metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 2| February 2011| Pages m175-m176

[μ-Bis(di­phenyl­phosphan­yl)ethane-1:2κ2P:P′]nona­carbonyl-1κ3C,2κ3C,3κ3C-[tris­­(4-(meth­­oxy­phen­yl)arsane-3κAs]-triangulo-triruthenium(0) chloro­form monosolvate

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 5 January 2011; online 15 January 2011)

The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C21H21AsO3)(C26H24P2)(CO)9]·CHCl3, consists of one mol­ecule of the triangulo-triruthenium complex and one chloro­form solvent mol­ecule. The bis(diphenyl­phosphan­yl)ethane ligand bridges an Ru—Ru bond and the monodentate arsane ligand bonds to the third Ru atom. Both the arsane and phosphine ligands are equatorial with respect to the Ru3 triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three arsane-substituted benzene rings make dihedral angles of 52.72 (19), 63.03 (19) and 88.19 (19)° with each other. The dihedral angles between the two benzene rings are 85.8 (2) and 89.2 (2)° for the two diphenyl­phosphanyl groups. In the crystal, mol­ecules are linked together into a three-dimensional network via inter­molecular C—H⋯O hydrogen bonds. Weak inter­molecular C—H⋯π inter­actions further stabilize the crystal structure.

Related literature

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985[Bruce, M. I., Shawkataly, O. bin & Williams, M. L. (1985). J. Organomet. Chem. 287, 127-131.], 1988a[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.],b[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.])1985[Bruce, M. I., Shawkataly, O. bin & Williams, M. L. (1985). J. Organomet. Chem. 287, 127-131.],. For related structures, see: Shawkataly et al. (1998[Shawkataly, O. bin, Ramalingam, K., Lee, S. T., Parameswary, M., Fun, H.-K. & Sivakumar, K. (1998). Polyhedron, 17, 1211-1216.], 2004[Shawkataly, O. bin, Ramalingam, K., Fun, H.-K., Abdul Rahman, A., & Razak, I. A. (2004). J. Cluster Sci. 15, 387-394.], 2010a[Shawkataly, O. bin, Khan, I. A., Yeap, C. S. & Fun, H.-K. (2010a). Acta Cryst. E66, m30-m31.],b[Shawkataly, O. bin, Khan, I. A., Yeap, C. S. & Fun, H.-K. (2010b). Acta Cryst. E66, m180-m181.]). For the synthesis of Ru3(CO)10(μ-Ph2PCH2CH2PPh2), see: Bruce et al. (1983[Bruce, M. I., Matisons, J. G. & Nicholson, B. K. (1983). J. Organomet. Chem. 247, 321-343.]). For the stability of the temperature controller used in the data collection, see: Cosier & Glazer (1986[Cosier, J. & Glazer, A. M. (1986). J. Appl. Cryst. 19, 105-107.]).

[Scheme 1]

Experimental

Crystal data
  • [Ru3(C21H21AsO3)(C26H24P2)(CO)9]·CHCl3

  • Mr = 1469.36

  • Monoclinic, P 21 /c

  • a = 13.1097 (2) Å

  • b = 19.8034 (4) Å

  • c = 22.5603 (4) Å

  • β = 98.689 (1)°

  • V = 5789.81 (18) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.59 mm−1

  • T = 100 K

  • 0.58 × 0.26 × 0.04 mm

Data collection
  • Bruker SMART APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.458, Tmax = 0.946

  • 64045 measured reflections

  • 16965 independent reflections

  • 12581 reflections with I > 2σ(I)

  • Rint = 0.051

Refinement
  • R[F2 > 2σ(F2)] = 0.067

  • wR(F2) = 0.108

  • S = 1.11

  • 16965 reflections

  • 706 parameters

  • H-atom parameters constrained

  • Δρmax = 2.13 e Å−3

  • Δρmin = −1.16 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

Cg1, Cg2 and Cg3 are the centroids of the C34–C39, C7–C12 and C1–C6 benzene rings, respectively.

D—H⋯A D—H H⋯A DA D—H⋯A
C19—H19A⋯O10i 0.93 2.34 3.269 (5) 176
C43—H43A⋯O10ii 0.93 2.52 3.065 (5) 118
C47—H47C⋯O1iii 0.96 2.56 3.400 (6) 146
C13—H13ACg1iv 0.97 2.96 3.856 (4) 155
C23—H23ACg2v 0.93 2.73 3.467 (4) 137
C46—H46ACg3iii 0.93 2.83 3.623 (4) 145
Symmetry codes: (i) [x+1, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]; (ii) -x, -y, -z; (iii) x-1, y, z; (iv) x+1, y, z; (v) [x, -y-{\script{1\over 2}}, z-{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]).

Supporting information


Comment top

A large number of substituted derivatives of the type 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, 2010a,b). Herein we report the synthesis and structure of the title compound.

The asymmetric unit of the title compound consists of one molecule of the triangulo-triruthenium complex and one molecule of chloroform (Fig. 1). The bis(diphenylphosphanyl)ethane ligand bridges the Ru1–Ru2 bond and the monodentate arsane ligand bonds to the Ru3 atom. Both the arsane and phosphine ligands are equatorial with respect to the Ru3 triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three arsane-substituted benzene rings make dihedral angles (C27–C32/C33–C38, C27–C32/C39–C44 and C33–C38/C39–C44) of 52.72 (19), 63.03 (19) and 88.19 (19)° with each other respectively. The dihedral angles between the two benzene rings (C1–C6/C7–C12 and C15–C20/C21–C26) are 85.8 (2) and 89.2 (2)° for the two diphenylphosphanyl groups respectively. The three methoxyphenyl groups are planar with torsion angles C33–O10–C30–C31 = 5.6 (6)°, C40–O11–C37–C36 = -8.9 (6)° and C47–O12–C44–C45 = -6.5 (6)°.

In the crystal packing, the molecules are linked together via intermolecular C19—H19A···O10, C43—H43A···O10 and C47—H47C···O1 hydrogen bonds (Table 1) into a three-dimensional nextwork (Fig. 2). Weak intermolecular C—H···π interactions (Table 1) further stabilize the crystal structure.

Related literature top

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985, 1988a,b)1985, . For related structures, see: Shawkataly et al. (1998, 2004, 2010a,b). For the synthesis of Ru3(CO)10(µ-Ph2PCH2CH2PPh2), see: Bruce et al. (1983). 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. Tris(4-methoxyphenyl)arsane is prepared by the reaction of AsCl3 with 4-OCH3C6H4MgBr and Ru3(CO)10(µ-Ph2PCH2 CH2PPh2) was prepared by reported procedure (Bruce et al.,1983). The title compound was obtained by refluxing equimolar quantities of Ru3(CO)10(µ-Ph2PCH2CH2PPh2) and tris(4-methoxylphenyl)arsane in hexane under nitrogen atmosphere. Crystals suitable for X-ray diffraction were grown by slow solvent / solvent diffusion of CH3OH into CHCl3.

Refinement top

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 applied for the methyl groups. The maximum and minimum residual electron density peaks of 2.13 and -1.16 e Å-3 were located 0.85 Å and 1.41 Å, respectively, from the RU3 atom.

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
[Figure 1] Fig. 1. The molecular structure of the title compound with 50% probability ellipsoids for non-H atoms.
[Figure 2] Fig. 2. The crystal packing of the title compound, viewed down the c axis, showing the molecules linked into a three-dimensional network. Hydrogen atoms that are not involved in the hydrogen-bonding (dashed lines) and solvent molecules have been omitted for clarity.
[µ-Bis(diphenylphosphanyl)ethane-1:2κ2P:P']nonacarbonyl- 1κ3C,2κ3C,3κ3C-[tris(4- (methoxyphenyl)arsane-3κAs]-triangulo-triruthenium(0) chloroform monosolvate top
Crystal data top
[Ru3(C21H21AsO3)(C26H24P2)(CO)9]·CHCl3F(000) = 2920
Mr = 1469.36Dx = 1.686 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9908 reflections
a = 13.1097 (2) Åθ = 2.2–30.0°
b = 19.8034 (4) ŵ = 1.59 mm1
c = 22.5603 (4) ÅT = 100 K
β = 98.689 (1)°Plate, brown
V = 5789.81 (18) Å30.58 × 0.26 × 0.04 mm
Z = 4
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer
16965 independent reflections
Radiation source: fine-focus sealed tube12581 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
ϕ and ω scansθmax = 30.1°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2009)
h = 1814
Tmin = 0.458, Tmax = 0.946k = 2327
64045 measured reflectionsl = 3131
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.067Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.0263P)2 + 20.0015P]
where P = (Fo2 + 2Fc2)/3
16965 reflections(Δ/σ)max < 0.001
706 parametersΔρmax = 2.13 e Å3
0 restraintsΔρmin = 1.16 e Å3
Crystal data top
[Ru3(C21H21AsO3)(C26H24P2)(CO)9]·CHCl3V = 5789.81 (18) Å3
Mr = 1469.36Z = 4
Monoclinic, P21/cMo Kα radiation
a = 13.1097 (2) ŵ = 1.59 mm1
b = 19.8034 (4) ÅT = 100 K
c = 22.5603 (4) Å0.58 × 0.26 × 0.04 mm
β = 98.689 (1)°
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer
16965 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2009)
12581 reflections with I > 2σ(I)
Tmin = 0.458, Tmax = 0.946Rint = 0.051
64045 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0670 restraints
wR(F2) = 0.108H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.0263P)2 + 20.0015P]
where P = (Fo2 + 2Fc2)/3
16965 reflectionsΔρmax = 2.13 e Å3
706 parametersΔρmin = 1.16 e Å3
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
xyzUiso*/Ueq
Ru10.32826 (2)0.210241 (17)0.048812 (14)0.01175 (8)
Ru20.36871 (2)0.252908 (17)0.170465 (14)0.01048 (7)
Ru30.16553 (2)0.216924 (17)0.120575 (14)0.01162 (8)
As10.00362 (3)0.19620 (2)0.060148 (19)0.01228 (9)
P10.47394 (8)0.25345 (6)0.01451 (5)0.0132 (2)
P20.54788 (8)0.25502 (6)0.18788 (5)0.0119 (2)
O10.4486 (2)0.08901 (16)0.10796 (14)0.0228 (7)
O20.2482 (3)0.11519 (19)0.05325 (16)0.0355 (9)
O30.2033 (2)0.33319 (16)0.00532 (14)0.0207 (7)
O40.3584 (2)0.38885 (16)0.10400 (14)0.0220 (7)
O50.3269 (3)0.31436 (17)0.28767 (14)0.0257 (8)
O60.3642 (2)0.11144 (16)0.22650 (14)0.0220 (7)
O70.2049 (2)0.06503 (16)0.10891 (14)0.0227 (7)
O80.1159 (3)0.20591 (18)0.24703 (14)0.0290 (8)
O90.1242 (2)0.37007 (17)0.11541 (16)0.0258 (8)
O100.0087 (2)0.09243 (16)0.19322 (13)0.0188 (7)
O110.2495 (2)0.45858 (16)0.04417 (14)0.0216 (7)
O120.2560 (2)0.01650 (16)0.16866 (14)0.0203 (7)
C10.5493 (3)0.1957 (2)0.02549 (18)0.0161 (9)
C20.5315 (3)0.1269 (2)0.0287 (2)0.0204 (10)
H2A0.47900.10870.01020.025*
C30.5906 (4)0.0844 (3)0.0590 (2)0.0268 (11)
H3A0.57810.03810.06010.032*
C40.6673 (4)0.1106 (3)0.0874 (2)0.0267 (12)
H4A0.70650.08220.10790.032*
C50.6861 (4)0.1789 (3)0.0855 (2)0.0303 (12)
H5A0.73780.19650.10500.036*
C60.6287 (4)0.2218 (3)0.0549 (2)0.0250 (11)
H6A0.64240.26790.05380.030*
C70.4436 (3)0.3220 (2)0.03952 (18)0.0156 (9)
C80.3745 (3)0.3076 (3)0.09188 (19)0.0226 (10)
H8A0.35030.26380.09910.027*
C90.3421 (4)0.3579 (3)0.1327 (2)0.0262 (11)
H9A0.29680.34770.16730.031*
C100.3765 (4)0.4235 (3)0.1224 (2)0.0291 (12)
H10A0.35310.45740.14960.035*
C110.4460 (4)0.4384 (3)0.0714 (2)0.0250 (11)
H11A0.47060.48220.06490.030*
C120.4791 (3)0.3878 (2)0.02999 (19)0.0193 (10)
H12A0.52520.39810.00430.023*
C130.5760 (3)0.2904 (2)0.07033 (18)0.0151 (9)
H13A0.63420.30280.05060.018*
H13B0.55000.33120.08650.018*
C140.6133 (3)0.2414 (2)0.12239 (18)0.0150 (9)
H14A0.68700.24700.13430.018*
H14B0.60110.19530.10840.018*
C150.6075 (3)0.3335 (2)0.21966 (17)0.0136 (9)
C160.5496 (3)0.3908 (2)0.22665 (19)0.0197 (10)
H16A0.47830.38950.21560.024*
C170.5960 (4)0.4502 (2)0.2499 (2)0.0218 (10)
H17A0.55620.48820.25430.026*
C180.7018 (4)0.4523 (2)0.2664 (2)0.0214 (10)
H18A0.73330.49200.28180.026*
C190.7608 (3)0.3960 (2)0.26024 (19)0.0218 (10)
H19A0.83190.39770.27180.026*
C200.7143 (3)0.3364 (2)0.23677 (19)0.0197 (10)
H20A0.75450.29850.23250.024*
C210.6075 (3)0.1921 (2)0.24149 (18)0.0135 (9)
C220.5769 (3)0.1893 (2)0.29748 (19)0.0202 (10)
H22A0.52940.22060.30740.024*
C230.6159 (3)0.1407 (2)0.33913 (19)0.0212 (10)
H23A0.59390.13940.37640.025*
C240.6868 (4)0.0947 (3)0.3253 (2)0.0311 (12)
H24A0.71210.06160.35280.037*
C250.7202 (5)0.0980 (3)0.2704 (2)0.0489 (18)
H25A0.76940.06750.26110.059*
C260.6809 (4)0.1466 (3)0.2288 (2)0.0369 (14)
H26A0.70430.14850.19190.044*
C270.0055 (3)0.1639 (2)0.02139 (18)0.0132 (8)
C280.0395 (3)0.0993 (2)0.0397 (2)0.0177 (9)
H28A0.06610.07090.01290.021*
C290.0341 (3)0.0772 (2)0.0971 (2)0.0188 (9)
H29A0.05770.03430.10890.023*
C300.0063 (3)0.1187 (2)0.13713 (19)0.0157 (9)
C310.0399 (3)0.1832 (2)0.12005 (19)0.0163 (9)
H31A0.06560.21170.14710.020*
C320.0347 (3)0.2047 (2)0.06233 (19)0.0169 (9)
H32A0.05870.24760.05060.020*
C330.0562 (4)0.1309 (3)0.2346 (2)0.0265 (11)
H33A0.05560.10560.27090.040*
H33B0.12620.14080.21750.040*
H33C0.01900.17230.24330.040*
C340.0929 (3)0.2752 (2)0.05044 (18)0.0131 (8)
C350.1244 (3)0.3061 (2)0.00462 (19)0.0174 (9)
H35A0.10960.28560.03940.021*
C360.1773 (3)0.3669 (2)0.00867 (19)0.0185 (10)
H36A0.19750.38700.04590.022*
C370.1999 (3)0.3977 (2)0.04264 (19)0.0168 (9)
C380.1715 (3)0.3668 (2)0.09850 (19)0.0168 (9)
H38A0.18890.38650.13300.020*
C390.1173 (3)0.3066 (2)0.10191 (19)0.0166 (9)
H39A0.09680.28670.13910.020*
C400.2656 (4)0.4963 (2)0.0106 (2)0.0249 (11)
H40A0.29260.54010.00330.037*
H40B0.31380.47280.03970.037*
H40C0.20120.50130.02560.037*
C410.0892 (3)0.1312 (2)0.09426 (18)0.0131 (8)
C420.0492 (3)0.0949 (2)0.14551 (19)0.0177 (9)
H42A0.01810.10310.16380.021*
C430.1069 (3)0.0473 (2)0.1695 (2)0.0184 (9)
H43A0.07940.02450.20430.022*
C440.2068 (3)0.0331 (2)0.14173 (19)0.0162 (9)
C450.2488 (3)0.0692 (2)0.09152 (19)0.0186 (9)
H45A0.31610.06070.07340.022*
C460.1902 (3)0.1182 (2)0.06823 (18)0.0174 (9)
H46A0.21910.14270.03470.021*
C470.3628 (3)0.0276 (3)0.1468 (2)0.0278 (11)
H47A0.38790.06430.16830.042*
H47B0.37110.03840.10480.042*
H47C0.40120.01260.15240.042*
C480.4032 (3)0.1360 (2)0.08991 (19)0.0171 (9)
C490.2750 (3)0.1535 (2)0.0164 (2)0.0191 (10)
C500.2461 (3)0.2880 (2)0.01819 (18)0.0161 (9)
C510.3595 (3)0.3359 (2)0.12580 (19)0.0164 (9)
C520.3433 (3)0.2911 (2)0.24342 (19)0.0154 (9)
C530.3647 (3)0.1630 (2)0.20333 (18)0.0132 (9)
C540.1966 (3)0.1227 (2)0.11232 (19)0.0167 (9)
C550.1310 (3)0.2102 (2)0.1980 (2)0.0189 (9)
C560.1434 (3)0.3135 (2)0.11644 (19)0.0167 (9)
Cl10.10327 (11)0.02867 (8)0.30956 (6)0.0430 (4)
Cl20.00052 (16)0.14019 (7)0.35662 (7)0.0564 (5)
Cl30.00018 (13)0.01080 (9)0.41315 (10)0.0681 (6)
C570.0695 (4)0.0661 (3)0.3742 (2)0.0300 (12)
H57A0.13340.07790.40060.036*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.00831 (15)0.01602 (18)0.01108 (15)0.00078 (13)0.00201 (12)0.00159 (13)
Ru20.00786 (14)0.01352 (17)0.01036 (15)0.00059 (13)0.00236 (11)0.00060 (13)
Ru30.00776 (15)0.01449 (18)0.01302 (16)0.00043 (13)0.00287 (12)0.00031 (13)
As10.00888 (19)0.0150 (2)0.0132 (2)0.00037 (16)0.00234 (16)0.00067 (17)
P10.0102 (5)0.0199 (6)0.0097 (5)0.0008 (4)0.0026 (4)0.0000 (4)
P20.0093 (5)0.0161 (6)0.0102 (5)0.0001 (4)0.0016 (4)0.0008 (4)
O10.0218 (17)0.0224 (18)0.0243 (17)0.0062 (14)0.0037 (14)0.0004 (14)
O20.0264 (19)0.039 (2)0.037 (2)0.0087 (16)0.0064 (16)0.0211 (18)
O30.0186 (16)0.0217 (18)0.0212 (16)0.0022 (14)0.0011 (13)0.0018 (14)
O40.0225 (17)0.0190 (17)0.0229 (17)0.0034 (14)0.0012 (14)0.0037 (14)
O50.0300 (19)0.0285 (19)0.0201 (17)0.0002 (15)0.0087 (14)0.0084 (15)
O60.0262 (18)0.0181 (18)0.0207 (16)0.0035 (14)0.0001 (14)0.0019 (14)
O70.0188 (16)0.0182 (18)0.0310 (18)0.0009 (13)0.0035 (14)0.0014 (14)
O80.034 (2)0.035 (2)0.0195 (17)0.0052 (16)0.0118 (15)0.0001 (15)
O90.0166 (16)0.0200 (19)0.042 (2)0.0042 (14)0.0095 (15)0.0027 (16)
O100.0163 (15)0.0230 (17)0.0185 (15)0.0035 (13)0.0070 (13)0.0067 (13)
O110.0237 (17)0.0217 (18)0.0208 (16)0.0103 (14)0.0082 (13)0.0040 (14)
O120.0116 (15)0.0227 (18)0.0271 (17)0.0014 (13)0.0048 (13)0.0060 (14)
C10.011 (2)0.026 (3)0.0108 (19)0.0017 (18)0.0022 (16)0.0015 (18)
C20.010 (2)0.032 (3)0.019 (2)0.0001 (19)0.0027 (17)0.008 (2)
C30.020 (2)0.033 (3)0.026 (3)0.003 (2)0.001 (2)0.012 (2)
C40.016 (2)0.047 (3)0.018 (2)0.008 (2)0.0053 (19)0.011 (2)
C50.018 (2)0.055 (4)0.021 (2)0.005 (2)0.0088 (19)0.000 (2)
C60.023 (2)0.032 (3)0.020 (2)0.001 (2)0.0025 (19)0.000 (2)
C70.012 (2)0.027 (3)0.0095 (19)0.0023 (18)0.0073 (16)0.0045 (17)
C80.018 (2)0.036 (3)0.014 (2)0.004 (2)0.0049 (18)0.003 (2)
C90.020 (2)0.048 (3)0.012 (2)0.002 (2)0.0048 (18)0.007 (2)
C100.027 (3)0.040 (3)0.023 (2)0.017 (2)0.011 (2)0.013 (2)
C110.032 (3)0.023 (3)0.023 (2)0.006 (2)0.014 (2)0.005 (2)
C120.019 (2)0.025 (3)0.015 (2)0.0044 (19)0.0082 (18)0.0017 (19)
C130.0114 (19)0.021 (2)0.0140 (19)0.0030 (17)0.0044 (16)0.0026 (18)
C140.0113 (19)0.021 (2)0.0127 (19)0.0003 (17)0.0009 (16)0.0006 (17)
C150.014 (2)0.018 (2)0.0087 (18)0.0061 (17)0.0017 (16)0.0009 (16)
C160.018 (2)0.022 (2)0.019 (2)0.0064 (19)0.0013 (18)0.0018 (19)
C170.024 (2)0.018 (2)0.023 (2)0.0043 (19)0.0020 (19)0.0013 (19)
C180.023 (2)0.023 (3)0.019 (2)0.010 (2)0.0051 (19)0.0025 (19)
C190.012 (2)0.035 (3)0.019 (2)0.010 (2)0.0041 (18)0.002 (2)
C200.016 (2)0.026 (3)0.018 (2)0.0036 (19)0.0050 (18)0.0011 (19)
C210.014 (2)0.015 (2)0.0119 (19)0.0012 (16)0.0018 (16)0.0004 (16)
C220.015 (2)0.029 (3)0.018 (2)0.0029 (19)0.0063 (18)0.0003 (19)
C230.017 (2)0.036 (3)0.012 (2)0.001 (2)0.0052 (17)0.0026 (19)
C240.047 (3)0.028 (3)0.017 (2)0.013 (2)0.000 (2)0.004 (2)
C250.073 (4)0.055 (4)0.021 (3)0.049 (4)0.012 (3)0.004 (3)
C260.053 (4)0.047 (4)0.012 (2)0.032 (3)0.011 (2)0.003 (2)
C270.0091 (19)0.017 (2)0.0137 (19)0.0009 (16)0.0021 (15)0.0001 (17)
C280.013 (2)0.017 (2)0.025 (2)0.0036 (17)0.0081 (18)0.0014 (19)
C290.016 (2)0.015 (2)0.027 (2)0.0031 (18)0.0082 (18)0.0078 (19)
C300.0090 (19)0.021 (2)0.018 (2)0.0044 (17)0.0028 (16)0.0031 (18)
C310.012 (2)0.021 (2)0.017 (2)0.0001 (17)0.0035 (16)0.0046 (18)
C320.013 (2)0.016 (2)0.020 (2)0.0030 (17)0.0011 (17)0.0002 (18)
C330.030 (3)0.035 (3)0.016 (2)0.008 (2)0.009 (2)0.003 (2)
C340.0088 (19)0.015 (2)0.016 (2)0.0014 (16)0.0039 (15)0.0017 (17)
C350.016 (2)0.023 (2)0.014 (2)0.0028 (18)0.0043 (17)0.0040 (18)
C360.021 (2)0.020 (2)0.013 (2)0.0050 (19)0.0017 (18)0.0024 (18)
C370.014 (2)0.014 (2)0.022 (2)0.0006 (17)0.0013 (17)0.0020 (18)
C380.015 (2)0.021 (2)0.016 (2)0.0015 (18)0.0067 (17)0.0018 (18)
C390.011 (2)0.025 (2)0.014 (2)0.0022 (17)0.0038 (16)0.0034 (18)
C400.032 (3)0.024 (3)0.021 (2)0.010 (2)0.012 (2)0.007 (2)
C410.0095 (19)0.018 (2)0.014 (2)0.0001 (16)0.0084 (16)0.0024 (17)
C420.014 (2)0.020 (2)0.018 (2)0.0023 (18)0.0010 (17)0.0021 (18)
C430.017 (2)0.019 (2)0.019 (2)0.0028 (18)0.0026 (18)0.0022 (19)
C440.016 (2)0.014 (2)0.021 (2)0.0002 (17)0.0088 (17)0.0032 (18)
C450.012 (2)0.023 (2)0.021 (2)0.0016 (18)0.0022 (17)0.0000 (19)
C460.017 (2)0.023 (2)0.011 (2)0.0025 (18)0.0010 (17)0.0016 (18)
C470.014 (2)0.027 (3)0.042 (3)0.002 (2)0.006 (2)0.009 (2)
C480.013 (2)0.025 (3)0.013 (2)0.0073 (18)0.0011 (17)0.0018 (18)
C490.014 (2)0.022 (2)0.020 (2)0.0030 (18)0.0014 (18)0.0025 (19)
C500.0107 (19)0.024 (2)0.014 (2)0.0072 (18)0.0034 (16)0.0024 (19)
C510.0063 (19)0.025 (3)0.017 (2)0.0029 (17)0.0010 (16)0.0033 (19)
C520.011 (2)0.018 (2)0.018 (2)0.0008 (17)0.0053 (16)0.0014 (18)
C530.0087 (19)0.017 (2)0.014 (2)0.0003 (16)0.0028 (16)0.0058 (18)
C540.009 (2)0.023 (3)0.017 (2)0.0014 (17)0.0006 (16)0.0041 (18)
C550.014 (2)0.017 (2)0.027 (2)0.0002 (18)0.0047 (18)0.003 (2)
C560.0084 (19)0.024 (3)0.019 (2)0.0026 (17)0.0041 (16)0.0015 (19)
Cl10.0401 (8)0.0504 (9)0.0371 (7)0.0130 (7)0.0012 (6)0.0164 (7)
Cl20.1012 (14)0.0258 (8)0.0519 (9)0.0151 (8)0.0433 (10)0.0064 (7)
Cl30.0499 (10)0.0429 (10)0.1242 (17)0.0157 (8)0.0542 (11)0.0373 (10)
C570.027 (3)0.035 (3)0.030 (3)0.009 (2)0.012 (2)0.005 (2)
Geometric parameters (Å, º) top
Ru1—C491.899 (4)C15—C161.387 (6)
Ru1—C481.926 (5)C15—C201.396 (6)
Ru1—C501.945 (5)C16—C171.390 (6)
Ru1—P12.3291 (11)C16—H16A0.9300
Ru1—Ru22.8439 (4)C17—C181.381 (6)
Ru1—Ru32.8694 (5)C17—H17A0.9300
Ru2—C521.886 (4)C18—C191.376 (7)
Ru2—C511.922 (5)C18—H18A0.9300
Ru2—C531.932 (4)C19—C201.396 (6)
Ru2—P22.3225 (11)C19—H19A0.9300
Ru2—Ru32.8221 (4)C20—H20A0.9300
Ru3—C551.875 (5)C21—C261.380 (6)
Ru3—C541.924 (5)C21—C221.383 (6)
Ru3—C561.935 (5)C22—C231.387 (6)
Ru3—As12.4558 (5)C22—H22A0.9300
As1—C411.942 (4)C23—C241.371 (7)
As1—C271.944 (4)C23—H23A0.9300
As1—C341.946 (4)C24—C251.377 (7)
P1—C71.827 (4)C24—H24A0.9300
P1—C11.836 (5)C25—C261.387 (7)
P1—C131.845 (4)C25—H25A0.9300
P2—C211.828 (4)C26—H26A0.9300
P2—C141.837 (4)C27—C321.390 (6)
P2—C151.837 (4)C27—C281.397 (6)
O1—C481.146 (5)C28—C291.378 (6)
O2—C491.141 (5)C28—H28A0.9300
O3—C501.144 (5)C29—C301.384 (6)
O4—C511.157 (5)C29—H29A0.9300
O5—C521.149 (5)C30—C311.388 (6)
O6—C531.148 (5)C31—C321.381 (6)
O7—C541.152 (5)C31—H31A0.9300
O8—C551.155 (5)C32—H32A0.9300
O9—C561.147 (5)C33—H33A0.9600
O10—C301.373 (5)C33—H33B0.9600
O10—C331.419 (5)C33—H33C0.9600
O11—C371.372 (5)C34—C351.391 (6)
O11—C401.432 (5)C34—C391.397 (6)
O12—C441.367 (5)C35—C361.386 (6)
O12—C471.430 (5)C35—H35A0.9300
C1—C21.382 (6)C36—C371.380 (6)
C1—C61.415 (6)C36—H36A0.9300
C2—C31.393 (6)C37—C381.400 (6)
C2—H2A0.9300C38—C391.384 (6)
C3—C41.373 (7)C38—H38A0.9300
C3—H3A0.9300C39—H39A0.9300
C4—C51.375 (8)C40—H40A0.9600
C4—H4A0.9300C40—H40B0.9600
C5—C61.386 (7)C40—H40C0.9600
C5—H5A0.9300C41—C461.389 (6)
C6—H6A0.9300C41—C421.395 (6)
C7—C121.389 (6)C42—C431.370 (6)
C7—C81.405 (6)C42—H42A0.9300
C8—C91.378 (7)C43—C441.393 (6)
C8—H8A0.9300C43—H43A0.9300
C9—C101.382 (7)C44—C451.381 (6)
C9—H9A0.9300C45—C461.389 (6)
C10—C111.387 (7)C45—H45A0.9300
C10—H10A0.9300C46—H46A0.9300
C11—C121.394 (6)C47—H47A0.9600
C11—H11A0.9300C47—H47B0.9600
C12—H12A0.9300C47—H47C0.9600
C13—C141.545 (6)Cl1—C571.751 (5)
C13—H13A0.9700Cl2—C571.737 (6)
C13—H13B0.9700Cl3—C571.746 (5)
C14—H14A0.9700C57—H57A0.9800
C14—H14B0.9700
C49—Ru1—C4891.33 (18)C17—C16—H16A119.4
C49—Ru1—C5094.22 (18)C18—C17—C16119.5 (5)
C48—Ru1—C50171.82 (18)C18—C17—H17A120.2
C49—Ru1—P1100.57 (14)C16—C17—H17A120.2
C48—Ru1—P193.20 (13)C19—C18—C17120.3 (4)
C50—Ru1—P191.67 (13)C19—C18—H18A119.9
C49—Ru1—Ru2156.51 (14)C17—C18—H18A119.9
C48—Ru1—Ru275.81 (13)C18—C19—C20120.2 (4)
C50—Ru1—Ru296.90 (12)C18—C19—H19A119.9
P1—Ru1—Ru299.71 (3)C20—C19—H19A119.9
C49—Ru1—Ru3104.31 (14)C19—C20—C15120.1 (4)
C48—Ru1—Ru397.61 (13)C19—C20—H20A119.9
C50—Ru1—Ru375.21 (12)C15—C20—H20A119.9
P1—Ru1—Ru3152.54 (3)C26—C21—C22118.1 (4)
Ru2—Ru1—Ru359.199 (11)C26—C21—P2123.4 (3)
C52—Ru2—C5196.26 (18)C22—C21—P2118.5 (3)
C52—Ru2—C5390.92 (18)C21—C22—C23121.2 (4)
C51—Ru2—C53170.33 (17)C21—C22—H22A119.4
C52—Ru2—P298.79 (13)C23—C22—H22A119.4
C51—Ru2—P293.15 (12)C24—C23—C22120.0 (4)
C53—Ru2—P292.13 (12)C24—C23—H23A120.0
C52—Ru2—Ru399.71 (12)C22—C23—H23A120.0
C51—Ru2—Ru391.50 (12)C23—C24—C25119.5 (5)
C53—Ru2—Ru380.89 (11)C23—C24—H24A120.3
P2—Ru2—Ru3160.31 (3)C25—C24—H24A120.3
C52—Ru2—Ru1158.34 (12)C24—C25—C26120.4 (5)
C51—Ru2—Ru176.13 (13)C24—C25—H25A119.8
C53—Ru2—Ru194.86 (12)C26—C25—H25A119.8
P2—Ru2—Ru1101.83 (3)C21—C26—C25120.8 (5)
Ru3—Ru2—Ru160.850 (11)C21—C26—H26A119.6
C55—Ru3—C5496.09 (19)C25—C26—H26A119.6
C55—Ru3—C5693.41 (19)C32—C27—C28118.2 (4)
C54—Ru3—C56170.41 (19)C32—C27—As1119.1 (3)
C55—Ru3—As1100.39 (13)C28—C27—As1122.6 (3)
C54—Ru3—As188.34 (12)C29—C28—C27120.5 (4)
C56—Ru3—As191.27 (12)C29—C28—H28A119.7
C55—Ru3—Ru289.58 (13)C27—C28—H28A119.7
C54—Ru3—Ru294.72 (12)C28—C29—C30120.3 (4)
C56—Ru3—Ru283.98 (12)C28—C29—H29A119.9
As1—Ru3—Ru2169.216 (19)C30—C29—H29A119.9
C55—Ru3—Ru1145.84 (13)O10—C30—C29116.2 (4)
C54—Ru3—Ru173.39 (13)O10—C30—C31123.6 (4)
C56—Ru3—Ru197.89 (13)C29—C30—C31120.1 (4)
As1—Ru3—Ru1111.410 (17)C32—C31—C30119.1 (4)
Ru2—Ru3—Ru159.951 (11)C32—C31—H31A120.4
C41—As1—C27103.39 (17)C30—C31—H31A120.4
C41—As1—C34101.75 (17)C31—C32—C27121.7 (4)
C27—As1—C34103.68 (17)C31—C32—H32A119.2
C41—As1—Ru3114.73 (12)C27—C32—H32A119.2
C27—As1—Ru3117.48 (12)O10—C33—H33A109.5
C34—As1—Ru3113.92 (12)O10—C33—H33B109.5
C7—P1—C1102.4 (2)H33A—C33—H33B109.5
C7—P1—C13102.9 (2)O10—C33—H33C109.5
C1—P1—C13101.18 (19)H33A—C33—H33C109.5
C7—P1—Ru1112.81 (14)H33B—C33—H33C109.5
C1—P1—Ru1117.63 (15)C35—C34—C39118.2 (4)
C13—P1—Ru1117.75 (14)C35—C34—As1123.1 (3)
C21—P2—C14103.13 (19)C39—C34—As1118.3 (3)
C21—P2—C15101.82 (18)C36—C35—C34121.3 (4)
C14—P2—C15102.47 (19)C36—C35—H35A119.3
C21—P2—Ru2114.83 (14)C34—C35—H35A119.3
C14—P2—Ru2116.38 (13)C37—C36—C35119.8 (4)
C15—P2—Ru2116.16 (14)C37—C36—H36A120.1
C30—O10—C33118.5 (3)C35—C36—H36A120.1
C37—O11—C40116.4 (3)O11—C37—C36124.9 (4)
C44—O12—C47117.4 (3)O11—C37—C38115.1 (4)
C2—C1—C6117.8 (4)C36—C37—C38120.0 (4)
C2—C1—P1122.7 (3)C39—C38—C37119.4 (4)
C6—C1—P1119.5 (4)C39—C38—H38A120.3
C1—C2—C3121.2 (4)C37—C38—H38A120.3
C1—C2—H2A119.4C38—C39—C34121.2 (4)
C3—C2—H2A119.4C38—C39—H39A119.4
C4—C3—C2120.2 (5)C34—C39—H39A119.4
C4—C3—H3A119.9O11—C40—H40A109.5
C2—C3—H3A119.9O11—C40—H40B109.5
C3—C4—C5119.9 (5)H40A—C40—H40B109.5
C3—C4—H4A120.1O11—C40—H40C109.5
C5—C4—H4A120.1H40A—C40—H40C109.5
C4—C5—C6120.7 (5)H40B—C40—H40C109.5
C4—C5—H5A119.7C46—C41—C42118.0 (4)
C6—C5—H5A119.7C46—C41—As1121.8 (3)
C5—C6—C1120.2 (5)C42—C41—As1120.2 (3)
C5—C6—H6A119.9C43—C42—C41121.4 (4)
C1—C6—H6A119.9C43—C42—H42A119.3
C12—C7—C8118.6 (4)C41—C42—H42A119.3
C12—C7—P1124.0 (3)C42—C43—C44119.9 (4)
C8—C7—P1117.3 (4)C42—C43—H43A120.0
C9—C8—C7120.6 (5)C44—C43—H43A120.0
C9—C8—H8A119.7O12—C44—C45125.5 (4)
C7—C8—H8A119.7O12—C44—C43114.8 (4)
C8—C9—C10120.5 (4)C45—C44—C43119.7 (4)
C8—C9—H9A119.8C44—C45—C46119.8 (4)
C10—C9—H9A119.8C44—C45—H45A120.1
C9—C10—C11119.7 (4)C46—C45—H45A120.1
C9—C10—H10A120.2C45—C46—C41121.0 (4)
C11—C10—H10A120.2C45—C46—H46A119.5
C10—C11—C12120.1 (5)C41—C46—H46A119.5
C10—C11—H11A119.9O12—C47—H47A109.5
C12—C11—H11A119.9O12—C47—H47B109.5
C7—C12—C11120.5 (4)H47A—C47—H47B109.5
C7—C12—H12A119.8O12—C47—H47C109.5
C11—C12—H12A119.8H47A—C47—H47C109.5
C14—C13—P1112.5 (3)H47B—C47—H47C109.5
C14—C13—H13A109.1O1—C48—Ru1172.1 (4)
P1—C13—H13A109.1O2—C49—Ru1174.1 (4)
C14—C13—H13B109.1O3—C50—Ru1172.3 (4)
P1—C13—H13B109.1O4—C51—Ru2173.3 (4)
H13A—C13—H13B107.8O5—C52—Ru2179.4 (4)
C13—C14—P2112.8 (3)O6—C53—Ru2175.5 (4)
C13—C14—H14A109.0O7—C54—Ru3172.7 (4)
P2—C14—H14A109.0O8—C55—Ru3175.9 (4)
C13—C14—H14B109.0O9—C56—Ru3175.4 (4)
P2—C14—H14B109.0Cl2—C57—Cl3110.5 (3)
H14A—C14—H14B107.8Cl2—C57—Cl1110.9 (3)
C16—C15—C20118.6 (4)Cl3—C57—Cl1111.8 (3)
C16—C15—P2121.9 (3)Cl2—C57—H57A107.8
C20—C15—P2119.5 (3)Cl3—C57—H57A107.8
C15—C16—C17121.2 (4)Cl1—C57—H57A107.8
C15—C16—H16A119.4
C49—Ru1—Ru2—C5277.7 (5)C7—P1—C1—C2133.3 (4)
C48—Ru1—Ru2—C52136.2 (4)C13—P1—C1—C2120.7 (4)
C50—Ru1—Ru2—C5240.0 (4)Ru1—P1—C1—C29.1 (4)
P1—Ru1—Ru2—C52132.9 (4)C7—P1—C1—C646.2 (4)
Ru3—Ru1—Ru2—C5228.2 (4)C13—P1—C1—C659.8 (4)
C49—Ru1—Ru2—C51149.2 (4)Ru1—P1—C1—C6170.4 (3)
C48—Ru1—Ru2—C51152.25 (18)C6—C1—C2—C31.0 (6)
C50—Ru1—Ru2—C5131.51 (17)P1—C1—C2—C3179.5 (3)
P1—Ru1—Ru2—C5161.39 (13)C1—C2—C3—C41.1 (7)
Ru3—Ru1—Ru2—C5199.70 (12)C2—C3—C4—C50.4 (7)
C49—Ru1—Ru2—C5327.2 (3)C3—C4—C5—C60.4 (7)
C48—Ru1—Ru2—C5331.31 (18)C4—C5—C6—C10.4 (7)
C50—Ru1—Ru2—C53144.93 (17)C2—C1—C6—C50.2 (6)
P1—Ru1—Ru2—C53122.17 (12)P1—C1—C6—C5179.8 (3)
Ru3—Ru1—Ru2—C5376.74 (12)C1—P1—C7—C12115.5 (4)
C49—Ru1—Ru2—P2120.5 (3)C13—P1—C7—C1210.8 (4)
C48—Ru1—Ru2—P261.90 (13)Ru1—P1—C7—C12117.1 (4)
C50—Ru1—Ru2—P2121.86 (12)C1—P1—C7—C869.0 (4)
P1—Ru1—Ru2—P228.97 (4)C13—P1—C7—C8173.7 (3)
Ru3—Ru1—Ru2—P2169.94 (3)Ru1—P1—C7—C858.3 (4)
C49—Ru1—Ru2—Ru349.5 (3)C12—C7—C8—C90.4 (7)
C48—Ru1—Ru2—Ru3108.05 (13)P1—C7—C8—C9175.3 (4)
C50—Ru1—Ru2—Ru368.19 (12)C7—C8—C9—C100.5 (7)
P1—Ru1—Ru2—Ru3161.09 (3)C8—C9—C10—C111.5 (7)
C52—Ru2—Ru3—C5526.39 (19)C9—C10—C11—C121.5 (7)
C51—Ru2—Ru3—C55123.00 (19)C8—C7—C12—C110.4 (6)
C53—Ru2—Ru3—C5562.98 (18)P1—C7—C12—C11175.0 (3)
P2—Ru2—Ru3—C55133.32 (16)C10—C11—C12—C70.6 (7)
Ru1—Ru2—Ru3—C55163.80 (14)C7—P1—C13—C14178.7 (3)
C52—Ru2—Ru3—C54122.47 (19)C1—P1—C13—C1475.7 (3)
C51—Ru2—Ru3—C54140.92 (19)Ru1—P1—C13—C1454.0 (3)
C53—Ru2—Ru3—C5433.09 (18)P1—C13—C14—P295.4 (3)
P2—Ru2—Ru3—C5437.25 (16)C21—P2—C14—C13179.3 (3)
Ru1—Ru2—Ru3—C5467.73 (13)C15—P2—C14—C1373.8 (3)
C52—Ru2—Ru3—C5667.08 (18)Ru2—P2—C14—C1354.1 (3)
C51—Ru2—Ru3—C5629.53 (18)C21—P2—C15—C16132.4 (4)
C53—Ru2—Ru3—C56156.45 (18)C14—P2—C15—C16121.1 (4)
P2—Ru2—Ru3—C56133.21 (16)Ru2—P2—C15—C166.9 (4)
Ru1—Ru2—Ru3—C56102.73 (13)C21—P2—C15—C2048.3 (4)
C52—Ru2—Ru3—As1131.37 (17)C14—P2—C15—C2058.2 (4)
C51—Ru2—Ru3—As134.76 (17)Ru2—P2—C15—C20173.8 (3)
C53—Ru2—Ru3—As1139.26 (16)C20—C15—C16—C170.3 (6)
P2—Ru2—Ru3—As168.92 (15)P2—C15—C16—C17179.0 (3)
Ru1—Ru2—Ru3—As138.44 (10)C15—C16—C17—C180.0 (7)
C52—Ru2—Ru3—Ru1169.81 (13)C16—C17—C18—C190.4 (7)
C51—Ru2—Ru3—Ru173.20 (13)C17—C18—C19—C200.6 (7)
C53—Ru2—Ru3—Ru1100.82 (12)C18—C19—C20—C150.3 (7)
P2—Ru2—Ru3—Ru130.47 (9)C16—C15—C20—C190.1 (6)
C49—Ru1—Ru3—C55132.0 (3)P2—C15—C20—C19179.1 (3)
C48—Ru1—Ru3—C5538.6 (3)C14—P2—C21—C262.0 (5)
C50—Ru1—Ru3—C55137.4 (3)C15—P2—C21—C26108.0 (4)
P1—Ru1—Ru3—C5573.6 (3)Ru2—P2—C21—C26125.6 (4)
Ru2—Ru1—Ru3—C5529.8 (2)C14—P2—C21—C22178.7 (3)
C49—Ru1—Ru3—C5456.01 (18)C15—P2—C21—C2272.7 (4)
C48—Ru1—Ru3—C5437.34 (17)Ru2—P2—C21—C2253.7 (4)
C50—Ru1—Ru3—C54146.65 (17)C26—C21—C22—C232.3 (7)
P1—Ru1—Ru3—C54149.61 (14)P2—C21—C22—C23177.1 (3)
Ru2—Ru1—Ru3—C54105.77 (12)C21—C22—C23—C240.6 (7)
C49—Ru1—Ru3—C56119.90 (18)C22—C23—C24—C251.2 (8)
C48—Ru1—Ru3—C56146.75 (17)C23—C24—C25—C261.4 (10)
C50—Ru1—Ru3—C5629.26 (17)C22—C21—C26—C252.1 (8)
P1—Ru1—Ru3—C5634.48 (14)P2—C21—C26—C25177.2 (5)
Ru2—Ru1—Ru3—C5678.32 (12)C24—C25—C26—C210.4 (10)
C49—Ru1—Ru3—As125.40 (14)C41—As1—C27—C32169.6 (3)
C48—Ru1—Ru3—As1118.75 (12)C34—As1—C27—C3263.8 (3)
C50—Ru1—Ru3—As165.24 (12)Ru3—As1—C27—C3262.9 (3)
P1—Ru1—Ru3—As1128.98 (6)C41—As1—C27—C2814.7 (4)
Ru2—Ru1—Ru3—As1172.82 (2)C34—As1—C27—C28120.5 (3)
C49—Ru1—Ru3—Ru2161.77 (14)Ru3—As1—C27—C28112.8 (3)
C48—Ru1—Ru3—Ru268.43 (12)C32—C27—C28—C290.7 (6)
C50—Ru1—Ru3—Ru2107.58 (12)As1—C27—C28—C29176.4 (3)
P1—Ru1—Ru3—Ru243.85 (6)C27—C28—C29—C300.7 (6)
C55—Ru3—As1—C4135.50 (19)C33—O10—C30—C29175.5 (4)
C54—Ru3—As1—C4160.39 (19)C33—O10—C30—C315.6 (6)
C56—Ru3—As1—C41129.19 (19)C28—C29—C30—O10179.9 (4)
Ru2—Ru3—As1—C41167.14 (16)C28—C29—C30—C311.2 (6)
Ru1—Ru3—As1—C41131.82 (13)O10—C30—C31—C32179.6 (4)
C55—Ru3—As1—C27157.3 (2)C29—C30—C31—C321.5 (6)
C54—Ru3—As1—C2761.41 (19)C30—C31—C32—C271.5 (6)
C56—Ru3—As1—C27109.00 (19)C28—C27—C32—C311.0 (6)
Ru2—Ru3—As1—C2745.33 (18)As1—C27—C32—C31176.9 (3)
Ru1—Ru3—As1—C2710.02 (14)C41—As1—C34—C35121.1 (4)
C55—Ru3—As1—C3481.22 (19)C27—As1—C34—C3514.0 (4)
C54—Ru3—As1—C34177.11 (19)Ru3—As1—C34—C35114.8 (3)
C56—Ru3—As1—C3412.48 (19)C41—As1—C34—C3966.1 (3)
Ru2—Ru3—As1—C3476.15 (17)C27—As1—C34—C39173.2 (3)
Ru1—Ru3—As1—C34111.46 (14)Ru3—As1—C34—C3958.0 (3)
C49—Ru1—P1—C779.4 (2)C39—C34—C35—C360.9 (6)
C48—Ru1—P1—C7171.4 (2)As1—C34—C35—C36171.9 (3)
C50—Ru1—P1—C715.2 (2)C34—C35—C36—C370.2 (7)
Ru2—Ru1—P1—C7112.51 (16)C40—O11—C37—C368.9 (6)
Ru3—Ru1—P1—C775.37 (17)C40—O11—C37—C38170.9 (4)
C49—Ru1—P1—C139.4 (2)C35—C36—C37—O11178.3 (4)
C48—Ru1—P1—C152.53 (19)C35—C36—C37—C381.5 (7)
C50—Ru1—P1—C1134.04 (19)O11—C37—C38—C39177.3 (4)
Ru2—Ru1—P1—C1128.67 (15)C36—C37—C38—C392.4 (6)
Ru3—Ru1—P1—C1165.80 (14)C37—C38—C39—C341.8 (6)
C49—Ru1—P1—C13160.9 (2)C35—C34—C39—C380.1 (6)
C48—Ru1—P1—C1369.0 (2)As1—C34—C39—C38173.3 (3)
C50—Ru1—P1—C13104.4 (2)C27—As1—C41—C4656.4 (4)
Ru2—Ru1—P1—C137.16 (17)C34—As1—C41—C4650.9 (4)
Ru3—Ru1—P1—C1344.29 (19)Ru3—As1—C41—C46174.4 (3)
C52—Ru2—P2—C2173.6 (2)C27—As1—C41—C42122.2 (4)
C51—Ru2—P2—C21170.4 (2)C34—As1—C41—C42130.5 (3)
C53—Ru2—P2—C2117.69 (19)Ru3—As1—C41—C427.0 (4)
Ru3—Ru2—P2—C2186.20 (18)C46—C41—C42—C430.5 (7)
Ru1—Ru2—P2—C21113.11 (15)As1—C41—C42—C43178.1 (3)
C52—Ru2—P2—C14165.8 (2)C41—C42—C43—C441.7 (7)
C51—Ru2—P2—C1469.0 (2)C47—O12—C44—C456.5 (6)
C53—Ru2—P2—C14102.9 (2)C47—O12—C44—C43172.5 (4)
Ru3—Ru2—P2—C1434.4 (2)C42—C43—C44—O12178.2 (4)
Ru1—Ru2—P2—C147.48 (16)C42—C43—C44—C452.7 (7)
C52—Ru2—P2—C1545.0 (2)O12—C44—C45—C46179.5 (4)
C51—Ru2—P2—C1551.8 (2)C43—C44—C45—C461.5 (7)
C53—Ru2—P2—C15136.30 (19)C44—C45—C46—C410.7 (7)
Ru3—Ru2—P2—C15155.19 (15)C42—C41—C46—C451.7 (6)
Ru1—Ru2—P2—C15128.28 (15)As1—C41—C46—C45176.8 (3)
Hydrogen-bond geometry (Å, º) top
Cg1, Cg2 and Cg3 are the centroids of the C34–C39, C7–C12 and C1–C6 benzene rings, respectively.
D—H···AD—HH···AD···AD—H···A
C19—H19A···O10i0.932.343.269 (5)176
C43—H43A···O10ii0.932.523.065 (5)118
C47—H47C···O1iii0.962.563.400 (6)146
C13—H13A···Cg1iv0.972.963.856 (4)155
C23—H23A···Cg2v0.932.733.467 (4)137
C46—H46A···Cg3iii0.932.833.623 (4)145
Symmetry codes: (i) x+1, y+1/2, z+1/2; (ii) x, y, z; (iii) x1, y, z; (iv) x+1, y, z; (v) x, y1/2, z1/2.

Experimental details

Crystal data
Chemical formula[Ru3(C21H21AsO3)(C26H24P2)(CO)9]·CHCl3
Mr1469.36
Crystal system, space groupMonoclinic, P21/c
Temperature (K)100
a, b, c (Å)13.1097 (2), 19.8034 (4), 22.5603 (4)
β (°) 98.689 (1)
V3)5789.81 (18)
Z4
Radiation typeMo Kα
µ (mm1)1.59
Crystal size (mm)0.58 × 0.26 × 0.04
Data collection
DiffractometerBruker SMART APEXII CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2009)
Tmin, Tmax0.458, 0.946
No. of measured, independent and
observed [I > 2σ(I)] reflections
64045, 16965, 12581
Rint0.051
(sin θ/λ)max1)0.706
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.067, 0.108, 1.11
No. of reflections16965
No. of parameters706
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0263P)2 + 20.0015P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)2.13, 1.16

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 C34–C39, C7–C12 and C1–C6 benzene rings, respectively.
D—H···AD—HH···AD···AD—H···A
C19—H19A···O10i0.932.343.269 (5)176
C43—H43A···O10ii0.932.523.065 (5)118
C47—H47C···O1iii0.962.563.400 (6)146
C13—H13A···Cg1iv0.972.963.856 (4)155
C23—H23A···Cg2v0.932.733.467 (4)137
C46—H46A···Cg3iii0.932.833.623 (4)145
Symmetry codes: (i) x+1, y+1/2, z+1/2; (ii) x, y, z; (iii) x1, y, z; (iv) x+1, y, z; (v) x, y1/2, z1/2.
 

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 USM for a Visiting Researcher position. SSS thanks USM for the G A 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 m175-m176
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