 (3)	0.4723 (2)	0.21440 (17)	0.0481 (10)
C2	0.2382 (4)	0.3932 (3)	0.2083 (2)	0.0716 (15)
H2A	0.1811	0.3768	0.1884	0.086*
C3	0.3043 (5)	0.3369 (3)	0.2320 (3)	0.0911 (19)
H3A	0.2912	0.2833	0.2277	0.109*
C4	0.3878 (4)	0.3614 (4)	0.2614 (3)	0.094 (2)
H4A	0.4324	0.3245	0.2765	0.112*
C5	0.4054 (4)	0.4390 (4)	0.2683 (3)	0.101 (2)
H5A	0.4611	0.4555	0.2893	0.121*
C6	0.3409 (4)	0.4949 (3)	0.2445 (2)	0.0832 (17)
H6A	0.3546	0.5483	0.2492	0.100*
C7	0.1002 (3)	0.4924 (2)	0.12512 (16)	0.0477 (10)
C8	0.0060 (4)	0.4655 (3)	0.1258 (2)	0.0788 (16)
H8A	−0.0306	0.4763	0.1554	0.095*
C9	−0.0385 (5)	0.4225 (5)	0.0844 (3)	0.113 (3)
H9A	−0.1046	0.4060	0.0859	0.136*
C10	0.0131 (6)	0.4048 (4)	0.0424 (3)	0.105 (2)
H10A	−0.0160	0.3736	0.0152	0.126*
C11	0.1077 (7)	0.4316 (4)	0.0389 (2)	0.106 (2)
H11A	0.1429	0.4208	0.0088	0.127*
C12	0.1522 (5)	0.4761 (3)	0.0812 (2)	0.0844 (17)
H12A	0.2174	0.4946	0.0792	0.101*
C13	0.0702 (3)	0.5543 (2)	0.23829 (14)	0.0378 (8)
H13A	0.1063	0.5544	0.2730	0.045*
H13B	0.0300	0.5067	0.2358	0.045*
C14	−0.1491 (3)	0.6061 (2)	0.20657 (14)	0.0384 (8)
C15	−0.2116 (3)	0.6561 (3)	0.17702 (19)	0.0597 (12)
H15A	−0.1909	0.7071	0.1695	0.072*
C16	−0.3055 (4)	0.6301 (3)	0.1586 (2)	0.0799 (17)
H16A	−0.3489	0.6643	0.1397	0.096*
C17	−0.3347 (3)	0.5534 (3)	0.1682 (2)	0.0675 (14)
H17A	−0.3968	0.5355	0.1546	0.081*
C18	−0.2734 (3)	0.5047 (3)	0.19719 (19)	0.0577 (11)
H18A	−0.2935	0.4533	0.2039	0.069*
C19	−0.1803 (3)	0.5312 (2)	0.21701 (17)	0.0479 (10)
H19A	−0.1388	0.4976	0.2376	0.057*
C20	−0.0419 (3)	0.6665 (2)	0.30814 (15)	0.0383 (8)
C21	−0.1360 (3)	0.6711 (3)	0.32606 (18)	0.0564 (12)
H21A	−0.1911	0.6639	0.3022	0.068*
C22	−0.1508 (4)	0.6862 (4)	0.3791 (2)	0.0784 (16)
H22A	−0.2154	0.6891	0.3909	0.094*
C23	−0.0700 (4)	0.6968 (4)	0.4144 (2)	0.0810 (17)
H23A	−0.0796	0.7069	0.4501	0.097*
C24	0.0267 (4)	0.6923 (4)	0.39655 (19)	0.0748 (16)
H24A	0.0822	0.6998	0.4201	0.090*
C25	0.0384 (3)	0.6768 (3)	0.34356 (17)	0.0580 (12)
H25A	0.1028	0.6732	0.3315	0.070*
C26	0.2623 (3)	0.9403 (3)	0.01425 (16)	0.0484 (10)
C27	0.3035 (4)	0.9174 (3)	−0.03199 (19)	0.0682 (13)
H27A	0.3594	0.8846	−0.0300	0.082*
C28	0.2647 (6)	0.9414 (4)	−0.0815 (2)	0.0913 (19)
H28A	0.2957	0.9266	−0.1122	0.110*
C29	0.1814 (6)	0.9865 (4)	−0.0850 (2)	0.096 (2)
H29A	0.1535	1.0009	−0.1184	0.115*
C30	0.1369 (4)	1.0116 (4)	−0.0392 (3)	0.0881 (19)
H30A	0.0808	1.0442	−0.0419	0.106*
C31	0.1770 (4)	0.9876 (3)	0.0106 (2)	0.0669 (13)
H31A	0.1469	1.0031	0.0414	0.080*
C32	0.4268 (3)	0.8588 (3)	0.06829 (16)	0.0464 (10)
C33	0.5216 (3)	0.8901 (3)	0.07825 (19)	0.0596 (12)
H33A	0.5285	0.9400	0.0934	0.072*
C34	0.6064 (3)	0.8484 (3)	0.0661 (2)	0.0695 (14)
H34A	0.6694	0.8702	0.0737	0.083*
C35	0.5986 (4)	0.7757 (3)	0.0429 (2)	0.0675 (14)
C36	0.5044 (4)	0.7428 (3)	0.0333 (2)	0.0720 (15)
H36A	0.4984	0.6928	0.0182	0.086*
C37	0.4195 (4)	0.7835 (3)	0.0458 (2)	0.0640 (13)
H37A	0.3569	0.7605	0.0393	0.077*
C38	0.3562 (3)	1.0063 (2)	0.10750 (16)	0.0452 (10)
C39	0.3977 (3)	1.0620 (3)	0.07448 (18)	0.0556 (11)
H39A	0.3988	1.0519	0.0381	0.067*
C40	0.4374 (4)	1.1319 (3)	0.0945 (2)	0.0633 (13)
H40A	0.4650	1.1679	0.0716	0.076*
C41	0.4363 (3)	1.1487 (3)	0.1486 (2)	0.0590 (12)
C42	0.3933 (3)	1.0958 (3)	0.18175 (19)	0.0580 (12)
H42A	0.3904	1.1071	0.2179	0.070*
C43	0.3542 (3)	1.0254 (3)	0.16138 (17)	0.0530 (11)
H43A	0.3257	0.9900	0.1844	0.064*
C44	0.2585 (3)	0.6956 (2)	0.2394 (2)	0.0509 (10)
C45	0.3716 (4)	0.6611 (3)	0.1550 (2)	0.0701 (14)
C46	0.2049 (3)	0.6743 (3)	0.0874 (2)	0.0514 (11)
C47	0.0074 (3)	0.7000 (3)	0.11873 (16)	0.0449 (9)
C48	−0.0595 (3)	0.8263 (3)	0.17773 (19)	0.0528 (11)
C49	0.1048 (3)	0.8074 (3)	0.24627 (17)	0.0478 (10)
C50	0.2913 (3)	0.8388 (2)	0.19054 (17)	0.0446 (9)
C51	0.1216 (3)	0.9336 (3)	0.14699 (16)	0.0457 (10)
C52	0.1119 (3)	0.8218 (3)	0.06718 (18)	0.0513 (10)
C53	0.7717 (5)	0.7646 (5)	0.0315 (3)	0.130 (3)
H53A	0.8198	0.7272	0.0198	0.195*
H53B	0.7884	0.7788	0.0680	0.195*
H53C	0.7727	0.8110	0.0095	0.195*
C54	0.5152 (6)	1.2734 (4)	0.1412 (3)	0.118 (3)
H54A	0.5435	1.3144	0.1638	0.177*
H54B	0.4639	1.2952	0.1172	0.177*
H54C	0.5667	1.2505	0.1210	0.177*
Cl1	0.4479 (13)	0.4905 (11)	0.0404 (6)	0.172 (6)*	0.15
Cl2	0.3550 (14)	0.5807 (10)	−0.0494 (6)	0.174 (7)*	0.15
C55	0.372 (2)	0.4939 (10)	−0.0163 (10)	0.083 (11)*	0.15
H55A	0.3065	0.4752	−0.0073	0.100*	0.15
H55B	0.3977	0.4562	−0.0411	0.100*	0.15

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ru1	0.03235 (15)	0.03420 (17)	0.05090 (19)	0.00299 (12)	0.00594 (13)	0.00324 (14)
Ru2	0.03279 (15)	0.03140 (16)	0.03801 (16)	0.00195 (12)	0.00618 (12)	0.00411 (12)
Ru3	0.03498 (16)	0.03388 (17)	0.03880 (17)	0.00010 (12)	0.00611 (12)	0.00484 (13)
As1	0.0374 (2)	0.0322 (2)	0.0447 (2)	0.00371 (16)	0.00232 (16)	−0.00020 (16)
As2	0.03317 (19)	0.0323 (2)	0.03523 (19)	0.00000 (15)	0.00221 (15)	0.00322 (15)
P1	0.0379 (5)	0.0412 (6)	0.0426 (5)	0.0010 (4)	0.0092 (4)	0.0065 (4)
O1	0.085 (3)	0.071 (2)	0.058 (2)	−0.0019 (19)	−0.0095 (19)	−0.0014 (18)
O2	0.046 (2)	0.174 (5)	0.172 (5)	0.040 (3)	0.027 (3)	0.053 (4)
O3	0.083 (3)	0.078 (3)	0.056 (2)	0.0012 (19)	0.0068 (18)	−0.0106 (18)
O4	0.063 (2)	0.083 (3)	0.0504 (19)	−0.0055 (18)	−0.0023 (16)	−0.0117 (17)
O5	0.059 (2)	0.069 (2)	0.146 (4)	0.0306 (19)	0.023 (2)	0.026 (2)
O6	0.093 (3)	0.061 (2)	0.063 (2)	−0.0188 (19)	0.0064 (19)	−0.0142 (18)
O7	0.062 (2)	0.054 (2)	0.077 (2)	−0.0101 (16)	−0.0204 (18)	0.0132 (17)
O8	0.068 (2)	0.0470 (19)	0.091 (3)	0.0143 (17)	0.0086 (18)	−0.0091 (18)
O9	0.097 (3)	0.089 (3)	0.059 (2)	−0.021 (2)	−0.020 (2)	0.0143 (19)
O10	0.083 (3)	0.093 (3)	0.130 (4)	0.045 (2)	0.050 (3)	0.020 (3)
O11	0.113 (3)	0.049 (2)	0.106 (3)	−0.028 (2)	0.014 (2)	−0.007 (2)
C1	0.045 (2)	0.040 (2)	0.059 (3)	0.0103 (18)	0.001 (2)	0.005 (2)
C2	0.061 (3)	0.042 (3)	0.110 (4)	0.004 (2)	−0.014 (3)	0.004 (3)
C3	0.081 (4)	0.041 (3)	0.149 (6)	0.009 (3)	−0.014 (4)	0.016 (3)
C4	0.072 (4)	0.068 (4)	0.139 (6)	0.023 (3)	−0.012 (4)	0.027 (4)
C5	0.079 (4)	0.066 (4)	0.150 (6)	0.009 (3)	−0.055 (4)	0.010 (4)
C6	0.081 (4)	0.043 (3)	0.120 (5)	0.006 (3)	−0.038 (3)	0.004 (3)
C7	0.063 (3)	0.034 (2)	0.046 (2)	0.0061 (19)	0.003 (2)	−0.0040 (18)
C8	0.073 (4)	0.091 (4)	0.073 (3)	−0.011 (3)	0.001 (3)	−0.037 (3)
C9	0.094 (5)	0.148 (7)	0.096 (5)	−0.026 (5)	−0.005 (4)	−0.063 (5)
C10	0.142 (7)	0.088 (5)	0.080 (5)	−0.019 (5)	−0.029 (5)	−0.023 (4)
C11	0.190 (8)	0.079 (5)	0.051 (3)	−0.001 (5)	0.020 (4)	−0.020 (3)
C12	0.115 (5)	0.074 (4)	0.066 (3)	−0.017 (3)	0.026 (3)	−0.020 (3)
C13	0.040 (2)	0.037 (2)	0.0354 (19)	0.0030 (16)	−0.0009 (16)	0.0036 (16)
C14	0.0369 (19)	0.043 (2)	0.0350 (19)	−0.0003 (16)	0.0006 (15)	0.0020 (16)
C15	0.041 (2)	0.055 (3)	0.082 (3)	−0.006 (2)	−0.008 (2)	0.022 (2)
C16	0.048 (3)	0.087 (4)	0.103 (4)	−0.003 (3)	−0.018 (3)	0.043 (3)
C17	0.040 (2)	0.079 (4)	0.081 (3)	−0.015 (2)	−0.012 (2)	0.011 (3)
C18	0.052 (3)	0.047 (3)	0.073 (3)	−0.011 (2)	−0.001 (2)	0.003 (2)
C19	0.047 (2)	0.043 (2)	0.053 (2)	−0.0032 (19)	−0.0024 (19)	0.0054 (19)
C20	0.044 (2)	0.032 (2)	0.040 (2)	−0.0016 (16)	0.0083 (17)	0.0009 (16)
C21	0.050 (3)	0.069 (3)	0.051 (3)	0.005 (2)	0.008 (2)	−0.002 (2)
C22	0.060 (3)	0.120 (5)	0.056 (3)	0.013 (3)	0.018 (3)	−0.011 (3)
C23	0.076 (4)	0.122 (5)	0.048 (3)	0.000 (3)	0.016 (3)	−0.014 (3)
C24	0.066 (3)	0.114 (5)	0.044 (3)	−0.007 (3)	−0.001 (2)	−0.012 (3)
C25	0.049 (3)	0.081 (3)	0.045 (2)	−0.002 (2)	0.009 (2)	−0.005 (2)
C26	0.045 (2)	0.051 (3)	0.049 (2)	−0.0077 (19)	0.0032 (19)	0.017 (2)
C27	0.079 (3)	0.074 (4)	0.052 (3)	0.004 (3)	0.008 (2)	0.005 (3)
C28	0.122 (5)	0.099 (5)	0.052 (3)	−0.002 (4)	−0.004 (3)	0.012 (3)
C29	0.126 (6)	0.096 (5)	0.062 (4)	−0.029 (4)	−0.026 (4)	0.027 (3)
C30	0.076 (4)	0.078 (4)	0.107 (5)	−0.002 (3)	−0.029 (4)	0.041 (4)
C31	0.063 (3)	0.064 (3)	0.073 (3)	0.005 (3)	0.000 (2)	0.023 (3)
C32	0.044 (2)	0.049 (3)	0.047 (2)	0.0102 (18)	0.0140 (18)	0.0071 (19)
C33	0.047 (2)	0.064 (3)	0.068 (3)	0.002 (2)	0.006 (2)	−0.006 (2)
C34	0.040 (2)	0.090 (4)	0.080 (4)	0.014 (3)	0.013 (2)	0.005 (3)
C35	0.068 (3)	0.066 (3)	0.071 (3)	0.021 (3)	0.032 (3)	0.020 (3)
C36	0.084 (4)	0.046 (3)	0.089 (4)	0.006 (3)	0.037 (3)	0.001 (3)
C37	0.059 (3)	0.056 (3)	0.079 (3)	−0.002 (2)	0.026 (3)	0.003 (3)
C38	0.041 (2)	0.043 (2)	0.053 (2)	0.0029 (18)	0.0133 (18)	0.0118 (19)
C39	0.060 (3)	0.054 (3)	0.054 (3)	−0.005 (2)	0.011 (2)	0.007 (2)
C40	0.068 (3)	0.049 (3)	0.075 (3)	−0.013 (2)	0.017 (3)	0.010 (2)
C41	0.058 (3)	0.045 (3)	0.075 (3)	−0.005 (2)	0.011 (2)	0.002 (2)
C42	0.066 (3)	0.052 (3)	0.057 (3)	−0.008 (2)	0.010 (2)	−0.002 (2)
C43	0.060 (3)	0.044 (3)	0.056 (3)	0.000 (2)	0.009 (2)	0.008 (2)
C44	0.049 (2)	0.038 (2)	0.065 (3)	−0.0013 (18)	−0.001 (2)	0.004 (2)
C45	0.048 (3)	0.080 (4)	0.083 (4)	0.018 (3)	0.009 (3)	0.019 (3)
C46	0.045 (2)	0.046 (3)	0.063 (3)	0.0041 (19)	0.008 (2)	0.003 (2)
C47	0.039 (2)	0.053 (3)	0.043 (2)	0.0051 (18)	0.0063 (18)	0.004 (2)
C48	0.047 (2)	0.045 (3)	0.067 (3)	0.005 (2)	0.014 (2)	0.009 (2)
C49	0.051 (2)	0.041 (2)	0.053 (3)	−0.0042 (19)	0.011 (2)	0.003 (2)
C50	0.043 (2)	0.038 (2)	0.053 (2)	−0.0007 (18)	0.0009 (19)	0.0079 (18)
C51	0.042 (2)	0.048 (3)	0.047 (2)	−0.0048 (19)	0.0031 (18)	0.0046 (19)
C52	0.058 (3)	0.049 (3)	0.047 (2)	−0.006 (2)	0.003 (2)	0.009 (2)
C53	0.075 (4)	0.167 (8)	0.154 (7)	0.058 (5)	0.042 (4)	0.031 (6)
C54	0.166 (7)	0.069 (4)	0.122 (6)	−0.048 (5)	0.029 (5)	−0.006 (4)

Geometric parameters (Å, º) top

Ru1—C45	1.884 (5)	C14—C15	1.376 (5)
Ru1—C44	1.929 (5)	C15—C16	1.385 (6)
Ru1—C46	1.931 (5)	C15—H15A	0.9300
Ru1—As1	2.4463 (5)	C16—C17	1.382 (7)
Ru1—Ru2	2.8469 (4)	C16—H16A	0.9300
Ru1—Ru3	2.8883 (4)	C17—C18	1.347 (6)
Ru2—C48	1.887 (4)	C17—H17A	0.9300
Ru2—C47	1.921 (4)	C18—C19	1.389 (6)
Ru2—C49	1.928 (5)	C18—H18A	0.9300
Ru2—As2	2.4335 (5)	C19—H19A	0.9300
Ru2—Ru3	2.8376 (4)	C20—C21	1.363 (5)
Ru3—C51	1.881 (5)	C20—C25	1.365 (6)
Ru3—C50	1.918 (4)	C21—C22	1.382 (6)
Ru3—C52	1.929 (5)	C21—H21A	0.9300
Ru3—P1	2.3511 (10)	C22—C23	1.368 (7)
As1—C7	1.940 (4)	C22—H22A	0.9300
As1—C13	1.952 (3)	C23—C24	1.395 (7)
As1—C1	1.953 (4)	C23—H23A	0.9300
As2—C20	1.948 (4)	C24—C25	1.374 (6)
As2—C14	1.949 (4)	C24—H24A	0.9300
As2—C13	1.974 (4)	C25—H25A	0.9300
P1—C32	1.824 (4)	C26—C27	1.369 (6)
P1—C38	1.830 (4)	C26—C31	1.392 (6)
P1—C26	1.836 (4)	C27—C28	1.380 (7)
O1—C44	1.140 (5)	C27—H27A	0.9300
O2—C45	1.130 (5)	C28—C29	1.350 (9)
O3—C46	1.140 (5)	C28—H28A	0.9300
O4—C47	1.138 (5)	C29—C30	1.390 (8)
O5—C48	1.145 (5)	C29—H29A	0.9300
O6—C49	1.143 (5)	C30—C31	1.393 (7)
O7—C50	1.155 (5)	C30—H30A	0.9300
O8—C51	1.138 (5)	C31—H31A	0.9300
O9—C52	1.140 (5)	C32—C33	1.383 (6)
O10—C35	1.361 (6)	C32—C37	1.396 (6)
O10—C53	1.394 (8)	C33—C34	1.386 (6)
O11—C41	1.364 (5)	C33—H33A	0.9300
O11—C54	1.388 (7)	C34—C35	1.363 (7)
C1—C6	1.359 (6)	C34—H34A	0.9300
C1—C2	1.373 (6)	C35—C36	1.386 (8)
C2—C3	1.410 (7)	C36—C37	1.380 (7)
C2—H2A	0.9300	C36—H36A	0.9300
C3—C4	1.366 (8)	C37—H37A	0.9300
C3—H3A	0.9300	C38—C43	1.392 (6)
C4—C5	1.346 (8)	C38—C39	1.393 (5)
C4—H4A	0.9300	C39—C40	1.381 (6)
C5—C6	1.392 (7)	C39—H39A	0.9300
C5—H5A	0.9300	C40—C41	1.388 (7)
C6—H6A	0.9300	C40—H40A	0.9300
C7—C8	1.340 (6)	C41—C42	1.370 (6)
C7—C12	1.365 (6)	C42—C43	1.388 (6)
C8—C9	1.375 (7)	C42—H42A	0.9300
C8—H8A	0.9300	C43—H43A	0.9300
C9—C10	1.329 (9)	C53—H53A	0.9600
C9—H9A	0.9300	C53—H53B	0.9600
C10—C11	1.351 (10)	C53—H53C	0.9600
C10—H10A	0.9300	C54—H54A	0.9600
C11—C12	1.406 (8)	C54—H54B	0.9600
C11—H11A	0.9300	C54—H54C	0.9600
C12—H12A	0.9300	Cl1—C55	1.6995 (10)
C13—H13A	0.9700	Cl2—C55	1.6995 (10)
C13—H13B	0.9700	C55—H55A	0.9700
C14—C19	1.367 (5)	C55—H55B	0.9700

C45—Ru1—C44	91.7 (2)	C16—C15—H15A	120.1
C45—Ru1—C46	91.4 (2)	C17—C16—C15	120.0 (5)
C44—Ru1—C46	175.99 (18)	C17—C16—H16A	120.0
C45—Ru1—As1	103.17 (16)	C15—C16—H16A	120.0
C44—Ru1—As1	87.29 (13)	C18—C17—C16	120.1 (4)
C46—Ru1—As1	94.46 (13)	C18—C17—H17A	120.0
C45—Ru1—Ru2	164.40 (17)	C16—C17—H17A	120.0
C44—Ru1—Ru2	82.56 (13)	C17—C18—C19	120.1 (4)
C46—Ru1—Ru2	93.79 (12)	C17—C18—H18A	120.0
As1—Ru1—Ru2	91.080 (14)	C19—C18—H18A	120.0
C45—Ru1—Ru3	108.02 (16)	C14—C19—C18	120.6 (4)
C44—Ru1—Ru3	100.56 (13)	C14—C19—H19A	119.7
C46—Ru1—Ru3	76.06 (13)	C18—C19—H19A	119.7
As1—Ru1—Ru3	147.496 (16)	C21—C20—C25	119.0 (4)
Ru2—Ru1—Ru3	59.304 (10)	C21—C20—As2	121.6 (3)
C48—Ru2—C47	93.72 (19)	C25—C20—As2	119.4 (3)
C48—Ru2—C49	91.44 (19)	C20—C21—C22	121.0 (4)
C47—Ru2—C49	174.09 (17)	C20—C21—H21A	119.5
C48—Ru2—As2	102.00 (13)	C22—C21—H21A	119.5
C47—Ru2—As2	88.23 (12)	C23—C22—C21	119.7 (5)
C49—Ru2—As2	93.51 (12)	C23—C22—H22A	120.2
C48—Ru2—Ru3	100.32 (13)	C21—C22—H22A	120.2
C47—Ru2—Ru3	92.30 (12)	C22—C23—C24	119.9 (5)
C49—Ru2—Ru3	83.93 (12)	C22—C23—H23A	120.0
As2—Ru2—Ru3	157.589 (16)	C24—C23—H23A	120.0
C48—Ru2—Ru1	160.42 (13)	C25—C24—C23	118.7 (5)
C47—Ru2—Ru1	81.75 (11)	C25—C24—H24A	120.7
C49—Ru2—Ru1	92.43 (12)	C23—C24—H24A	120.7
As2—Ru2—Ru1	96.913 (14)	C20—C25—C24	121.7 (4)
Ru3—Ru2—Ru1	61.075 (11)	C20—C25—H25A	119.1
C51—Ru3—C50	101.40 (17)	C24—C25—H25A	119.1
C51—Ru3—C52	92.56 (18)	C27—C26—C31	118.4 (4)
C50—Ru3—C52	165.87 (18)	C27—C26—P1	123.9 (4)
C51—Ru3—P1	94.76 (12)	C31—C26—P1	117.7 (3)
C50—Ru3—P1	89.91 (12)	C26—C27—C28	122.0 (5)
C52—Ru3—P1	91.12 (13)	C26—C27—H27A	119.0
C51—Ru3—Ru2	86.89 (12)	C28—C27—H27A	119.0
C50—Ru3—Ru2	93.93 (12)	C29—C28—C27	119.5 (6)
C52—Ru3—Ru2	84.57 (12)	C29—C28—H28A	120.3
P1—Ru3—Ru2	175.45 (3)	C27—C28—H28A	120.3
C51—Ru3—Ru1	143.17 (12)	C28—C29—C30	120.7 (6)
C50—Ru3—Ru1	68.93 (12)	C28—C29—H29A	119.7
C52—Ru3—Ru1	98.49 (13)	C30—C29—H29A	119.7
P1—Ru3—Ru1	119.86 (3)	C29—C30—C31	119.4 (6)
Ru2—Ru3—Ru1	59.621 (10)	C29—C30—H30A	120.3
C7—As1—C13	104.42 (17)	C31—C30—H30A	120.3
C7—As1—C1	101.18 (18)	C26—C31—C30	120.0 (5)
C13—As1—C1	98.61 (16)	C26—C31—H31A	120.0
C7—As1—Ru1	118.67 (12)	C30—C31—H31A	120.0
C13—As1—Ru1	113.06 (11)	C33—C32—C37	117.7 (4)
C1—As1—Ru1	118.13 (13)	C33—C32—P1	123.9 (4)
C20—As2—C14	102.10 (15)	C37—C32—P1	118.4 (3)
C20—As2—C13	101.59 (15)	C32—C33—C34	121.2 (5)
C14—As2—C13	105.44 (16)	C32—C33—H33A	119.4
C20—As2—Ru2	116.95 (11)	C34—C33—H33A	119.4
C14—As2—Ru2	116.29 (11)	C35—C34—C33	120.7 (5)
C13—As2—Ru2	112.70 (11)	C35—C34—H34A	119.6
C32—P1—C38	103.28 (19)	C33—C34—H34A	119.6
C32—P1—C26	103.33 (19)	O10—C35—C34	125.6 (5)
C38—P1—C26	100.68 (19)	O10—C35—C36	115.4 (5)
C32—P1—Ru3	116.51 (14)	C34—C35—C36	119.0 (4)
C38—P1—Ru3	117.01 (13)	C37—C36—C35	120.7 (5)
C26—P1—Ru3	113.89 (13)	C37—C36—H36A	119.7
C35—O10—C53	117.6 (5)	C35—C36—H36A	119.7
C41—O11—C54	119.2 (5)	C36—C37—C32	120.7 (5)
C6—C1—C2	118.8 (4)	C36—C37—H37A	119.7
C6—C1—As1	120.1 (3)	C32—C37—H37A	119.7
C2—C1—As1	121.1 (3)	C43—C38—C39	116.8 (4)
C1—C2—C3	120.1 (5)	C43—C38—P1	122.1 (3)
C1—C2—H2A	119.9	C39—C38—P1	121.1 (3)
C3—C2—H2A	119.9	C40—C39—C38	121.5 (4)
C4—C3—C2	119.7 (5)	C40—C39—H39A	119.2
C4—C3—H3A	120.2	C38—C39—H39A	119.2
C2—C3—H3A	120.2	C39—C40—C41	120.5 (4)
C5—C4—C3	119.9 (5)	C39—C40—H40A	119.8
C5—C4—H4A	120.1	C41—C40—H40A	119.8
C3—C4—H4A	120.1	O11—C41—C42	115.8 (5)
C4—C5—C6	120.6 (6)	O11—C41—C40	125.0 (4)
C4—C5—H5A	119.7	C42—C41—C40	119.2 (4)
C6—C5—H5A	119.7	C41—C42—C43	120.1 (4)
C1—C6—C5	120.9 (5)	C41—C42—H42A	120.0
C1—C6—H6A	119.6	C43—C42—H42A	120.0
C5—C6—H6A	119.6	C42—C43—C38	122.0 (4)
C8—C7—C12	117.7 (5)	C42—C43—H43A	119.0
C8—C7—As1	124.0 (3)	C38—C43—H43A	119.0
C12—C7—As1	118.3 (4)	O1—C44—Ru1	173.5 (4)
C7—C8—C9	122.5 (5)	O2—C45—Ru1	178.9 (5)
C7—C8—H8A	118.8	O3—C46—Ru1	171.8 (4)
C9—C8—H8A	118.8	O4—C47—Ru2	173.7 (4)
C10—C9—C8	119.8 (7)	O5—C48—Ru2	178.8 (4)
C10—C9—H9A	120.1	O6—C49—Ru2	174.8 (4)
C8—C9—H9A	120.1	O7—C50—Ru3	169.5 (3)
C9—C10—C11	120.4 (6)	O8—C51—Ru3	177.2 (4)
C9—C10—H10A	119.8	O9—C52—Ru3	175.4 (4)
C11—C10—H10A	119.8	O10—C53—H53A	109.5
C10—C11—C12	119.3 (6)	O10—C53—H53B	109.5
C10—C11—H11A	120.4	H53A—C53—H53B	109.5
C12—C11—H11A	120.4	O10—C53—H53C	109.5
C7—C12—C11	120.3 (6)	H53A—C53—H53C	109.5
C7—C12—H12A	119.9	H53B—C53—H53C	109.5
C11—C12—H12A	119.9	O11—C54—H54A	109.5
As1—C13—As2	113.38 (17)	O11—C54—H54B	109.5
As1—C13—H13A	108.9	H54A—C54—H54B	109.5
As2—C13—H13A	108.9	O11—C54—H54C	109.5
As1—C13—H13B	108.9	H54A—C54—H54C	109.5
As2—C13—H13B	108.9	H54B—C54—H54C	109.5
H13A—C13—H13B	107.7	Cl1—C55—Cl2	119.77 (11)
C19—C14—C15	119.5 (4)	Cl1—C55—H55A	107.4
C19—C14—As2	122.5 (3)	Cl2—C55—H55A	107.4
C15—C14—As2	117.9 (3)	Cl1—C55—H55B	107.4
C14—C15—C16	119.7 (4)	Cl2—C55—H55B	107.4
C14—C15—H15A	120.1	H55A—C55—H55B	106.9

C45—Ru1—Ru2—C48	57.4 (7)	C13—As1—C1—C2	82.7 (4)
C44—Ru1—Ru2—C48	126.5 (5)	Ru1—As1—C1—C2	−155.3 (4)
C46—Ru1—Ru2—C48	−51.8 (5)	C6—C1—C2—C3	−1.3 (8)
As1—Ru1—Ru2—C48	−146.4 (4)	As1—C1—C2—C3	−179.1 (4)
Ru3—Ru1—Ru2—C48	19.5 (4)	C1—C2—C3—C4	0.3 (10)
C45—Ru1—Ru2—C47	135.2 (6)	C2—C3—C4—C5	1.4 (11)
C44—Ru1—Ru2—C47	−155.73 (18)	C3—C4—C5—C6	−2.0 (11)
C46—Ru1—Ru2—C47	25.94 (18)	C2—C1—C6—C5	0.7 (9)
As1—Ru1—Ru2—C47	−68.60 (12)	As1—C1—C6—C5	178.5 (5)
Ru3—Ru1—Ru2—C47	97.27 (12)	C4—C5—C6—C1	1.0 (11)
C45—Ru1—Ru2—C49	−43.8 (6)	C13—As1—C7—C8	3.4 (5)
C44—Ru1—Ru2—C49	25.30 (17)	C1—As1—C7—C8	105.5 (4)
C46—Ru1—Ru2—C49	−153.03 (18)	Ru1—As1—C7—C8	−123.5 (4)
As1—Ru1—Ru2—C49	112.42 (12)	C13—As1—C7—C12	−176.0 (4)
Ru3—Ru1—Ru2—C49	−81.71 (12)	C1—As1—C7—C12	−73.9 (4)
C45—Ru1—Ru2—As2	−137.6 (6)	Ru1—As1—C7—C12	57.0 (4)
C44—Ru1—Ru2—As2	−68.54 (13)	C12—C7—C8—C9	0.3 (9)
C46—Ru1—Ru2—As2	113.14 (13)	As1—C7—C8—C9	−179.1 (5)
As1—Ru1—Ru2—As2	18.590 (17)	C7—C8—C9—C10	1.7 (11)
Ru3—Ru1—Ru2—As2	−175.538 (16)	C8—C9—C10—C11	−3.0 (12)
C45—Ru1—Ru2—Ru3	38.0 (6)	C9—C10—C11—C12	2.4 (12)
C44—Ru1—Ru2—Ru3	107.00 (13)	C8—C7—C12—C11	−1.0 (8)
C46—Ru1—Ru2—Ru3	−71.33 (13)	As1—C7—C12—C11	178.5 (5)
As1—Ru1—Ru2—Ru3	−165.872 (17)	C10—C11—C12—C7	−0.4 (10)
C48—Ru2—Ru3—C51	22.56 (19)	C7—As1—C13—As2	−90.9 (2)
C47—Ru2—Ru3—C51	116.77 (17)	C1—As1—C13—As2	165.1 (2)
C49—Ru2—Ru3—C51	−67.80 (18)	Ru1—As1—C13—As2	39.4 (2)
As2—Ru2—Ru3—C51	−152.28 (13)	C20—As2—C13—As1	−147.17 (19)
Ru1—Ru2—Ru3—C51	−163.97 (12)	C14—As2—C13—As1	106.6 (2)
C48—Ru2—Ru3—C50	123.78 (19)	Ru2—As2—C13—As1	−21.2 (2)
C47—Ru2—Ru3—C50	−142.01 (17)	C20—As2—C14—C19	−75.6 (3)
C49—Ru2—Ru3—C50	33.42 (18)	C13—As2—C14—C19	30.2 (4)
As2—Ru2—Ru3—C50	−51.06 (13)	Ru2—As2—C14—C19	155.8 (3)
Ru1—Ru2—Ru3—C50	−62.74 (12)	C20—As2—C14—C15	103.0 (3)
C48—Ru2—Ru3—C52	−70.3 (2)	C13—As2—C14—C15	−151.2 (3)
C47—Ru2—Ru3—C52	23.89 (18)	Ru2—As2—C14—C15	−25.5 (4)
C49—Ru2—Ru3—C52	−160.67 (19)	C19—C14—C15—C16	0.5 (7)
As2—Ru2—Ru3—C52	114.85 (14)	As2—C14—C15—C16	−178.2 (4)
Ru1—Ru2—Ru3—C52	103.16 (14)	C14—C15—C16—C17	−2.3 (8)
C48—Ru2—Ru3—Ru1	−173.47 (15)	C15—C16—C17—C18	2.4 (9)
C47—Ru2—Ru3—Ru1	−79.27 (12)	C16—C17—C18—C19	−0.7 (8)
C49—Ru2—Ru3—Ru1	96.17 (13)	C15—C14—C19—C18	1.3 (6)
As2—Ru2—Ru3—Ru1	11.69 (4)	As2—C14—C19—C18	179.9 (3)
C45—Ru1—Ru3—C51	−142.6 (3)	C17—C18—C19—C14	−1.2 (7)
C44—Ru1—Ru3—C51	−47.3 (2)	C14—As2—C20—C21	−17.1 (4)
C46—Ru1—Ru3—C51	130.5 (2)	C13—As2—C20—C21	−125.9 (4)
As1—Ru1—Ru3—C51	54.4 (2)	Ru2—As2—C20—C21	111.0 (3)
Ru2—Ru1—Ru3—C51	27.4 (2)	C14—As2—C20—C25	163.7 (3)
C45—Ru1—Ru3—C50	−61.9 (2)	C13—As2—C20—C25	54.9 (4)
C44—Ru1—Ru3—C50	33.41 (18)	Ru2—As2—C20—C25	−68.2 (4)
C46—Ru1—Ru3—C50	−148.79 (19)	C25—C20—C21—C22	0.2 (7)
As1—Ru1—Ru3—C50	135.12 (13)	As2—C20—C21—C22	−179.0 (4)
Ru2—Ru1—Ru3—C50	108.11 (13)	C20—C21—C22—C23	0.0 (9)
C45—Ru1—Ru3—C52	111.5 (2)	C21—C22—C23—C24	0.0 (10)
C44—Ru1—Ru3—C52	−153.26 (19)	C22—C23—C24—C25	−0.4 (9)
C46—Ru1—Ru3—C52	24.54 (19)	C21—C20—C25—C24	−0.6 (7)
As1—Ru1—Ru3—C52	−51.54 (14)	As2—C20—C25—C24	178.7 (4)
Ru2—Ru1—Ru3—C52	−78.55 (13)	C23—C24—C25—C20	0.7 (8)
C45—Ru1—Ru3—P1	15.24 (18)	C32—P1—C26—C27	6.0 (4)
C44—Ru1—Ru3—P1	110.52 (13)	C38—P1—C26—C27	112.6 (4)
C46—Ru1—Ru3—P1	−71.68 (13)	Ru3—P1—C26—C27	−121.3 (4)
As1—Ru1—Ru3—P1	−147.77 (4)	C32—P1—C26—C31	−175.1 (4)
Ru2—Ru1—Ru3—P1	−174.78 (3)	C38—P1—C26—C31	−68.5 (4)
C45—Ru1—Ru3—Ru2	−169.99 (18)	Ru3—P1—C26—C31	57.6 (4)
C44—Ru1—Ru3—Ru2	−74.71 (13)	C31—C26—C27—C28	1.8 (8)
C46—Ru1—Ru3—Ru2	103.10 (13)	P1—C26—C27—C28	−179.3 (4)
As1—Ru1—Ru3—Ru2	27.01 (3)	C26—C27—C28—C29	−2.5 (9)
C45—Ru1—As1—C7	−97.8 (2)	C27—C28—C29—C30	2.7 (10)
C44—Ru1—As1—C7	171.09 (19)	C28—C29—C30—C31	−2.2 (10)
C46—Ru1—As1—C7	−5.30 (19)	C27—C26—C31—C30	−1.3 (7)
Ru2—Ru1—As1—C7	88.58 (14)	P1—C26—C31—C30	179.8 (4)
Ru3—Ru1—As1—C7	65.59 (15)	C29—C30—C31—C26	1.5 (8)
C45—Ru1—As1—C13	139.4 (2)	C38—P1—C32—C33	0.5 (4)
C44—Ru1—As1—C13	48.32 (17)	C26—P1—C32—C33	105.0 (4)
C46—Ru1—As1—C13	−128.08 (17)	Ru3—P1—C32—C33	−129.3 (3)
Ru2—Ru1—As1—C13	−34.19 (12)	C38—P1—C32—C37	−177.9 (3)
Ru3—Ru1—As1—C13	−57.18 (12)	C26—P1—C32—C37	−73.3 (4)
C45—Ru1—As1—C1	25.1 (2)	Ru3—P1—C32—C37	52.4 (4)
C44—Ru1—As1—C1	−66.02 (19)	C37—C32—C33—C34	0.4 (7)
C46—Ru1—As1—C1	117.59 (19)	P1—C32—C33—C34	−177.9 (4)
Ru2—Ru1—As1—C1	−148.53 (14)	C32—C33—C34—C35	1.2 (8)
Ru3—Ru1—As1—C1	−171.52 (14)	C53—O10—C35—C34	−5.4 (8)
C48—Ru2—As2—C20	−70.3 (2)	C53—O10—C35—C36	174.0 (5)
C47—Ru2—As2—C20	−163.71 (17)	C33—C34—C35—O10	177.3 (5)
C49—Ru2—As2—C20	21.94 (18)	C33—C34—C35—C36	−2.1 (8)
Ru3—Ru2—As2—C20	104.53 (13)	O10—C35—C36—C37	−178.1 (5)
Ru1—Ru2—As2—C20	114.82 (13)	C34—C35—C36—C37	1.3 (8)
C48—Ru2—As2—C14	50.62 (19)	C35—C36—C37—C32	0.3 (8)
C47—Ru2—As2—C14	−42.82 (17)	C33—C32—C37—C36	−1.2 (7)
C49—Ru2—As2—C14	142.84 (18)	P1—C32—C37—C36	177.3 (4)
Ru3—Ru2—As2—C14	−134.58 (13)	C32—P1—C38—C43	−106.0 (4)
Ru1—Ru2—As2—C14	−124.29 (12)	C26—P1—C38—C43	147.4 (4)
C48—Ru2—As2—C13	172.52 (19)	Ru3—P1—C38—C43	23.4 (4)
C47—Ru2—As2—C13	79.09 (16)	C32—P1—C38—C39	71.5 (4)
C49—Ru2—As2—C13	−95.26 (17)	C26—P1—C38—C39	−35.1 (4)
Ru3—Ru2—As2—C13	−12.67 (13)	Ru3—P1—C38—C39	−159.1 (3)
Ru1—Ru2—As2—C13	−2.38 (12)	C43—C38—C39—C40	1.7 (7)
C51—Ru3—P1—C32	163.9 (2)	P1—C38—C39—C40	−175.9 (4)
C50—Ru3—P1—C32	62.4 (2)	C38—C39—C40—C41	−0.4 (7)
C52—Ru3—P1—C32	−103.5 (2)	C54—O11—C41—C42	−177.5 (6)
Ru1—Ru3—P1—C32	−3.02 (17)	C54—O11—C41—C40	1.5 (8)
C51—Ru3—P1—C38	41.01 (19)	C39—C40—C41—O11	179.5 (5)
C50—Ru3—P1—C38	−60.42 (19)	C39—C40—C41—C42	−1.4 (7)
C52—Ru3—P1—C38	133.7 (2)	O11—C41—C42—C43	−179.1 (4)
Ru1—Ru3—P1—C38	−125.87 (15)	C40—C41—C42—C43	1.8 (7)
C51—Ru3—P1—C26	−75.9 (2)	C41—C42—C43—C38	−0.4 (7)
C50—Ru3—P1—C26	−177.4 (2)	C39—C38—C43—C42	−1.3 (6)
C52—Ru3—P1—C26	16.7 (2)	P1—C38—C43—C42	176.3 (3)
Ru1—Ru3—P1—C26	117.18 (16)	C51—Ru3—C50—O7	−57 (2)
C7—As1—C1—C6	158.3 (4)	C52—Ru3—C50—O7	132.2 (19)
C13—As1—C1—C6	−95.0 (4)	P1—Ru3—C50—O7	38 (2)
Ru1—As1—C1—C6	27.0 (5)	Ru2—Ru3—C50—O7	−144 (2)
C7—As1—C1—C2	−23.9 (4)	Ru1—Ru3—C50—O7	160 (2)

Experimental details

Crystal data
Chemical formula	[Ru₃(C₂₅H₂₂As₂)(C₂₀H₁₉O₂P)(CO)₉]·0.15CH₂Cl₂
M_r	1362.63
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	296
a, b, c (Å)	13.3723 (4), 16.9461 (6), 25.0956 (8)
β (°)	93.293 (2)
V (Å³)	5677.5 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.04
Crystal size (mm)	0.31 × 0.21 × 0.16

Data collection
Diffractometer	Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2005)
T_min, T_max	0.571, 0.741
No. of measured, independent and observed [I > 2σ(I)] reflections	67215, 16557, 10503
R_int	0.041
(sin θ/λ)_max (Å⁻¹)	0.703

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.039, 0.121, 1.02
No. of reflections	16557
No. of parameters	654
No. of restraints	3
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.00, −0.38

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Footnotes

‡On secondment to: Multimedia University, Melaka Campus, Jalan Ayer Keroh Lama, 74750 Melaka, Malaysia.

§Thomson Reuters ResearcherID: A-5523-2009.

¶Thomson Reuters ResearcherID: A-3561-2009. Additional correspondence author, e-mail: hkfun@usm.my.

Acknowledgements

The authors would like to thank the Malaysian Government and Universiti Sains Malaysia (USM) for the Research grant 1001/PJJAUH/811115. IAK is grateful to USM for a Postdoctoral Fellowship and to Gokhale Centenary College, Ankola, Karnataka, India, for postdoctoral study leave. HKF thanks USM for the Research University Golden Goose grant 1001/PFIZIK/811012. CSY thanks USM for the award of a USM Fellowship.

References

Bruce, M. I., Liddell, M. J., Hughes, C. A., Patrick, J. M., Skelton, B. W. & White, A. H. (1988a). J. Organomet. Chem. 347, 181–205. CSD CrossRef CAS Web of Science Google Scholar
Bruce, M. I., Liddell, M. J., Shawkataly, O. bin, Hughes, C. A., Skelton, B. W. & White, A. H. (1988b). J. Organomet. Chem. 347, 207–235. CSD CrossRef CAS Web of Science Google Scholar
Bruce, M. I., Matisons, J. G. & Nicholson, B. K. (1983). J. Organomet. Chem. 247, 321–343. CrossRef CAS Web of Science Google Scholar
Bruce, M. I., Shawkataly, O. bin & Williams, M. L. (1985). J. Organomet. Chem. 287, 127–131. Google Scholar
Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Shawkataly, O. bin, Khan, I. A., Yeap, C. S. & Fun, H.-K. (2009). Acta Cryst. E65, m1620–m1621. Web of Science CSD CrossRef IUCr Journals Google Scholar
Shawkataly, O. bin, Ramalingam, K., Fun, H.-K., Abdul Rahman, A., & Razak, I. A. (2004). J. Cluster Sci. 15, 387–394. Web of Science CSD CrossRef Google Scholar
Shawkataly, O. bin, Ramalingam, K., Lee, S. T., Parameswary, M., Fun, H.-K. & Sivakumar, K. (1998). Polyhedron, 17, 1211–1216. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spek, A. L. (2009). Acta Cryst. D65, 148–155. Web of Science CrossRef CAS IUCr Journals Google Scholar

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