[μ-Bis(diphenyl­arsanyl)methane-1:2κ2As:As']nona­carbonyl-1κ3C,2κ3C,3κ3C-[(4-methyl­sulfanylphen­yl)diphenyl­phosphane-3κP]-triangulo-triruthenium(0)

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

doi:10.1107/S1600536810054206

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 2| February 2011| Pages m179-m180

doi:10.1107/S1600536810054206

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[μ-Bis(diphenylarsanyl)methane-1:2κ²As:As']nonacarbonyl-1κ³C,2κ³C,3κ³C-[(4-methylsulfanylphenyl)diphenylphosphane-3κP]-triangulo-triruthenium(0)

Omar bin Shawkataly,^a ^*‡ Imthyaz Ahmed Khan,^a § H. A. Hafiz Malik,^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 21 December 2010; accepted 25 December 2010; online 15 January 2011)

In the title triangulo-triruthenium compound, [Ru₃(C₂₅H₂₂As₂)(C₁₉H₁₇PS)(CO)₉], the bis(diphenylarsanyl)methane ligand bridges an Ru—Ru bond and the monodentate phosphane ligand bonds to the third Ru atom. Both arsine and phosphane 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 phosphane-substituted benzene rings make dihedral angles of 57.91 (19), 84.31 (15) and 59.37 (18)° with each other. The dihedral angles between the two benzene rings are 60.9 (2) and 85.40 (18)° for the two diphenylarsanyl groups. In the crystal, molecules are linked into a three-dimensional framework by intermolecular C—H⋯O hydrogen bonds. Weak intermolecular C—H⋯π interactions stabilize the crystal structure.

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 , 2010a ,b ). For the synthesis of Ru₃(CO)₁₀(μ-Ph₂AsCH₂AsPh₂), see: Bruce et al. (1983 ) and for that of 4-methylthiophenyldiphenylphosphane, see: Fuhr et al. (2002 ). For the stability of the temperature controller used in the data collection, see: Cosier & Glazer (1986 ).

Experimental

Crystal data

[Ru₃(C₂₅H₂₂As₂)(C₁₉H₁₇PS)(CO)₉]
M_r = 1335.92
Monoclinic, P 2₁ /c
a = 16.1070 (11) Å
b = 16.7244 (12) Å
c = 24.3147 (13) Å
β = 129.712 (3)°
V = 5038.6 (6) Å³
Z = 4
Mo Kα radiation
μ = 2.32 mm⁻¹
T = 100 K
0.19 × 0.07 × 0.03 mm

Data collection

Bruker APEXII DUO CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2009 ) T_min = 0.660, T_max = 0.927
41559 measured reflections
14623 independent reflections
11553 reflections with I > 2σ(I)
R_int = 0.036

Refinement

R[F² > 2σ(F²)] = 0.032
wR(F²) = 0.081
S = 1.02
14623 reflections
623 parameters
H-atom parameters constrained
Δρ_max = 1.24 e Å⁻³
Δρ_min = −0.97 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

Cg1, Cg2 and Cg3 are the centroids of the C7–C12, C38–C43 and C14–C19 benzene rings, respectively.

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C4—H4A⋯O6ⁱ	0.93	2.48	3.278 (6)	144
C24—H24A⋯O7ⁱⁱ	0.93	2.56	3.259 (5)	132
C42—H42A⋯O1ⁱⁱⁱ	0.93	2.57	3.414 (5)	151
C30—H30A⋯Cg1ⁱⁱⁱ	0.93	3.00	3.890 (6)	161
C34—H34A⋯Cg2^iv	0.93	2.89	3.785 (4)	163
C40—H40A⋯Cg3^v	0.93	2.88	3.672 (4)	144
Symmetry codes: (i) -x, -y+2, -z+1; (ii) $[x+1, -y+{\script{3\over 2}}, z+{\script{1\over 2}}]$ ; (iii) $[-x, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iv) $[-x, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (v) $[-x+1, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ .

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); 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: 10.1107/S1600536810054206/sj5088sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810054206/sj5088Isup2.hkl

checkCIF report

Comment top

A large number of substituted derivatives of the type Ru₃(CO)_12-nL_n (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, 2010a,b). Herein we report the synthesis and structure of the title compound.

The bis(diphenylarsanyl)methane ligand bridges the Ru1—Ru2 bond and the monodentate phosphane ligand bonds to the Ru3 atom. Both arsine and phosphane ligands are equatorial with respect to the Ru₃ triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands (Fig 1). The three phosphane-substituted benzene rings make dihedral angles (C26–C31/C32–C37, C26–C31/C38–C43 and C32–C37/C38–C43) of 57.91 (19), 84.31 (15) and 59.37 (18)° with each other respectively. The dihedral angles between the two benzene rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 60.9 (2) and 85.40 (18)° for the two diphenylarsanyl groups respectively. The torsion angle of the methylthio group (C53–S1–C41–C42) being -4.5 (3)°.

In the crystal packing, the molecules are linked into a three-dimensional framework by intermolecular C4—H4A···O6, C24—H24A···O7 and C42—H42A···O1 hydrogen bonds (Fig. 2, Table 1). Weak intermolecular C—H···π interactions (Table 1) stabilize the crystal structure.

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, 2010a,b). For the synthesis of Ru₃(CO)₁₀(µ-Ph₂AsCH₂AsPh₂), see: Bruce et al. (1983) and for that of 4-methylthiophenyldiphenylphosphane, see: Fuhr et al. (2002). For the stability of the temperature controller used in the data collection, see: Cosier & Glazer (1986).

Experimental top

All manipulations were performed under a dry oxygen-free nitrogen atmosphere using standard Schlenk techniques. All solvents were dried over sodium and distilled from sodium benzophenone ketyl under dry oxygen free nitrogen. 4-Methylthiophenyldiphenylphosphane (Fuhr et al., 2002) and Ru₃(CO)₁₀(µ-Ph₂AsCH₂AsPh₂) (Bruce et al., 1983) was prepared by reported procedure. The title compound was obtained by refluxing equimolar quantities of Ru₃(CO)₁₀(µ-Ph₂AsCH₂AsPh₂) and 4-methylthiophenyldiphenylphosphane in hexane under nitrogen atmosphere. Crystals suitable for X-ray diffraction were grown by slow solvent / solvent diffusion of CH₃OH into CH₂Cl₂.

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); 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 50% probability ellipsoids for non-H atoms.
	Fig. 2. The crystal packing of the title compound, viewed down the b axis, showing the molecules are linked into a three-dimensional framework. Hydrogen atoms not involved in the hydrogen-bonding (dashed lines) have been omitted for clarity.

[µ-Bis(diphenylarsanyl)methane-1:2κ²As:As']nonacarbonyl- 1κ³C,2κ³C,3κ³C-[(4- methylsulfanylphenyl)diphenylphosphane-3κP]-triangulo- triruthenium(0) top

Crystal data top

[Ru₃(C₂₅H₂₂As₂)(C₁₉H₁₇PS)(CO)₉]	F(000) = 2632
M_r = 1335.92	D_x = 1.761 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9884 reflections
a = 16.1070 (11) Å	θ = 2.8–30.0°
b = 16.7244 (12) Å	µ = 2.32 mm⁻¹
c = 24.3147 (13) Å	T = 100 K
β = 129.712 (3)°	Needle, brown
V = 5038.6 (6) Å³	0.19 × 0.07 × 0.03 mm
Z = 4

Data collection top

Bruker APEXII DUO CCD area-detector diffractometer	14623 independent reflections
Radiation source: fine-focus sealed tube	11553 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.036
ϕ and ω scans	θ_max = 30.0°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2009)	h = −22→22
T_min = 0.660, T_max = 0.927	k = −22→23
41559 measured reflections	l = −34→30

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.081	H-atom parameters constrained
S = 1.02	w = 1/[σ²(F_o²) + (0.043P)² + 0.5735P] where P = (F_o² + 2F_c²)/3
14623 reflections	(Δ/σ)_max = 0.002
623 parameters	Δρ_max = 1.24 e Å⁻³
0 restraints	Δρ_min = −0.97 e Å⁻³

Crystal data top

[Ru₃(C₂₅H₂₂As₂)(C₁₉H₁₇PS)(CO)₉]	V = 5038.6 (6) Å³
M_r = 1335.92	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 16.1070 (11) Å	µ = 2.32 mm⁻¹
b = 16.7244 (12) Å	T = 100 K
c = 24.3147 (13) Å	0.19 × 0.07 × 0.03 mm
β = 129.712 (3)°

Data collection top

Bruker APEXII DUO CCD area-detector diffractometer	14623 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2009)	11553 reflections with I > 2σ(I)
T_min = 0.660, T_max = 0.927	R_int = 0.036
41559 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	0 restraints
wR(F²) = 0.081	H-atom parameters constrained
S = 1.02	Δρ_max = 1.24 e Å⁻³
14623 reflections	Δρ_min = −0.97 e Å⁻³
623 parameters

Special details top

Experimental. The crystal was placed in the cold stream of an Oxford Cryosystems Cobra open-flow nitrogen cryostat (Cosier & Glazer, 1986) operating at 100.0 (1) K.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ru1	0.298134 (17)	0.831631 (12)	0.779202 (12)	0.01628 (5)
Ru2	0.366549 (16)	0.752105 (11)	0.710419 (11)	0.01393 (5)
Ru3	0.229637 (16)	0.671585 (12)	0.727742 (11)	0.01448 (5)
As1	0.34320 (2)	0.961468 (15)	0.760642 (15)	0.01670 (6)
As2	0.48023 (2)	0.861583 (15)	0.726315 (14)	0.01358 (6)
S1	0.29520 (7)	0.30382 (5)	0.94198 (5)	0.03403 (18)
P1	0.11515 (5)	0.61875 (4)	0.74696 (4)	0.01794 (13)
O1	0.06273 (17)	0.85680 (13)	0.64359 (13)	0.0332 (5)
O2	0.2509 (2)	0.88001 (16)	0.87696 (15)	0.0481 (7)
O3	0.53465 (17)	0.81202 (12)	0.91484 (12)	0.0290 (5)
O4	0.55898 (18)	0.66694 (12)	0.84723 (12)	0.0305 (5)
O5	0.3699 (2)	0.62869 (13)	0.62036 (14)	0.0384 (6)
O6	0.17484 (18)	0.83165 (13)	0.57129 (12)	0.0314 (5)
O7	0.03756 (19)	0.70147 (14)	0.56881 (12)	0.0384 (5)
O8	0.2900 (2)	0.52208 (12)	0.69080 (13)	0.0350 (5)
O9	0.40236 (17)	0.65945 (12)	0.89112 (11)	0.0274 (4)
C1	0.2316 (2)	1.01511 (17)	0.67165 (17)	0.0258 (6)
C2	0.2373 (3)	1.02328 (19)	0.61772 (18)	0.0327 (7)
H2A	0.2977	1.0049	0.6244	0.039*
C3	0.1528 (3)	1.0589 (2)	0.5532 (2)	0.0501 (10)
H3A	0.1564	1.0628	0.5166	0.060*
C4	0.0652 (3)	1.0880 (3)	0.5430 (2)	0.0597 (12)
H4A	0.0101	1.1130	0.5002	0.072*
C5	0.0581 (3)	1.0804 (2)	0.5963 (3)	0.0587 (12)
H5A	−0.0018	1.1006	0.5893	0.070*
C6	0.1400 (3)	1.0425 (2)	0.6607 (2)	0.0422 (9)
H6A	0.1336	1.0355	0.6959	0.051*
C7	0.3912 (2)	1.04386 (16)	0.83213 (16)	0.0214 (5)
C8	0.3521 (3)	1.12121 (19)	0.8150 (2)	0.0395 (8)
H8A	0.3008	1.1363	0.7674	0.047*
C9	0.3895 (4)	1.1766 (2)	0.8691 (2)	0.0472 (10)
H9A	0.3613	1.2282	0.8574	0.057*
C10	0.4683 (3)	1.15544 (19)	0.9401 (2)	0.0368 (8)
H10A	0.4933	1.1927	0.9761	0.044*
C11	0.5094 (3)	1.07953 (19)	0.95709 (18)	0.0331 (7)
H11A	0.5640	1.0655	1.0046	0.040*
C12	0.4693 (2)	1.02319 (18)	0.90326 (17)	0.0286 (6)
H12A	0.4955	0.9711	0.9153	0.034*
C13	0.4691 (2)	0.96050 (15)	0.76505 (15)	0.0188 (5)
H13A	0.5341	0.9667	0.8144	0.023*
H13B	0.4647	1.0058	0.7383	0.023*
C14	0.4548 (2)	0.89586 (15)	0.63982 (14)	0.0168 (5)
C15	0.4669 (2)	0.97424 (16)	0.62777 (15)	0.0212 (5)
H15A	0.4911	1.0129	0.6626	0.025*
C16	0.4429 (2)	0.99524 (17)	0.56330 (16)	0.0257 (6)
H16A	0.4479	1.0483	0.5543	0.031*
C17	0.4117 (2)	0.93731 (17)	0.51296 (15)	0.0259 (6)
H17A	0.3957	0.9513	0.4701	0.031*
C18	0.4044 (2)	0.85851 (17)	0.52652 (16)	0.0263 (6)
H18A	0.3868	0.8191	0.4936	0.032*
C19	0.4231 (2)	0.83779 (16)	0.58862 (15)	0.0214 (5)
H19A	0.4145	0.7850	0.5962	0.026*
C20	0.6352 (2)	0.84273 (15)	0.79266 (14)	0.0172 (5)
C21	0.6878 (3)	0.8239 (2)	0.76698 (18)	0.0362 (8)
H21A	0.6499	0.8229	0.7179	0.043*
C22	0.7977 (3)	0.8064 (3)	0.8140 (2)	0.0511 (11)
H22A	0.8329	0.7937	0.7963	0.061*
C23	0.8542 (3)	0.8079 (2)	0.8867 (2)	0.0410 (8)
H23A	0.9271	0.7945	0.9180	0.049*
C24	0.8029 (3)	0.8291 (2)	0.91276 (18)	0.0397 (8)
H24A	0.8416	0.8323	0.9618	0.048*
C25	0.6924 (2)	0.8461 (2)	0.86547 (17)	0.0328 (7)
H25A	0.6573	0.8597	0.8832	0.039*
C26	−0.0185 (2)	0.58590 (17)	0.66644 (16)	0.0247 (6)
C27	−0.0235 (3)	0.54188 (19)	0.61625 (18)	0.0324 (7)
H27A	0.0397	0.5317	0.6236	0.039*
C28	−0.1211 (3)	0.5126 (2)	0.5550 (2)	0.0440 (9)
H28A	−0.1227	0.4827	0.5221	0.053*
C29	−0.2153 (3)	0.5280 (2)	0.5434 (2)	0.0475 (10)
H29A	−0.2810	0.5097	0.5020	0.057*
C30	−0.2115 (3)	0.5704 (2)	0.5933 (2)	0.0500 (10)
H30A	−0.2749	0.5799	0.5858	0.060*
C31	−0.1137 (2)	0.5997 (2)	0.6553 (2)	0.0367 (8)
H31A	−0.1122	0.6282	0.6887	0.044*
C32	0.0890 (2)	0.68742 (16)	0.79316 (16)	0.0210 (5)
C33	0.0218 (2)	0.75348 (16)	0.75643 (17)	0.0260 (6)
H33A	−0.0135	0.7601	0.7080	0.031*
C34	0.0078 (3)	0.80941 (18)	0.79248 (19)	0.0320 (7)
H34A	−0.0383	0.8526	0.7678	0.038*
C35	0.0627 (3)	0.80081 (19)	0.8652 (2)	0.0336 (7)
H35A	0.0541	0.8388	0.8891	0.040*
C36	0.1295 (3)	0.73659 (19)	0.90170 (19)	0.0341 (7)
H36A	0.1657	0.7310	0.9503	0.041*
C37	0.1433 (2)	0.67957 (17)	0.86618 (17)	0.0268 (6)
H37A	0.1889	0.6362	0.8913	0.032*
C38	0.1634 (2)	0.52798 (15)	0.80201 (15)	0.0191 (5)
C39	0.2553 (2)	0.48814 (16)	0.82327 (15)	0.0209 (5)
H39A	0.2932	0.5077	0.8091	0.025*
C40	0.2921 (2)	0.41979 (16)	0.86515 (15)	0.0223 (5)
H40A	0.3532	0.3937	0.8779	0.027*
C41	0.2383 (2)	0.38980 (15)	0.88827 (15)	0.0206 (5)
C42	0.1459 (2)	0.42901 (17)	0.86758 (16)	0.0240 (6)
H42A	0.1093	0.4102	0.8829	0.029*
C43	0.1082 (2)	0.49637 (16)	0.82400 (16)	0.0236 (6)
H43A	0.0450	0.5209	0.8092	0.028*
C44	0.1501 (2)	0.84081 (16)	0.69206 (17)	0.0242 (6)
C45	0.2641 (2)	0.86080 (18)	0.83811 (17)	0.0274 (6)
C46	0.4472 (2)	0.81506 (15)	0.86264 (16)	0.0211 (5)
C47	0.4857 (2)	0.69993 (16)	0.79802 (16)	0.0215 (5)
C48	0.3713 (2)	0.67561 (16)	0.65498 (16)	0.0231 (6)
C49	0.2428 (2)	0.80292 (16)	0.62486 (15)	0.0211 (5)
C50	0.1099 (2)	0.69369 (17)	0.62778 (16)	0.0246 (6)
C51	0.2650 (2)	0.57719 (16)	0.70502 (15)	0.0216 (5)
C52	0.3425 (2)	0.67135 (15)	0.83039 (15)	0.0194 (5)
C53	0.2174 (3)	0.2842 (2)	0.9688 (2)	0.0429 (9)
H53A	0.2453	0.2377	0.9990	0.064*
H53B	0.1436	0.2749	0.9273	0.064*
H53C	0.2210	0.3293	0.9947	0.064*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ru1	0.01661 (10)	0.01670 (10)	0.01801 (11)	−0.00152 (7)	0.01220 (9)	−0.00249 (8)
Ru2	0.01341 (9)	0.01460 (9)	0.01386 (10)	−0.00012 (7)	0.00875 (8)	−0.00023 (7)
Ru3	0.01278 (9)	0.01571 (10)	0.01328 (10)	−0.00109 (7)	0.00754 (8)	0.00002 (7)
As1	0.01609 (12)	0.01591 (12)	0.01858 (14)	0.00069 (9)	0.01129 (12)	−0.00089 (10)
As2	0.01239 (12)	0.01535 (12)	0.01197 (12)	0.00032 (9)	0.00731 (10)	0.00076 (9)
S1	0.0378 (4)	0.0299 (4)	0.0409 (5)	0.0113 (3)	0.0281 (4)	0.0160 (3)
P1	0.0141 (3)	0.0199 (3)	0.0190 (3)	0.0006 (2)	0.0102 (3)	0.0025 (3)
O1	0.0187 (11)	0.0406 (13)	0.0310 (13)	0.0015 (9)	0.0116 (10)	−0.0017 (10)
O2	0.0478 (16)	0.0701 (18)	0.0462 (16)	−0.0237 (13)	0.0392 (15)	−0.0314 (14)
O3	0.0225 (11)	0.0317 (11)	0.0220 (11)	0.0001 (9)	0.0092 (10)	0.0004 (9)
O4	0.0251 (11)	0.0290 (11)	0.0265 (12)	0.0067 (9)	0.0113 (10)	0.0087 (9)
O5	0.0584 (17)	0.0286 (12)	0.0450 (15)	−0.0044 (11)	0.0407 (15)	−0.0102 (10)
O6	0.0223 (11)	0.0380 (12)	0.0222 (11)	0.0046 (9)	0.0088 (10)	0.0073 (9)
O7	0.0273 (12)	0.0419 (13)	0.0180 (11)	−0.0101 (10)	0.0014 (10)	0.0039 (10)
O8	0.0475 (15)	0.0246 (11)	0.0422 (15)	0.0024 (10)	0.0329 (13)	−0.0018 (10)
O9	0.0277 (11)	0.0290 (11)	0.0170 (10)	−0.0040 (8)	0.0105 (10)	0.0027 (8)
C1	0.0174 (13)	0.0218 (13)	0.0274 (16)	0.0036 (10)	0.0094 (13)	0.0018 (12)
C2	0.0225 (15)	0.0345 (17)	0.0273 (17)	0.0013 (13)	0.0095 (14)	0.0065 (13)
C3	0.035 (2)	0.056 (2)	0.029 (2)	0.0036 (17)	0.0070 (17)	0.0167 (17)
C4	0.034 (2)	0.056 (3)	0.044 (3)	0.0121 (18)	0.004 (2)	0.023 (2)
C5	0.0236 (18)	0.053 (2)	0.063 (3)	0.0188 (17)	0.011 (2)	0.008 (2)
C6	0.0255 (17)	0.047 (2)	0.049 (2)	0.0115 (15)	0.0211 (18)	0.0067 (17)
C7	0.0244 (14)	0.0220 (13)	0.0240 (14)	−0.0030 (10)	0.0183 (13)	−0.0060 (11)
C8	0.062 (2)	0.0271 (16)	0.0338 (19)	0.0045 (16)	0.033 (2)	−0.0005 (14)
C9	0.086 (3)	0.0215 (16)	0.047 (2)	0.0041 (17)	0.048 (3)	−0.0027 (15)
C10	0.055 (2)	0.0294 (16)	0.039 (2)	−0.0137 (15)	0.036 (2)	−0.0135 (14)
C11	0.0319 (17)	0.0369 (17)	0.0244 (16)	−0.0085 (13)	0.0151 (15)	−0.0105 (13)
C12	0.0245 (15)	0.0258 (15)	0.0299 (17)	−0.0049 (12)	0.0148 (14)	−0.0103 (12)
C13	0.0159 (12)	0.0213 (13)	0.0181 (13)	−0.0016 (10)	0.0104 (11)	−0.0027 (10)
C14	0.0162 (12)	0.0202 (12)	0.0132 (12)	0.0012 (9)	0.0090 (11)	0.0030 (10)
C15	0.0221 (13)	0.0212 (13)	0.0174 (13)	−0.0008 (10)	0.0112 (12)	0.0011 (10)
C16	0.0282 (15)	0.0235 (14)	0.0226 (15)	−0.0015 (11)	0.0150 (13)	0.0051 (11)
C17	0.0263 (15)	0.0326 (15)	0.0142 (13)	−0.0034 (12)	0.0108 (12)	0.0029 (11)
C18	0.0295 (16)	0.0286 (15)	0.0178 (14)	−0.0033 (12)	0.0137 (13)	−0.0027 (12)
C19	0.0259 (14)	0.0176 (12)	0.0195 (14)	−0.0026 (10)	0.0139 (13)	−0.0002 (10)
C20	0.0107 (11)	0.0191 (12)	0.0166 (13)	0.0003 (9)	0.0063 (11)	0.0024 (10)
C21	0.0195 (15)	0.061 (2)	0.0220 (16)	0.0041 (14)	0.0104 (14)	−0.0085 (15)
C22	0.0197 (16)	0.094 (3)	0.034 (2)	0.0078 (18)	0.0144 (16)	−0.014 (2)
C23	0.0148 (14)	0.058 (2)	0.036 (2)	0.0091 (14)	0.0097 (15)	0.0066 (17)
C24	0.0187 (15)	0.070 (2)	0.0204 (16)	0.0041 (15)	0.0077 (14)	0.0133 (16)
C25	0.0183 (14)	0.059 (2)	0.0199 (15)	0.0046 (14)	0.0118 (13)	0.0092 (14)
C26	0.0163 (13)	0.0242 (14)	0.0252 (15)	−0.0027 (10)	0.0093 (12)	0.0055 (11)
C27	0.0253 (15)	0.0383 (17)	0.0255 (16)	−0.0085 (13)	0.0125 (14)	−0.0021 (13)
C28	0.041 (2)	0.045 (2)	0.0294 (19)	−0.0199 (17)	0.0149 (17)	−0.0050 (16)
C29	0.0271 (18)	0.045 (2)	0.034 (2)	−0.0156 (15)	0.0027 (16)	0.0013 (17)
C30	0.0155 (15)	0.046 (2)	0.062 (3)	0.0002 (14)	0.0127 (18)	0.007 (2)
C31	0.0185 (15)	0.0367 (18)	0.045 (2)	−0.0029 (13)	0.0161 (16)	−0.0007 (15)
C32	0.0205 (13)	0.0220 (13)	0.0254 (15)	0.0002 (10)	0.0169 (13)	0.0009 (11)
C33	0.0262 (15)	0.0267 (15)	0.0257 (15)	0.0045 (11)	0.0168 (14)	0.0047 (12)
C34	0.0325 (17)	0.0277 (15)	0.0396 (19)	0.0074 (13)	0.0248 (16)	0.0037 (14)
C35	0.0383 (18)	0.0324 (16)	0.045 (2)	−0.0012 (14)	0.0336 (18)	−0.0054 (15)
C36	0.0415 (19)	0.0359 (17)	0.0312 (18)	−0.0007 (14)	0.0262 (17)	−0.0003 (14)
C37	0.0256 (15)	0.0283 (15)	0.0280 (16)	0.0031 (12)	0.0178 (14)	0.0023 (12)
C38	0.0154 (12)	0.0199 (12)	0.0179 (13)	−0.0025 (10)	0.0088 (11)	0.0005 (10)
C39	0.0222 (13)	0.0217 (13)	0.0210 (14)	0.0008 (10)	0.0147 (12)	0.0015 (11)
C40	0.0212 (13)	0.0234 (13)	0.0213 (14)	0.0022 (10)	0.0131 (12)	0.0000 (11)
C41	0.0225 (13)	0.0163 (12)	0.0179 (13)	−0.0001 (10)	0.0106 (12)	0.0021 (10)
C42	0.0233 (14)	0.0252 (14)	0.0251 (15)	−0.0031 (11)	0.0162 (13)	0.0030 (11)
C43	0.0179 (13)	0.0247 (14)	0.0272 (15)	0.0006 (10)	0.0139 (13)	0.0043 (12)
C44	0.0229 (14)	0.0240 (14)	0.0284 (16)	−0.0032 (11)	0.0177 (14)	−0.0060 (12)
C45	0.0242 (14)	0.0319 (15)	0.0303 (16)	−0.0087 (12)	0.0193 (14)	−0.0101 (13)
C46	0.0264 (14)	0.0171 (12)	0.0229 (14)	−0.0017 (10)	0.0172 (13)	−0.0007 (10)
C47	0.0220 (13)	0.0209 (13)	0.0252 (15)	−0.0018 (11)	0.0167 (13)	−0.0004 (11)
C48	0.0296 (15)	0.0198 (13)	0.0257 (15)	−0.0010 (11)	0.0204 (14)	−0.0005 (11)
C49	0.0175 (13)	0.0234 (13)	0.0203 (14)	−0.0026 (10)	0.0112 (12)	−0.0021 (11)
C50	0.0210 (14)	0.0227 (14)	0.0229 (15)	−0.0045 (11)	0.0107 (13)	0.0013 (11)
C51	0.0192 (13)	0.0235 (13)	0.0204 (14)	−0.0003 (10)	0.0118 (12)	0.0002 (11)
C52	0.0205 (13)	0.0190 (12)	0.0202 (14)	−0.0041 (10)	0.0138 (12)	−0.0015 (10)
C53	0.0381 (19)	0.051 (2)	0.044 (2)	0.0112 (16)	0.0284 (19)	0.0252 (17)

Geometric parameters (Å, º) top

Ru1—C45	1.895 (3)	C13—H13B	0.9700
Ru1—C46	1.932 (3)	C14—C15	1.384 (3)
Ru1—C44	1.934 (3)	C14—C19	1.394 (4)
Ru1—As1	2.4217 (3)	C15—C16	1.398 (4)
Ru1—Ru2	2.8522 (3)	C15—H15A	0.9300
Ru1—Ru3	2.8606 (3)	C16—C17	1.380 (4)
Ru2—C48	1.895 (3)	C16—H16A	0.9300
Ru2—C49	1.930 (3)	C17—C18	1.382 (4)
Ru2—C47	1.938 (3)	C17—H17A	0.9300
Ru2—As2	2.4393 (3)	C18—C19	1.382 (4)
Ru2—Ru3	2.8357 (3)	C18—H18A	0.9300
Ru3—C51	1.878 (3)	C19—H19A	0.9300
Ru3—C52	1.933 (3)	C20—C21	1.372 (4)
Ru3—C50	1.943 (3)	C20—C25	1.379 (4)
Ru3—P1	2.3453 (7)	C21—C22	1.393 (4)
As1—C1	1.936 (3)	C21—H21A	0.9300
As1—C7	1.950 (3)	C22—C23	1.377 (5)
As1—C13	1.962 (2)	C22—H22A	0.9300
As2—C20	1.946 (3)	C23—C24	1.372 (5)
As2—C14	1.954 (2)	C23—H23A	0.9300
As2—C13	1.967 (3)	C24—C25	1.399 (4)
S1—C41	1.756 (3)	C24—H24A	0.9300
S1—C53	1.775 (3)	C25—H25A	0.9300
P1—C32	1.834 (3)	C26—C27	1.383 (4)
P1—C38	1.836 (3)	C26—C31	1.395 (4)
P1—C26	1.839 (3)	C27—C28	1.392 (5)
O1—C44	1.150 (4)	C27—H27A	0.9300
O2—C45	1.140 (3)	C28—C29	1.379 (6)
O3—C46	1.146 (4)	C28—H28A	0.9300
O4—C47	1.151 (3)	C29—C30	1.374 (6)
O5—C48	1.140 (3)	C29—H29A	0.9300
O6—C49	1.142 (3)	C30—C31	1.399 (5)
O7—C50	1.138 (4)	C30—H30A	0.9300
O8—C51	1.144 (3)	C31—H31A	0.9300
O9—C52	1.153 (3)	C32—C37	1.397 (4)
C1—C2	1.378 (4)	C32—C33	1.398 (4)
C1—C6	1.400 (4)	C33—C34	1.395 (4)
C2—C3	1.394 (5)	C33—H33A	0.9300
C2—H2A	0.9300	C34—C35	1.389 (5)
C3—C4	1.358 (6)	C34—H34A	0.9300
C3—H3A	0.9300	C35—C36	1.371 (5)
C4—C5	1.377 (7)	C35—H35A	0.9300
C4—H4A	0.9300	C36—C37	1.397 (4)
C5—C6	1.399 (6)	C36—H36A	0.9300
C5—H5A	0.9300	C37—H37A	0.9300
C6—H6A	0.9300	C38—C39	1.388 (4)
C7—C8	1.381 (4)	C38—C43	1.401 (3)
C7—C12	1.383 (4)	C39—C40	1.387 (4)
C8—C9	1.392 (5)	C39—H39A	0.9300
C8—H8A	0.9300	C40—C41	1.394 (4)
C9—C10	1.385 (6)	C40—H40A	0.9300
C9—H9A	0.9300	C41—C42	1.393 (4)
C10—C11	1.368 (5)	C42—C43	1.392 (4)
C10—H10A	0.9300	C42—H42A	0.9300
C11—C12	1.392 (4)	C43—H43A	0.9300
C11—H11A	0.9300	C53—H53A	0.9600
C12—H12A	0.9300	C53—H53B	0.9600
C13—H13A	0.9700	C53—H53C	0.9600

C45—Ru1—C46	90.51 (13)	C15—C14—C19	119.4 (2)
C45—Ru1—C44	93.36 (13)	C15—C14—As2	123.0 (2)
C46—Ru1—C44	175.24 (11)	C19—C14—As2	117.54 (19)
C45—Ru1—As1	100.13 (9)	C14—C15—C16	120.0 (3)
C46—Ru1—As1	90.28 (8)	C14—C15—H15A	120.0
C44—Ru1—As1	91.78 (8)	C16—C15—H15A	120.0
C45—Ru1—Ru2	165.84 (10)	C17—C16—C15	120.1 (3)
C46—Ru1—Ru2	82.08 (8)	C17—C16—H16A	120.0
C44—Ru1—Ru2	93.56 (8)	C15—C16—H16A	120.0
As1—Ru1—Ru2	91.991 (10)	C16—C17—C18	119.8 (3)
C45—Ru1—Ru3	110.76 (9)	C16—C17—H17A	120.1
C46—Ru1—Ru3	101.44 (8)	C18—C17—H17A	120.1
C44—Ru1—Ru3	74.58 (8)	C17—C18—C19	120.5 (3)
As1—Ru1—Ru3	146.643 (11)	C17—C18—H18A	119.7
Ru2—Ru1—Ru3	59.519 (7)	C19—C18—H18A	119.7
C48—Ru2—C49	90.79 (12)	C18—C19—C14	120.1 (2)
C48—Ru2—C47	90.92 (12)	C18—C19—H19A	120.0
C49—Ru2—C47	176.61 (11)	C14—C19—H19A	120.0
C48—Ru2—As2	104.59 (8)	C21—C20—C25	119.6 (3)
C49—Ru2—As2	89.66 (8)	C21—C20—As2	119.9 (2)
C47—Ru2—As2	92.75 (8)	C25—C20—As2	120.5 (2)
C48—Ru2—Ru3	100.01 (8)	C20—C21—C22	120.3 (3)
C49—Ru2—Ru3	90.21 (8)	C20—C21—H21A	119.8
C47—Ru2—Ru3	86.61 (7)	C22—C21—H21A	119.8
As2—Ru2—Ru3	155.395 (11)	C23—C22—C21	120.1 (3)
C48—Ru2—Ru1	159.76 (8)	C23—C22—H22A	120.0
C49—Ru2—Ru1	84.66 (8)	C21—C22—H22A	120.0
C47—Ru2—Ru1	92.74 (8)	C24—C23—C22	119.9 (3)
As2—Ru2—Ru1	95.117 (10)	C24—C23—H23A	120.1
Ru3—Ru2—Ru1	60.388 (8)	C22—C23—H23A	120.1
C51—Ru3—C52	99.57 (12)	C23—C24—C25	119.9 (3)
C51—Ru3—C50	92.14 (12)	C23—C24—H24A	120.0
C52—Ru3—C50	168.17 (12)	C25—C24—H24A	120.0
C51—Ru3—P1	99.62 (8)	C20—C25—C24	120.1 (3)
C52—Ru3—P1	87.27 (8)	C20—C25—H25A	119.9
C50—Ru3—P1	92.44 (8)	C24—C25—H25A	119.9
C51—Ru3—Ru2	86.81 (8)	C27—C26—C31	118.7 (3)
C52—Ru3—Ru2	90.79 (7)	C27—C26—P1	117.8 (2)
C50—Ru3—Ru2	88.19 (8)	C31—C26—P1	123.4 (3)
P1—Ru3—Ru2	173.506 (19)	C26—C27—C28	121.3 (3)
C51—Ru3—Ru1	144.16 (8)	C26—C27—H27A	119.3
C52—Ru3—Ru1	69.84 (8)	C28—C27—H27A	119.3
C50—Ru3—Ru1	99.57 (8)	C29—C28—C27	119.8 (4)
P1—Ru3—Ru1	113.452 (19)	C29—C28—H28A	120.1
Ru2—Ru3—Ru1	60.093 (7)	C27—C28—H28A	120.1
C1—As1—C7	103.01 (12)	C30—C29—C28	119.6 (3)
C1—As1—C13	104.72 (12)	C30—C29—H29A	120.2
C7—As1—C13	98.63 (11)	C28—C29—H29A	120.2
C1—As1—Ru1	116.68 (9)	C29—C30—C31	121.1 (3)
C7—As1—Ru1	117.57 (8)	C29—C30—H30A	119.5
C13—As1—Ru1	113.89 (8)	C31—C30—H30A	119.5
C20—As2—C14	102.46 (11)	C26—C31—C30	119.5 (4)
C20—As2—C13	101.54 (11)	C26—C31—H31A	120.2
C14—As2—C13	104.34 (11)	C30—C31—H31A	120.2
C20—As2—Ru2	116.43 (7)	C37—C32—C33	119.1 (3)
C14—As2—Ru2	115.44 (8)	C37—C32—P1	121.2 (2)
C13—As2—Ru2	114.74 (7)	C33—C32—P1	119.4 (2)
C41—S1—C53	105.61 (15)	C34—C33—C32	119.9 (3)
C32—P1—C38	103.11 (12)	C34—C33—H33A	120.1
C32—P1—C26	105.57 (13)	C32—C33—H33A	120.1
C38—P1—C26	101.02 (12)	C35—C34—C33	120.2 (3)
C32—P1—Ru3	113.81 (9)	C35—C34—H34A	119.9
C38—P1—Ru3	115.89 (8)	C33—C34—H34A	119.9
C26—P1—Ru3	115.78 (9)	C36—C35—C34	120.2 (3)
C2—C1—C6	119.4 (3)	C36—C35—H35A	119.9
C2—C1—As1	122.1 (2)	C34—C35—H35A	119.9
C6—C1—As1	118.5 (3)	C35—C36—C37	120.2 (3)
C1—C2—C3	120.2 (3)	C35—C36—H36A	119.9
C1—C2—H2A	119.9	C37—C36—H36A	119.9
C3—C2—H2A	119.9	C36—C37—C32	120.3 (3)
C4—C3—C2	120.8 (4)	C36—C37—H37A	119.9
C4—C3—H3A	119.6	C32—C37—H37A	119.9
C2—C3—H3A	119.6	C39—C38—C43	117.6 (2)
C3—C4—C5	119.8 (4)	C39—C38—P1	121.46 (19)
C3—C4—H4A	120.1	C43—C38—P1	120.9 (2)
C5—C4—H4A	120.1	C40—C39—C38	121.5 (2)
C4—C5—C6	120.7 (4)	C40—C39—H39A	119.3
C4—C5—H5A	119.7	C38—C39—H39A	119.3
C6—C5—H5A	119.7	C39—C40—C41	120.6 (2)
C5—C6—C1	119.1 (4)	C39—C40—H40A	119.7
C5—C6—H6A	120.5	C41—C40—H40A	119.7
C1—C6—H6A	120.5	C42—C41—C40	118.8 (2)
C8—C7—C12	119.1 (3)	C42—C41—S1	125.7 (2)
C8—C7—As1	123.3 (2)	C40—C41—S1	115.5 (2)
C12—C7—As1	117.6 (2)	C43—C42—C41	120.1 (2)
C7—C8—C9	120.0 (3)	C43—C42—H42A	119.9
C7—C8—H8A	120.0	C41—C42—H42A	119.9
C9—C8—H8A	120.0	C42—C43—C38	121.4 (2)
C10—C9—C8	120.4 (3)	C42—C43—H43A	119.3
C10—C9—H9A	119.8	C38—C43—H43A	119.3
C8—C9—H9A	119.8	O1—C44—Ru1	170.4 (2)
C11—C10—C9	119.7 (3)	O2—C45—Ru1	175.3 (3)
C11—C10—H10A	120.2	O3—C46—Ru1	173.1 (2)
C9—C10—H10A	120.2	O4—C47—Ru2	174.8 (2)
C10—C11—C12	120.0 (3)	O5—C48—Ru2	177.1 (3)
C10—C11—H11A	120.0	O6—C49—Ru2	172.8 (2)
C12—C11—H11A	120.0	O7—C50—Ru3	175.4 (2)
C7—C12—C11	120.7 (3)	O8—C51—Ru3	176.4 (2)
C7—C12—H12A	119.6	O9—C52—Ru3	168.7 (2)
C11—C12—H12A	119.6	S1—C53—H53A	109.5
As1—C13—As2	112.81 (12)	S1—C53—H53B	109.5
As1—C13—H13A	109.0	H53A—C53—H53B	109.5
As2—C13—H13A	109.0	S1—C53—H53C	109.5
As1—C13—H13B	109.0	H53A—C53—H53C	109.5
As2—C13—H13B	109.0	H53B—C53—H53C	109.5
H13A—C13—H13B	107.8

C45—Ru1—Ru2—C48	64.9 (5)	Ru1—As1—C1—C2	−108.3 (2)
C46—Ru1—Ru2—C48	123.9 (3)	C7—As1—C1—C6	−62.1 (3)
C44—Ru1—Ru2—C48	−54.2 (3)	C13—As1—C1—C6	−164.8 (2)
As1—Ru1—Ru2—C48	−146.1 (3)	Ru1—As1—C1—C6	68.2 (3)
Ru3—Ru1—Ru2—C48	15.6 (3)	C6—C1—C2—C3	0.4 (5)
C45—Ru1—Ru2—C49	142.6 (4)	As1—C1—C2—C3	176.9 (3)
C46—Ru1—Ru2—C49	−158.40 (11)	C1—C2—C3—C4	1.8 (6)
C44—Ru1—Ru2—C49	23.51 (12)	C2—C3—C4—C5	−1.8 (7)
As1—Ru1—Ru2—C49	−68.39 (8)	C3—C4—C5—C6	−0.4 (7)
Ru3—Ru1—Ru2—C49	93.29 (8)	C4—C5—C6—C1	2.5 (6)
C45—Ru1—Ru2—C47	−35.2 (4)	C2—C1—C6—C5	−2.5 (5)
C46—Ru1—Ru2—C47	23.78 (11)	As1—C1—C6—C5	−179.2 (3)
C44—Ru1—Ru2—C47	−154.31 (11)	C1—As1—C7—C8	−3.5 (3)
As1—Ru1—Ru2—C47	113.78 (8)	C13—As1—C7—C8	103.9 (3)
Ru3—Ru1—Ru2—C47	−84.53 (8)	Ru1—As1—C7—C8	−133.3 (2)
C45—Ru1—Ru2—As2	−128.2 (4)	C1—As1—C7—C12	177.4 (2)
C46—Ru1—Ru2—As2	−69.22 (8)	C13—As1—C7—C12	−75.2 (2)
C44—Ru1—Ru2—As2	112.68 (8)	Ru1—As1—C7—C12	47.5 (2)
As1—Ru1—Ru2—As2	20.778 (12)	C12—C7—C8—C9	−1.5 (5)
Ru3—Ru1—Ru2—As2	−177.538 (11)	As1—C7—C8—C9	179.4 (3)
C45—Ru1—Ru2—Ru3	49.3 (4)	C7—C8—C9—C10	2.0 (6)
C46—Ru1—Ru2—Ru3	108.32 (8)	C8—C9—C10—C11	−0.2 (6)
C44—Ru1—Ru2—Ru3	−69.78 (8)	C9—C10—C11—C12	−2.1 (5)
As1—Ru1—Ru2—Ru3	−161.683 (12)	C8—C7—C12—C11	−0.8 (4)
C48—Ru2—Ru3—C51	19.80 (13)	As1—C7—C12—C11	178.4 (2)
C49—Ru2—Ru3—C51	110.64 (12)	C10—C11—C12—C7	2.7 (5)
C47—Ru2—Ru3—C51	−70.54 (12)	C1—As1—C13—As2	−93.82 (15)
As2—Ru2—Ru3—C51	−159.73 (9)	C7—As1—C13—As2	160.20 (14)
Ru1—Ru2—Ru3—C51	−165.63 (9)	Ru1—As1—C13—As2	34.79 (15)
C48—Ru2—Ru3—C52	119.35 (12)	C20—As2—C13—As1	−141.11 (13)
C49—Ru2—Ru3—C52	−149.81 (11)	C14—As2—C13—As1	112.66 (14)
C47—Ru2—Ru3—C52	29.01 (11)	Ru2—As2—C13—As1	−14.64 (16)
As2—Ru2—Ru3—C52	−60.18 (8)	C20—As2—C14—C15	−85.2 (2)
Ru1—Ru2—Ru3—C52	−66.08 (8)	C13—As2—C14—C15	20.4 (2)
C48—Ru2—Ru3—C50	−72.44 (13)	Ru2—As2—C14—C15	147.2 (2)
C49—Ru2—Ru3—C50	18.40 (12)	C20—As2—C14—C19	94.7 (2)
C47—Ru2—Ru3—C50	−162.78 (12)	C13—As2—C14—C19	−159.7 (2)
As2—Ru2—Ru3—C50	108.03 (9)	Ru2—As2—C14—C19	−32.9 (2)
Ru1—Ru2—Ru3—C50	102.13 (9)	C19—C14—C15—C16	2.8 (4)
C48—Ru2—Ru3—Ru1	−174.57 (9)	As2—C14—C15—C16	−177.3 (2)
C49—Ru2—Ru3—Ru1	−83.73 (8)	C14—C15—C16—C17	−2.9 (4)
C47—Ru2—Ru3—Ru1	95.09 (8)	C15—C16—C17—C18	0.0 (5)
As2—Ru2—Ru3—Ru1	5.90 (3)	C16—C17—C18—C19	3.1 (5)
C45—Ru1—Ru3—C51	−143.52 (18)	C17—C18—C19—C14	−3.2 (5)
C46—Ru1—Ru3—C51	−48.56 (17)	C15—C14—C19—C18	0.2 (4)
C44—Ru1—Ru3—C51	128.75 (17)	As2—C14—C19—C18	−179.7 (2)
As1—Ru1—Ru3—C51	59.88 (15)	C14—As2—C20—C21	−25.6 (3)
Ru2—Ru1—Ru3—C51	25.04 (15)	C13—As2—C20—C21	−133.3 (2)
C45—Ru1—Ru3—C52	−65.38 (13)	Ru2—As2—C20—C21	101.4 (2)
C46—Ru1—Ru3—C52	29.57 (11)	C14—As2—C20—C25	156.1 (2)
C44—Ru1—Ru3—C52	−153.11 (12)	C13—As2—C20—C25	48.4 (3)
As1—Ru1—Ru3—C52	138.01 (8)	Ru2—As2—C20—C25	−76.9 (2)
Ru2—Ru1—Ru3—C52	103.18 (8)	C25—C20—C21—C22	1.6 (5)
C45—Ru1—Ru3—C50	109.14 (14)	As2—C20—C21—C22	−176.8 (3)
C46—Ru1—Ru3—C50	−155.90 (12)	C20—C21—C22—C23	0.0 (6)
C44—Ru1—Ru3—C50	21.41 (12)	C21—C22—C23—C24	−2.1 (6)
As1—Ru1—Ru3—C50	−47.46 (9)	C22—C23—C24—C25	2.6 (6)
Ru2—Ru1—Ru3—C50	−82.30 (9)	C21—C20—C25—C24	−1.0 (5)
C45—Ru1—Ru3—P1	12.24 (11)	As2—C20—C25—C24	177.3 (3)
C46—Ru1—Ru3—P1	107.19 (8)	C23—C24—C25—C20	−1.0 (5)
C44—Ru1—Ru3—P1	−75.49 (9)	C32—P1—C26—C27	171.3 (2)
As1—Ru1—Ru3—P1	−144.37 (3)	C38—P1—C26—C27	−81.6 (2)
Ru2—Ru1—Ru3—P1	−179.20 (2)	Ru3—P1—C26—C27	44.4 (3)
C45—Ru1—Ru3—Ru2	−168.56 (11)	C32—P1—C26—C31	−11.9 (3)
C46—Ru1—Ru3—Ru2	−73.61 (8)	C38—P1—C26—C31	95.2 (3)
C44—Ru1—Ru3—Ru2	103.71 (8)	Ru3—P1—C26—C31	−138.8 (2)
As1—Ru1—Ru3—Ru2	34.83 (2)	C31—C26—C27—C28	0.9 (5)
C45—Ru1—As1—C1	−98.91 (14)	P1—C26—C27—C28	177.9 (3)
C46—Ru1—As1—C1	170.52 (12)	C26—C27—C28—C29	0.5 (5)
C44—Ru1—As1—C1	−5.19 (13)	C27—C28—C29—C30	−1.6 (6)
Ru2—Ru1—As1—C1	88.44 (10)	C28—C29—C30—C31	1.2 (6)
Ru3—Ru1—As1—C1	58.93 (10)	C27—C26—C31—C30	−1.3 (5)
C45—Ru1—As1—C7	24.23 (14)	P1—C26—C31—C30	−178.1 (3)
C46—Ru1—As1—C7	−66.34 (12)	C29—C30—C31—C26	0.3 (6)
C44—Ru1—As1—C7	117.95 (12)	C38—P1—C32—C37	25.6 (3)
Ru2—Ru1—As1—C7	−148.42 (9)	C26—P1—C32—C37	131.2 (2)
Ru3—Ru1—As1—C7	−177.93 (9)	Ru3—P1—C32—C37	−100.8 (2)
C45—Ru1—As1—C13	138.84 (13)	C38—P1—C32—C33	−160.9 (2)
C46—Ru1—As1—C13	48.28 (12)	C26—P1—C32—C33	−55.3 (2)
C44—Ru1—As1—C13	−127.43 (12)	Ru3—P1—C32—C33	72.7 (2)
Ru2—Ru1—As1—C13	−33.81 (9)	C37—C32—C33—C34	−1.5 (4)
Ru3—Ru1—As1—C13	−63.32 (9)	P1—C32—C33—C34	−175.1 (2)
C48—Ru2—As2—C20	−73.55 (13)	C32—C33—C34—C35	1.7 (5)
C49—Ru2—As2—C20	−164.28 (12)	C33—C34—C35—C36	−1.1 (5)
C47—Ru2—As2—C20	18.12 (12)	C34—C35—C36—C37	0.3 (5)
Ru3—Ru2—As2—C20	105.97 (9)	C35—C36—C37—C32	−0.2 (5)
Ru1—Ru2—As2—C20	111.12 (9)	C33—C32—C37—C36	0.8 (4)
C48—Ru2—As2—C14	46.67 (13)	P1—C32—C37—C36	174.3 (2)
C49—Ru2—As2—C14	−44.06 (11)	C32—P1—C38—C39	−132.6 (2)
C47—Ru2—As2—C14	138.34 (11)	C26—P1—C38—C39	118.4 (2)
Ru3—Ru2—As2—C14	−133.81 (8)	Ru3—P1—C38—C39	−7.6 (3)
Ru1—Ru2—As2—C14	−128.66 (8)	C32—P1—C38—C43	47.5 (3)
C48—Ru2—As2—C13	168.08 (13)	C26—P1—C38—C43	−61.5 (3)
C49—Ru2—As2—C13	77.35 (12)	Ru3—P1—C38—C43	172.5 (2)
C47—Ru2—As2—C13	−100.25 (12)	C43—C38—C39—C40	−0.4 (4)
Ru3—Ru2—As2—C13	−12.39 (10)	P1—C38—C39—C40	179.7 (2)
Ru1—Ru2—As2—C13	−7.25 (9)	C38—C39—C40—C41	−1.1 (4)
C51—Ru3—P1—C32	164.97 (14)	C39—C40—C41—C42	1.0 (4)
C52—Ru3—P1—C32	65.71 (13)	C39—C40—C41—S1	−179.1 (2)
C50—Ru3—P1—C32	−102.45 (14)	C53—S1—C41—C42	−4.5 (3)
Ru1—Ru3—P1—C32	−0.92 (11)	C53—S1—C41—C40	175.6 (2)
C51—Ru3—P1—C38	45.64 (13)	C40—C41—C42—C43	0.7 (4)
C52—Ru3—P1—C38	−53.62 (13)	S1—C41—C42—C43	−179.2 (2)
C50—Ru3—P1—C38	138.22 (13)	C41—C42—C43—C38	−2.3 (5)
Ru1—Ru3—P1—C38	−120.25 (10)	C39—C38—C43—C42	2.1 (4)
C51—Ru3—P1—C26	−72.42 (14)	P1—C38—C43—C42	−178.0 (2)
C52—Ru3—P1—C26	−171.68 (13)	C51—Ru3—C52—O9	−60.8 (12)
C50—Ru3—P1—C26	20.16 (13)	C50—Ru3—C52—O9	127.4 (11)
Ru1—Ru3—P1—C26	121.69 (10)	P1—Ru3—C52—O9	38.5 (12)
C7—As1—C1—C2	121.3 (3)	Ru2—Ru3—C52—O9	−147.7 (12)
C13—As1—C1—C2	18.6 (3)	Ru1—Ru3—C52—O9	154.8 (12)

Hydrogen-bond geometry (Å, º) top

Cg1, Cg2 and Cg3 are the centroids of the C7–C12, C38–C43 and C14–C19 benzene rings, respectively.

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4A···O6ⁱ	0.93	2.48	3.278 (6)	144
C24—H24A···O7ⁱⁱ	0.93	2.56	3.259 (5)	132
C42—H42A···O1ⁱⁱⁱ	0.93	2.57	3.414 (5)	151
C30—H30A···Cg1ⁱⁱⁱ	0.93	3.00	3.890 (6)	161
C34—H34A···Cg2^iv	0.93	2.89	3.785 (4)	163
C40—H40A···Cg3^v	0.93	2.88	3.672 (4)	144

Symmetry codes: (i) −x, −y+2, −z+1; (ii) x+1, −y+3/2, z+1/2; (iii) −x, y−1/2, −z+3/2; (iv) −x, y+1/2, −z+3/2; (v) −x+1, y−1/2, −z+3/2.

Experimental details

Crystal data
Chemical formula	[Ru₃(C₂₅H₂₂As₂)(C₁₉H₁₇PS)(CO)₉]
M_r	1335.92
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	100
a, b, c (Å)	16.1070 (11), 16.7244 (12), 24.3147 (13)
β (°)	129.712 (3)
V (Å³)	5038.6 (6)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.32
Crystal size (mm)	0.19 × 0.07 × 0.03

Data collection
Diffractometer	Bruker APEXII DUO CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2009)
T_min, T_max	0.660, 0.927
No. of measured, independent and observed [I > 2σ(I)] reflections	41559, 14623, 11553
R_int	0.036
(sin θ/λ)_max (Å⁻¹)	0.703

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.081, 1.02
No. of reflections	14623
No. of parameters	623
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.24, −0.97

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

Hydrogen-bond geometry (Å, º) top

Cg1, Cg2 and Cg3 are the centroids of the C7–C12, C38–C43 and C14–C19 benzene rings, respectively.

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4A···O6ⁱ	0.93	2.48	3.278 (6)	144
C24—H24A···O7ⁱⁱ	0.93	2.56	3.259 (5)	132
C42—H42A···O1ⁱⁱⁱ	0.93	2.57	3.414 (5)	151
C30—H30A···Cg1ⁱⁱⁱ	0.93	3.00	3.890 (6)	161
C34—H34A···Cg2^iv	0.93	2.89	3.785 (4)	163
C40—H40A···Cg3^v	0.93	2.88	3.672 (4)	144

Symmetry codes: (i) −x, −y+2, −z+1; (ii) x+1, −y+3/2, z+1/2; (iii) −x, y−1/2, −z+3/2; (iv) −x, y+1/2, −z+3/2; (v) −x+1, y−1/2, −z+3/2.

Footnotes

‡Thomson Reuters ResearcherID: B-6034-2009. On secondment to: Multimedia University, Melaka Campus, Jalan Ayer Keroh Lama, 74750 Melaka, Malaysia.

§Thomson Reuters ResearcherID: E-2833-2010 Current address: Department of Chemistry, Gokhale Centenary College, Ankola 581 314, NK, Karnataka, India.

¶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 Universiti Sains Malaysia for a Visiting Researcher position. HKF and CSY thank USM for the Research University Grant No. 1001/PFIZIK/811160.

References

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Volume 67| Part 2| February 2011| Pages m179-m180

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