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Acta Cryst. (2009). E65, m1628-m1629    [ doi:10.1107/S1600536809047783 ]

[mu]-Bis(diphenylarsino)methane-1:2[kappa]2As:As-nonacarbonyl-1[kappa]3C,2[kappa]3C,3[kappa]3C-[(2-methoxyphenyl)diphenylphosphino-3[kappa]P]-triangulo-triruthenium(0)

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

Abstract top

In the title triangulo-triruthenium compound, [Ru3(C25H22As2)(C19H17OP)(CO)9], the bis(diphenylarsino)methane ligand bridges a Ru-Ru bond and the monodentate phosphine ligand bonds to the third Ru atom. Both the phosphine and arsine ligands are equatorial with respect to the Ru3 triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three phosphine substituted phenyl rings make dihedral angles of 74.34 (12), 68.34 (12) and 85.45 (11)° with each other. The dihedral angles between the two phenyl rings are 87.56 (11) and 60.56 (11)° for the two diphenylarsino groups. In the crystal packing, the molecules are linked together into chains via intermolecular C-H...O hydrogen bonds down the a axis. Weak intermolecular C-H...[pi] interactions further stabilize the crystal structure.

Comment top

Tri-angulotriruthenium clusters are known for their interesting structural variations and related catalytic activity. A large number of substituted derivatives, Ru3(CO)12-nLn (L = group 15 ligand) have been reported (Bruce et al., 1985 1988a,b;). As part of our study on the substitution of transition metal-carbonyl clusters with mixed-ligand complexes, we have published several structures of tri-angulotriruthenium-carbonyl clusters containing mixed P/As and P/Sb ligands (Shawkataly et al., 1998, 2004, 2009a,b). Herein we report the synthesis and structure of Ru3(C19H17OP)(C25H22As2)(CO)9.

The bond lengths and angles of title compound (Fig. 1) are comparable to those in related structures (Shawkataly et al., 2009a,b). The bis(diphenylarsino)methane ligand bridges the Ru1—Ru2 bond and the monodentate phosphine ligand bonds to the Ru3 atom. Both the phosphine and arsine ligands are equatorial with respect to the Ru3 triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three phosphine substituted phenyl rings make dihedral angles (C26–C31/C32–C37, C26–C31/C38–C43 and C32–C37/C38–C43) of 74.34 (12), 68.34 (12) and 85.45 (11)° with each other respectively. The dihedral angles between the two phenyl rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 87.56 (11) and 60.56 (11)° for the two diphenylarsino groups respectively.

In the crystal packing (Fig. 2), the molecules are linked together into chains via intermolecular C16—H16A···O4 and C29—H29A···O5 hydrogen bonds down a axis. Weak intermolecular C—H···π interaction further stabilize the crystal structure (Table 1).

Related literature top

For general background to tri-angulotriruthenium derivatives, see: Bruce et al. (1985, 1988a,b); Shawkataly et al. (1998, 2004, 2009a,b). For related structures, see: Shawkataly et al. (2009a,b). For the synthesis of bis(diphenylphosphino)methane, see: Bruce et al. (1983). For the stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986). Cg1, Cg2 and Cg3 are the centroids of the C7–C12, C1–C6 and C14–C19 rings, respectively.

Experimental top

The reactions were conducted under an atmosphere of nitrogen using standard Schlenk techniques and hexane-dried over sodium metal. (2-Methoxyphenyl)diphenylphosphine (Strem Chemicals) was used as received and bis(diphenylarsino)methane (Bruce et al., 1983) was prepared by the reported procedure. The title compound was obtained by refluxing equimolar quantities of Ru3(CO)10(µ-Ph2AsCH2AsPh2) (105.5 mg, 0.1 mmol) and (2-methoxyphenyl)diphenylphosphine (29.23 mg, 0.1 mmol) in hexane under a nitrogen atmosphere. Crystals suitable for X-ray diffraction were grown by slow solvent / solvent diffusion of CH3OH into 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 used for the methyl groups.

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
[Figure 1] Fig. 1. The molecular structure of the title compound with 30% probability ellipsoids for non-H atoms.
[Figure 2] Fig. 2. The crystal packing of the title compound, viewed down the a axis, showing the molecules linked down a axis. Hydrogen atoms that not involved in the hydrogen-bonding (dashed lines) have been omitted for clarity.
µ-Bis(diphenylarsino)methane-1:2κ2As:As-nonacarbonyl- 1κ3C,2κ3C,3κ3C-[(2- methoxyphenyl)diphenylphosphino-3κP]-triangulo-triruthenium(0) top
Crystal data top
[Ru3(C25H22As2)(C19H17OP)(CO)9]Z = 2
Mr = 1319.86F(000) = 1300
Triclinic, P1Dx = 1.782 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.4414 (1) ÅCell parameters from 9969 reflections
b = 11.6541 (1) Åθ = 2.3–32.5°
c = 21.7581 (3) ŵ = 2.34 mm−1
α = 84.220 (1)°T = 100 K
β = 84.910 (1)°Block, purple
γ = 69.324 (1)°0.22 × 0.15 × 0.08 mm
V = 2460.49 (5) Å3
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		14256 independent reflections
Radiation source: fine-focus sealed tube11583 reflections with I > 2σ(I)
graphiteRint = 0.042
φ and ω scansθmax = 30.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2005)		h = −14→14
Tmin = 0.624, Tmax = 0.830k = −16→16
66801 measured reflectionsl = −30→30
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)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.059H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0249P)2 + 1.1204P]
where P = (Fo2 + 2Fc2)/3
14256 reflections(Δ/σ)max = 0.001
623 parametersΔρmax = 0.67 e Å−3
0 restraintsΔρmin = −0.80 e Å−3
Crystal data top
[Ru3(C25H22As2)(C19H17OP)(CO)9]γ = 69.324 (1)°
Mr = 1319.86V = 2460.49 (5) Å3
Triclinic, P1Z = 2
a = 10.4414 (1) ÅMo Kα radiation
b = 11.6541 (1) ŵ = 2.34 mm−1
c = 21.7581 (3) ÅT = 100 K
α = 84.220 (1)°0.22 × 0.15 × 0.08 mm
β = 84.910 (1)°
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		14256 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2005)		11583 reflections with I > 2σ(I)
Tmin = 0.624, Tmax = 0.830Rint = 0.042
66801 measured reflectionsθmax = 30.0°
Refinement top
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.059Δρmax = 0.67 e Å−3
S = 1.02Δρmin = −0.80 e Å−3
14256 reflectionsAbsolute structure: ?
623 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Special details top

Experimental. The crystal was placed in the cold stream of an Oxford Cyrosystems 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
Ru10.304381 (17)0.169488 (15)0.205414 (8)0.01208 (4)
Ru20.134145 (17)0.409411 (15)0.239146 (8)0.01210 (4)
Ru30.366826 (17)0.266015 (15)0.309439 (8)0.01236 (4)
As10.14602 (2)0.160785 (19)0.131363 (10)0.01190 (5)
As20.03462 (2)0.457750 (19)0.139265 (10)0.01170 (5)
P10.42521 (6)0.35723 (5)0.38908 (3)0.01382 (11)
O10.17427 (18)0.03586 (15)0.30752 (7)0.0228 (4)
O20.55893 (18)−0.06037 (15)0.20185 (8)0.0273 (4)
O30.45546 (17)0.30219 (15)0.11329 (8)0.0234 (4)
O40.33593 (17)0.53968 (15)0.19120 (8)0.0236 (4)
O5−0.0492 (2)0.64365 (15)0.29555 (8)0.0298 (4)
O6−0.07509 (17)0.28542 (16)0.28668 (8)0.0242 (4)
O70.11632 (17)0.25538 (16)0.39212 (7)0.0223 (4)
O80.53996 (19)0.00676 (15)0.35308 (8)0.0291 (4)
O90.59248 (17)0.33052 (15)0.22840 (8)0.0228 (4)
O100.35430 (18)0.17638 (16)0.47263 (8)0.0246 (4)
C10.2071 (2)0.07700 (19)0.05505 (10)0.0134 (4)
C20.3397 (2)−0.0067 (2)0.04739 (10)0.0164 (4)
H2A0.4021−0.01860.07750.020*
C30.3793 (2)−0.0725 (2)−0.00503 (10)0.0182 (4)
H3A0.4676−0.1293−0.00970.022*
C40.2873 (2)−0.0534 (2)−0.05045 (10)0.0182 (5)
H4A0.3145−0.0966−0.08580.022*
C50.1552 (2)0.0296 (2)−0.04332 (10)0.0180 (4)
H5A0.09380.0426−0.07390.022*
C60.1146 (2)0.0933 (2)0.00947 (10)0.0167 (4)
H6A0.02500.14730.01470.020*
C70.0285 (2)0.0696 (2)0.16641 (10)0.0149 (4)
C80.0956 (2)−0.0566 (2)0.18016 (10)0.0175 (4)
H8A0.1891−0.09180.17030.021*
C90.0238 (2)−0.1294 (2)0.20841 (10)0.0201 (5)
H9A0.0692−0.21300.21750.024*
C10−0.1162 (3)−0.0774 (2)0.22309 (11)0.0224 (5)
H10A−0.1649−0.12610.24170.027*
C11−0.1828 (3)0.0478 (2)0.20972 (11)0.0225 (5)
H11A−0.27630.08280.21950.027*
C12−0.1106 (2)0.1215 (2)0.18172 (10)0.0183 (4)
H12A−0.15580.20530.17330.022*
C130.0169 (2)0.32006 (19)0.09980 (10)0.0145 (4)
H13A0.03410.33100.05540.017*
H13B−0.07610.32020.10740.017*
C14−0.1539 (2)0.56912 (19)0.13745 (10)0.0142 (4)
C15−0.2506 (2)0.5387 (2)0.17774 (11)0.0192 (5)
H15A−0.22220.46970.20550.023*
C16−0.3882 (2)0.6101 (2)0.17687 (11)0.0212 (5)
H16A−0.45210.58890.20370.025*
C17−0.4304 (2)0.7133 (2)0.13582 (12)0.0223 (5)
H17A−0.52310.76040.13430.027*
C18−0.3347 (2)0.7466 (2)0.09695 (11)0.0222 (5)
H18A−0.36320.81740.07030.027*
C19−0.1965 (2)0.6748 (2)0.09750 (10)0.0172 (4)
H19A−0.13270.69740.07130.021*
C200.1329 (2)0.5313 (2)0.07702 (10)0.0144 (4)
C210.1333 (2)0.6484 (2)0.08547 (10)0.0165 (4)
H21A0.07940.69220.11760.020*
C220.2144 (2)0.6995 (2)0.04593 (11)0.0205 (5)
H22A0.21380.77780.05140.025*
C230.2957 (2)0.6342 (2)−0.00136 (11)0.0230 (5)
H23A0.35020.6685−0.02760.028*
C240.2965 (2)0.5178 (2)−0.00993 (11)0.0226 (5)
H24A0.35130.4740−0.04190.027*
C250.2148 (2)0.4663 (2)0.02946 (10)0.0180 (4)
H25A0.21540.38800.02370.022*
C260.3085 (2)0.3882 (2)0.45772 (10)0.0171 (4)
C270.2424 (2)0.5067 (2)0.47683 (11)0.0225 (5)
H27A0.26190.57220.45530.027*
C280.1483 (3)0.5289 (3)0.52739 (12)0.0303 (6)
H28A0.10520.60840.53960.036*
C290.1194 (3)0.4319 (3)0.55912 (12)0.0336 (7)
H29A0.05490.44670.59240.040*
C300.1848 (3)0.3124 (3)0.54234 (11)0.0307 (6)
H30A0.16490.24760.56450.037*
C310.2803 (3)0.2903 (2)0.49224 (11)0.0225 (5)
C320.5915 (2)0.2698 (2)0.42165 (10)0.0165 (4)
C330.6086 (3)0.2668 (2)0.48475 (11)0.0215 (5)
H33A0.53450.30670.51110.026*
C340.7365 (3)0.2039 (2)0.50829 (12)0.0262 (5)
H34A0.74700.20060.55050.031*
C350.8479 (3)0.1465 (2)0.46937 (12)0.0263 (5)
H35A0.93350.10620.48530.032*
C360.8325 (2)0.1487 (2)0.40697 (12)0.0251 (5)
H36A0.90740.10970.38080.030*
C370.7044 (2)0.2096 (2)0.38307 (11)0.0205 (5)
H37A0.69400.21010.34100.025*
C380.4412 (2)0.5069 (2)0.36453 (10)0.0156 (4)
C390.5592 (2)0.5330 (2)0.37148 (11)0.0206 (5)
H39A0.63410.47310.38940.025*
C400.5655 (3)0.6487 (2)0.35168 (11)0.0261 (5)
H40A0.64500.66510.35600.031*
C410.4541 (3)0.7389 (2)0.32574 (11)0.0277 (6)
H41A0.45840.81620.31310.033*
C420.3359 (3)0.7140 (2)0.31854 (11)0.0256 (5)
H42A0.26060.77460.30130.031*
C430.3305 (3)0.5985 (2)0.33716 (11)0.0204 (5)
H43A0.25190.58170.33140.024*
C440.2190 (2)0.0905 (2)0.27097 (10)0.0168 (4)
C450.4604 (2)0.0246 (2)0.20180 (10)0.0182 (5)
C460.3947 (2)0.2583 (2)0.14876 (10)0.0167 (4)
C470.2710 (2)0.4822 (2)0.21067 (10)0.0173 (4)
C480.0229 (2)0.5545 (2)0.27574 (10)0.0182 (5)
C490.0088 (2)0.3253 (2)0.26981 (10)0.0170 (4)
C500.2029 (2)0.2631 (2)0.35747 (10)0.0175 (4)
C510.4774 (2)0.1058 (2)0.33704 (10)0.0178 (4)
C520.5059 (2)0.3065 (2)0.25589 (10)0.0173 (4)
C530.3141 (3)0.0748 (3)0.49814 (14)0.0371 (7)
H53A0.36830.00210.47800.056*
H53B0.21890.09290.49180.056*
H53C0.32830.06140.54170.056*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.01299 (8)0.01047 (8)0.01293 (8)−0.00370 (6)−0.00310 (6)−0.00082 (6)
Ru20.01320 (8)0.01058 (8)0.01226 (8)−0.00360 (6)−0.00261 (6)−0.00003 (6)
Ru30.01372 (8)0.01118 (8)0.01253 (8)−0.00423 (6)−0.00349 (6)−0.00038 (6)
As10.01311 (10)0.01034 (10)0.01269 (10)−0.00425 (8)−0.00292 (8)−0.00022 (8)
As20.01245 (10)0.01009 (10)0.01241 (10)−0.00383 (8)−0.00205 (8)0.00073 (8)
P10.0157 (3)0.0133 (3)0.0136 (3)−0.0060 (2)−0.0029 (2)−0.0005 (2)
O10.0313 (10)0.0192 (8)0.0195 (8)−0.0113 (7)−0.0010 (7)0.0004 (7)
O20.0214 (9)0.0183 (9)0.0372 (10)0.0009 (7)−0.0057 (8)−0.0051 (8)
O30.0232 (9)0.0246 (9)0.0219 (9)−0.0087 (7)0.0018 (7)−0.0004 (7)
O40.0202 (9)0.0234 (9)0.0297 (9)−0.0109 (7)−0.0069 (7)0.0044 (7)
O50.0387 (11)0.0162 (9)0.0269 (10)−0.0024 (8)0.0089 (8)−0.0027 (7)
O60.0216 (9)0.0260 (9)0.0261 (9)−0.0115 (7)−0.0050 (7)0.0080 (7)
O70.0203 (9)0.0317 (9)0.0161 (8)−0.0104 (7)−0.0009 (7)−0.0025 (7)
O80.0355 (11)0.0154 (8)0.0341 (10)−0.0043 (8)−0.0139 (8)0.0024 (8)
O90.0191 (8)0.0248 (9)0.0234 (9)−0.0079 (7)−0.0009 (7)0.0033 (7)
O100.0321 (10)0.0238 (9)0.0223 (9)−0.0165 (8)−0.0063 (7)0.0067 (7)
C10.0175 (10)0.0102 (9)0.0135 (10)−0.0064 (8)0.0001 (8)0.0000 (8)
C20.0170 (11)0.0157 (10)0.0170 (11)−0.0062 (9)−0.0036 (8)0.0009 (9)
C30.0165 (11)0.0152 (10)0.0212 (11)−0.0036 (9)0.0000 (9)−0.0024 (9)
C40.0246 (12)0.0168 (11)0.0158 (11)−0.0103 (9)0.0003 (9)−0.0024 (9)
C50.0209 (11)0.0181 (11)0.0159 (11)−0.0074 (9)−0.0067 (9)0.0016 (9)
C60.0157 (11)0.0137 (10)0.0202 (11)−0.0044 (8)−0.0038 (9)0.0002 (9)
C70.0201 (11)0.0152 (10)0.0121 (10)−0.0090 (9)−0.0014 (8)−0.0016 (8)
C80.0181 (11)0.0162 (11)0.0193 (11)−0.0069 (9)−0.0039 (9)−0.0005 (9)
C90.0282 (13)0.0149 (11)0.0190 (11)−0.0096 (10)−0.0054 (9)0.0020 (9)
C100.0267 (13)0.0216 (12)0.0232 (12)−0.0146 (10)0.0000 (10)0.0010 (10)
C110.0195 (12)0.0229 (12)0.0256 (12)−0.0090 (10)0.0031 (10)−0.0020 (10)
C120.0181 (11)0.0147 (10)0.0211 (11)−0.0045 (9)−0.0020 (9)−0.0008 (9)
C130.0153 (10)0.0115 (10)0.0163 (10)−0.0036 (8)−0.0047 (8)0.0001 (8)
C140.0141 (10)0.0132 (10)0.0150 (10)−0.0036 (8)−0.0034 (8)−0.0011 (8)
C150.0172 (11)0.0186 (11)0.0207 (11)−0.0059 (9)−0.0034 (9)0.0037 (9)
C160.0191 (11)0.0235 (12)0.0234 (12)−0.0103 (10)0.0009 (9)−0.0035 (10)
C170.0133 (11)0.0198 (11)0.0317 (13)−0.0020 (9)−0.0035 (10)−0.0049 (10)
C180.0234 (12)0.0156 (11)0.0255 (12)−0.0034 (9)−0.0065 (10)0.0004 (10)
C190.0182 (11)0.0134 (10)0.0203 (11)−0.0060 (9)−0.0024 (9)0.0012 (9)
C200.0139 (10)0.0157 (10)0.0146 (10)−0.0068 (8)−0.0032 (8)0.0034 (8)
C210.0170 (11)0.0167 (10)0.0162 (10)−0.0064 (9)−0.0020 (8)0.0002 (9)
C220.0222 (12)0.0167 (11)0.0243 (12)−0.0094 (9)−0.0043 (10)0.0031 (9)
C230.0200 (12)0.0275 (13)0.0219 (12)−0.0110 (10)−0.0015 (9)0.0070 (10)
C240.0201 (12)0.0288 (13)0.0164 (11)−0.0065 (10)0.0022 (9)−0.0010 (10)
C250.0196 (11)0.0173 (11)0.0179 (11)−0.0073 (9)−0.0013 (9)−0.0017 (9)
C260.0173 (11)0.0231 (11)0.0135 (10)−0.0096 (9)−0.0032 (8)−0.0018 (9)
C270.0192 (12)0.0291 (13)0.0200 (12)−0.0080 (10)−0.0036 (9)−0.0050 (10)
C280.0237 (13)0.0435 (16)0.0221 (13)−0.0072 (12)−0.0014 (10)−0.0108 (12)
C290.0232 (14)0.062 (2)0.0147 (12)−0.0135 (14)0.0026 (10)−0.0069 (13)
C300.0311 (14)0.0494 (17)0.0165 (12)−0.0219 (13)−0.0034 (10)0.0071 (12)
C310.0243 (12)0.0323 (13)0.0163 (11)−0.0162 (11)−0.0074 (9)0.0024 (10)
C320.0185 (11)0.0134 (10)0.0200 (11)−0.0082 (9)−0.0072 (9)0.0033 (9)
C330.0269 (13)0.0172 (11)0.0208 (12)−0.0069 (10)−0.0077 (10)−0.0007 (9)
C340.0332 (14)0.0222 (12)0.0253 (13)−0.0102 (11)−0.0140 (11)0.0022 (10)
C350.0241 (13)0.0208 (12)0.0338 (14)−0.0077 (10)−0.0142 (11)0.0090 (11)
C360.0176 (12)0.0218 (12)0.0341 (14)−0.0061 (10)−0.0024 (10)0.0043 (11)
C370.0201 (12)0.0241 (12)0.0189 (11)−0.0102 (10)−0.0035 (9)0.0035 (10)
C380.0222 (11)0.0146 (10)0.0121 (10)−0.0083 (9)−0.0019 (8)−0.0028 (8)
C390.0228 (12)0.0210 (12)0.0206 (11)−0.0106 (10)−0.0049 (9)0.0015 (9)
C400.0311 (14)0.0282 (13)0.0261 (13)−0.0191 (11)−0.0056 (11)0.0014 (11)
C410.0477 (17)0.0179 (12)0.0223 (12)−0.0176 (12)−0.0048 (11)0.0022 (10)
C420.0351 (15)0.0170 (11)0.0233 (12)−0.0059 (11)−0.0108 (11)0.0012 (10)
C430.0249 (12)0.0164 (11)0.0209 (12)−0.0073 (9)−0.0064 (9)−0.0015 (9)
C440.0199 (11)0.0132 (10)0.0165 (11)−0.0039 (9)−0.0042 (9)−0.0022 (9)
C450.0213 (12)0.0183 (11)0.0182 (11)−0.0098 (9)−0.0027 (9)−0.0037 (9)
C460.0175 (11)0.0140 (10)0.0171 (11)−0.0028 (9)−0.0029 (9)−0.0033 (9)
C470.0161 (11)0.0170 (11)0.0182 (11)−0.0038 (9)−0.0043 (9)−0.0031 (9)
C480.0221 (12)0.0171 (11)0.0161 (11)−0.0088 (9)0.0003 (9)0.0021 (9)
C490.0193 (11)0.0155 (10)0.0138 (10)−0.0026 (9)−0.0064 (9)0.0022 (9)
C500.0188 (11)0.0169 (11)0.0169 (11)−0.0044 (9)−0.0060 (9)−0.0044 (9)
C510.0221 (12)0.0178 (11)0.0158 (11)−0.0089 (9)−0.0049 (9)−0.0011 (9)
C520.0209 (11)0.0141 (10)0.0159 (11)−0.0041 (9)−0.0058 (9)0.0002 (9)
C530.0394 (16)0.0335 (15)0.0441 (17)−0.0230 (14)−0.0149 (13)0.0211 (13)
Geometric parameters (Å, °) top
Ru1—C451.890 (2)C13—H13B0.9700
Ru1—C461.925 (2)C14—C191.392 (3)
Ru1—C441.941 (2)C14—C151.395 (3)
Ru1—As12.4423 (3)C15—C161.384 (3)
Ru1—Ru32.8471 (2)C15—H15A0.9300
Ru1—Ru22.8616 (2)C16—C171.385 (3)
Ru2—C481.887 (2)C16—H16A0.9300
Ru2—C471.933 (2)C17—C181.386 (3)
Ru2—C491.934 (2)C17—H17A0.9300
Ru2—As22.4209 (3)C18—C191.389 (3)
Ru2—Ru32.8830 (2)C18—H18A0.9300
Ru3—C511.885 (2)C19—H19A0.9300
Ru3—C501.933 (2)C20—C251.386 (3)
Ru3—C521.939 (2)C20—C211.397 (3)
Ru3—P12.3495 (6)C21—C221.391 (3)
As1—C71.952 (2)C21—H21A0.9300
As1—C11.953 (2)C22—C231.380 (3)
As1—C131.968 (2)C22—H22A0.9300
As2—C141.939 (2)C23—C241.385 (3)
As2—C201.940 (2)C23—H23A0.9300
As2—C131.965 (2)C24—C251.396 (3)
P1—C261.822 (2)C24—H24A0.9300
P1—C381.833 (2)C25—H25A0.9300
P1—C321.838 (2)C26—C271.396 (3)
O1—C441.139 (3)C26—C311.407 (3)
O2—C451.148 (3)C27—C281.389 (3)
O3—C461.150 (3)C27—H27A0.9300
O4—C471.141 (3)C28—C291.375 (4)
O5—C481.145 (3)C28—H28A0.9300
O6—C491.146 (3)C29—C301.388 (4)
O7—C501.148 (3)C29—H29A0.9300
O8—C511.144 (3)C30—C311.389 (4)
O9—C521.142 (3)C30—H30A0.9300
O10—C311.368 (3)C32—C371.395 (3)
O10—C531.436 (3)C32—C331.395 (3)
C1—C21.391 (3)C33—C341.392 (3)
C1—C61.399 (3)C33—H33A0.9300
C2—C31.389 (3)C34—C351.381 (4)
C2—H2A0.9300C34—H34A0.9300
C3—C41.387 (3)C35—C361.378 (4)
C3—H3A0.9300C35—H35A0.9300
C4—C51.383 (3)C36—C371.394 (3)
C4—H4A0.9300C36—H36A0.9300
C5—C61.383 (3)C37—H37A0.9300
C5—H5A0.9300C38—C391.393 (3)
C6—H6A0.9300C38—C431.398 (3)
C7—C121.386 (3)C39—C401.395 (3)
C7—C81.401 (3)C39—H39A0.9300
C8—C91.387 (3)C40—C411.382 (4)
C8—H8A0.9300C40—H40A0.9300
C9—C101.391 (3)C41—C421.389 (4)
C9—H9A0.9300C41—H41A0.9300
C10—C111.389 (3)C42—C431.385 (3)
C10—H10A0.9300C42—H42A0.9300
C11—C121.395 (3)C43—H43A0.9300
C11—H11A0.9300C53—H53A0.9600
C12—H12A0.9300C53—H53B0.9600
C13—H13A0.9700C53—H53C0.9600
C45—Ru1—C4691.04 (9)C19—C14—C15119.3 (2)
C45—Ru1—C4490.46 (9)C19—C14—As2123.36 (16)
C46—Ru1—C44172.53 (9)C15—C14—As2117.35 (16)
C45—Ru1—As1107.84 (7)C16—C15—C14120.7 (2)
C46—Ru1—As195.19 (6)C16—C15—H15A119.6
C44—Ru1—As191.31 (6)C14—C15—H15A119.6
C45—Ru1—Ru398.86 (7)C15—C16—C17119.7 (2)
C46—Ru1—Ru391.92 (6)C15—C16—H16A120.2
C44—Ru1—Ru380.62 (6)C17—C16—H16A120.2
As1—Ru1—Ru3152.186 (9)C16—C17—C18120.1 (2)
C45—Ru1—Ru2158.58 (6)C16—C17—H17A120.0
C46—Ru1—Ru283.95 (7)C18—C17—H17A120.0
C44—Ru1—Ru292.01 (7)C17—C18—C19120.4 (2)
As1—Ru1—Ru293.368 (8)C17—C18—H18A119.8
Ru3—Ru1—Ru260.666 (6)C19—C18—H18A119.8
C48—Ru2—C4791.34 (9)C18—C19—C14119.8 (2)
C48—Ru2—C4991.77 (9)C18—C19—H19A120.1
C47—Ru2—C49175.54 (9)C14—C19—H19A120.1
C48—Ru2—As297.50 (7)C25—C20—C21119.46 (19)
C47—Ru2—As291.55 (6)C25—C20—As2122.17 (16)
C49—Ru2—As291.22 (6)C21—C20—As2117.89 (16)
C48—Ru2—Ru1169.88 (7)C22—C21—C20120.1 (2)
C47—Ru2—Ru193.48 (7)C22—C21—H21A120.0
C49—Ru2—Ru182.96 (7)C20—C21—H21A120.0
As2—Ru2—Ru191.262 (8)C23—C22—C21120.2 (2)
C48—Ru2—Ru3113.31 (7)C23—C22—H22A119.9
C47—Ru2—Ru376.67 (6)C21—C22—H22A119.9
C49—Ru2—Ru399.15 (6)C22—C23—C24120.2 (2)
As2—Ru2—Ru3146.953 (10)C22—C23—H23A119.9
Ru1—Ru2—Ru359.420 (6)C24—C23—H23A119.9
C51—Ru3—C5095.57 (10)C23—C24—C25119.9 (2)
C51—Ru3—C5297.26 (10)C23—C24—H24A120.1
C50—Ru3—C52167.15 (9)C25—C24—H24A120.1
C51—Ru3—P193.36 (7)C20—C25—C24120.2 (2)
C50—Ru3—P190.24 (6)C20—C25—H25A119.9
C52—Ru3—P188.34 (7)C24—C25—H25A119.9
C51—Ru3—Ru189.47 (7)C27—C26—C31118.2 (2)
C50—Ru3—Ru193.66 (6)C27—C26—P1122.46 (17)
C52—Ru3—Ru187.15 (6)C31—C26—P1119.37 (18)
P1—Ru3—Ru1174.946 (15)C28—C27—C26121.4 (2)
C51—Ru3—Ru2145.12 (6)C28—C27—H27A119.3
C50—Ru3—Ru272.13 (6)C26—C27—H27A119.3
C52—Ru3—Ru297.40 (6)C29—C28—C27119.2 (3)
P1—Ru3—Ru2118.530 (16)C29—C28—H28A120.4
Ru1—Ru3—Ru259.915 (6)C27—C28—H28A120.4
C7—As1—C197.55 (9)C28—C29—C30121.2 (2)
C7—As1—C13104.20 (9)C28—C29—H29A119.4
C1—As1—C13100.98 (9)C30—C29—H29A119.4
C7—As1—Ru1112.20 (6)C29—C30—C31119.5 (2)
C1—As1—Ru1122.94 (6)C29—C30—H30A120.3
C13—As1—Ru1116.04 (6)C31—C30—H30A120.3
C14—As2—C20104.26 (9)O10—C31—C30124.8 (2)
C14—As2—C1399.21 (9)O10—C31—C26114.7 (2)
C20—As2—C13104.44 (9)C30—C31—C26120.5 (2)
C14—As2—Ru2116.46 (6)C37—C32—C33118.9 (2)
C20—As2—Ru2114.03 (6)C37—C32—P1120.28 (17)
C13—As2—Ru2116.51 (6)C33—C32—P1120.79 (18)
C26—P1—C38103.46 (10)C34—C33—C32120.1 (2)
C26—P1—C32102.75 (10)C34—C33—H33A120.0
C38—P1—C32102.83 (10)C32—C33—H33A120.0
C26—P1—Ru3117.33 (7)C35—C34—C33120.4 (2)
C38—P1—Ru3113.44 (7)C35—C34—H34A119.8
C32—P1—Ru3115.22 (7)C33—C34—H34A119.8
C31—O10—C53117.7 (2)C36—C35—C34120.1 (2)
C2—C1—C6119.1 (2)C36—C35—H35A119.9
C2—C1—As1120.56 (16)C34—C35—H35A119.9
C6—C1—As1120.17 (16)C35—C36—C37119.9 (2)
C3—C2—C1120.2 (2)C35—C36—H36A120.0
C3—C2—H2A119.9C37—C36—H36A120.0
C1—C2—H2A119.9C36—C37—C32120.6 (2)
C4—C3—C2120.0 (2)C36—C37—H37A119.7
C4—C3—H3A120.0C32—C37—H37A119.7
C2—C3—H3A120.0C39—C38—C43118.6 (2)
C5—C4—C3120.2 (2)C39—C38—P1122.91 (18)
C5—C4—H4A119.9C43—C38—P1118.50 (16)
C3—C4—H4A119.9C38—C39—C40120.3 (2)
C6—C5—C4119.8 (2)C38—C39—H39A119.9
C6—C5—H5A120.1C40—C39—H39A119.9
C4—C5—H5A120.1C41—C40—C39120.4 (2)
C5—C6—C1120.6 (2)C41—C40—H40A119.8
C5—C6—H6A119.7C39—C40—H40A119.8
C1—C6—H6A119.7C40—C41—C42119.9 (2)
C12—C7—C8119.4 (2)C40—C41—H41A120.0
C12—C7—As1125.02 (16)C42—C41—H41A120.0
C8—C7—As1115.46 (16)C43—C42—C41119.8 (2)
C9—C8—C7120.5 (2)C43—C42—H42A120.1
C9—C8—H8A119.7C41—C42—H42A120.1
C7—C8—H8A119.7C42—C43—C38121.1 (2)
C8—C9—C10120.0 (2)C42—C43—H43A119.5
C8—C9—H9A120.0C38—C43—H43A119.5
C10—C9—H9A120.0O1—C44—Ru1174.8 (2)
C11—C10—C9119.5 (2)O2—C45—Ru1175.9 (2)
C11—C10—H10A120.2O3—C46—Ru1174.4 (2)
C9—C10—H10A120.2O4—C47—Ru2170.1 (2)
C10—C11—C12120.6 (2)O5—C48—Ru2176.4 (2)
C10—C11—H11A119.7O6—C49—Ru2173.66 (19)
C12—C11—H11A119.7O7—C50—Ru3171.28 (19)
C7—C12—C11119.9 (2)O8—C51—Ru3176.9 (2)
C7—C12—H12A120.0O9—C52—Ru3174.72 (19)
C11—C12—H12A120.0O10—C53—H53A109.5
As2—C13—As1111.74 (10)O10—C53—H53B109.5
As2—C13—H13A109.3H53A—C53—H53B109.5
As1—C13—H13A109.3O10—C53—H53C109.5
As2—C13—H13B109.3H53A—C53—H53C109.5
As1—C13—H13B109.3H53B—C53—H53C109.5
H13A—C13—H13B107.9
C45—Ru1—Ru2—C48−64.4 (4)C7—As1—C1—C2−106.30 (17)
C46—Ru1—Ru2—C48−141.6 (4)C13—As1—C1—C2147.58 (16)
C44—Ru1—Ru2—C4832.1 (4)Ru1—As1—C1—C216.38 (19)
As1—Ru1—Ru2—C48123.5 (4)C7—As1—C1—C668.64 (18)
Ru3—Ru1—Ru2—C48−46.0 (4)C13—As1—C1—C6−37.49 (18)
C45—Ru1—Ru2—C4753.9 (2)Ru1—As1—C1—C6−168.68 (13)
C46—Ru1—Ru2—C47−23.35 (9)C6—C1—C2—C30.3 (3)
C44—Ru1—Ru2—C47150.35 (9)As1—C1—C2—C3175.31 (16)
As1—Ru1—Ru2—C47−118.22 (6)C1—C2—C3—C41.1 (3)
Ru3—Ru1—Ru2—C4772.29 (6)C2—C3—C4—C5−1.0 (3)
C45—Ru1—Ru2—C49−123.4 (2)C3—C4—C5—C6−0.4 (3)
C46—Ru1—Ru2—C49159.35 (9)C4—C5—C6—C11.8 (3)
C44—Ru1—Ru2—C49−26.95 (9)C2—C1—C6—C5−1.8 (3)
As1—Ru1—Ru2—C4964.48 (6)As1—C1—C6—C5−176.76 (16)
Ru3—Ru1—Ru2—C49−105.01 (6)C1—As1—C7—C12−120.94 (19)
C45—Ru1—Ru2—As2145.56 (19)C13—As1—C7—C12−17.5 (2)
C46—Ru1—Ru2—As268.28 (6)Ru1—As1—C7—C12108.78 (18)
C44—Ru1—Ru2—As2−118.02 (6)C1—As1—C7—C863.38 (18)
As1—Ru1—Ru2—As2−26.588 (9)C13—As1—C7—C8166.78 (16)
Ru3—Ru1—Ru2—As2163.916 (9)Ru1—As1—C7—C8−66.90 (17)
C45—Ru1—Ru2—Ru3−18.36 (19)C12—C7—C8—C90.5 (3)
C46—Ru1—Ru2—Ru3−95.63 (6)As1—C7—C8—C9176.41 (17)
C44—Ru1—Ru2—Ru378.06 (6)C7—C8—C9—C100.3 (3)
As1—Ru1—Ru2—Ru3169.496 (9)C8—C9—C10—C11−0.6 (4)
C45—Ru1—Ru3—C51−24.23 (10)C9—C10—C11—C120.1 (4)
C46—Ru1—Ru3—C51−115.58 (10)C8—C7—C12—C11−0.9 (3)
C44—Ru1—Ru3—C5164.77 (10)As1—C7—C12—C11−176.44 (17)
As1—Ru1—Ru3—C51139.50 (7)C10—C11—C12—C70.6 (4)
Ru2—Ru1—Ru3—C51162.45 (7)C14—As2—C13—As1−148.46 (11)
C45—Ru1—Ru3—C50−119.78 (9)C20—As2—C13—As1104.11 (11)
C46—Ru1—Ru3—C50148.86 (9)Ru2—As2—C13—As1−22.64 (13)
C44—Ru1—Ru3—C50−30.78 (9)C7—As1—C13—As2120.32 (11)
As1—Ru1—Ru3—C5043.95 (7)C1—As1—C13—As2−138.89 (10)
Ru2—Ru1—Ru3—C5066.90 (7)Ru1—As1—C13—As2−3.55 (13)
C45—Ru1—Ru3—C5273.07 (9)C20—As2—C14—C190.7 (2)
C46—Ru1—Ru3—C52−18.29 (9)C13—As2—C14—C19−106.86 (19)
C44—Ru1—Ru3—C52162.07 (9)Ru2—As2—C14—C19127.29 (17)
As1—Ru1—Ru3—C52−123.20 (7)C20—As2—C14—C15179.39 (17)
Ru2—Ru1—Ru3—C52−100.25 (7)C13—As2—C14—C1571.82 (18)
C45—Ru1—Ru3—Ru2173.32 (7)Ru2—As2—C14—C15−54.04 (18)
C46—Ru1—Ru3—Ru281.96 (7)C19—C14—C15—C162.2 (3)
C44—Ru1—Ru3—Ru2−97.68 (7)As2—C14—C15—C16−176.57 (18)
As1—Ru1—Ru3—Ru2−22.956 (18)C14—C15—C16—C17−0.4 (3)
C48—Ru2—Ru3—C51140.28 (14)C15—C16—C17—C18−1.7 (4)
C47—Ru2—Ru3—C51−134.08 (14)C16—C17—C18—C192.0 (4)
C49—Ru2—Ru3—C5144.34 (14)C17—C18—C19—C14−0.2 (3)
As2—Ru2—Ru3—C51−62.34 (12)C15—C14—C19—C18−1.8 (3)
Ru1—Ru2—Ru3—C51−31.81 (12)As2—C14—C19—C18176.81 (17)
C48—Ru2—Ru3—C5066.77 (10)C14—As2—C20—C25−126.47 (18)
C47—Ru2—Ru3—C50152.42 (10)C13—As2—C20—C25−22.8 (2)
C49—Ru2—Ru3—C50−29.16 (10)Ru2—As2—C20—C25105.46 (17)
As2—Ru2—Ru3—C50−135.84 (7)C14—As2—C20—C2161.52 (18)
Ru1—Ru2—Ru3—C50−105.32 (7)C13—As2—C20—C21165.16 (16)
C48—Ru2—Ru3—C52−105.57 (10)Ru2—As2—C20—C21−66.56 (18)
C47—Ru2—Ru3—C52−19.92 (10)C25—C20—C21—C220.7 (3)
C49—Ru2—Ru3—C52158.50 (9)As2—C20—C21—C22172.95 (16)
As2—Ru2—Ru3—C5251.82 (7)C20—C21—C22—C23−0.7 (3)
Ru1—Ru2—Ru3—C5282.34 (7)C21—C22—C23—C240.4 (3)
C48—Ru2—Ru3—P1−13.43 (7)C22—C23—C24—C25−0.1 (4)
C47—Ru2—Ru3—P172.22 (7)C21—C20—C25—C24−0.4 (3)
C49—Ru2—Ru3—P1−109.36 (7)As2—C20—C25—C24−172.32 (17)
As2—Ru2—Ru3—P1143.96 (2)C23—C24—C25—C200.1 (3)
Ru1—Ru2—Ru3—P1174.484 (18)C38—P1—C26—C276.5 (2)
C48—Ru2—Ru3—Ru1172.09 (7)C32—P1—C26—C27113.28 (19)
C47—Ru2—Ru3—Ru1−102.26 (7)Ru3—P1—C26—C27−119.22 (17)
C49—Ru2—Ru3—Ru176.15 (7)C38—P1—C26—C31−175.21 (17)
As2—Ru2—Ru3—Ru1−30.525 (15)C32—P1—C26—C31−68.45 (19)
C45—Ru1—As1—C785.03 (10)Ru3—P1—C26—C3159.04 (19)
C46—Ru1—As1—C7177.80 (10)C31—C26—C27—C28−1.8 (3)
C44—Ru1—As1—C7−5.88 (10)P1—C26—C27—C28176.48 (18)
Ru3—Ru1—As1—C7−78.06 (7)C26—C27—C28—C29−0.2 (4)
Ru2—Ru1—As1—C7−97.98 (7)C27—C28—C29—C301.4 (4)
C45—Ru1—As1—C1−30.66 (10)C28—C29—C30—C31−0.6 (4)
C46—Ru1—As1—C162.12 (10)C53—O10—C31—C3011.7 (3)
C44—Ru1—As1—C1−121.57 (10)C53—O10—C31—C26−169.1 (2)
Ru3—Ru1—As1—C1166.25 (7)C29—C30—C31—O10177.8 (2)
Ru2—Ru1—As1—C1146.34 (7)C29—C30—C31—C26−1.4 (4)
C45—Ru1—As1—C13−155.35 (10)C27—C26—C31—O10−176.68 (19)
C46—Ru1—As1—C13−62.58 (10)P1—C26—C31—O105.0 (3)
C44—Ru1—As1—C13113.73 (10)C27—C26—C31—C302.6 (3)
Ru3—Ru1—As1—C1341.55 (8)P1—C26—C31—C30−175.73 (18)
Ru2—Ru1—As1—C1321.64 (7)C26—P1—C32—C37168.47 (18)
C48—Ru2—As2—C14−26.10 (10)C38—P1—C32—C37−84.30 (19)
C47—Ru2—As2—C14−117.66 (10)Ru3—P1—C32—C3739.64 (19)
C49—Ru2—As2—C1465.84 (10)C26—P1—C32—C33−14.2 (2)
Ru1—Ru2—As2—C14148.83 (7)C38—P1—C32—C3393.00 (19)
Ru3—Ru2—As2—C14174.76 (7)Ru3—P1—C32—C33−143.06 (16)
C48—Ru2—As2—C2095.45 (10)C37—C32—C33—C34−0.3 (3)
C47—Ru2—As2—C203.89 (10)P1—C32—C33—C34−177.61 (17)
C49—Ru2—As2—C20−172.61 (10)C32—C33—C34—C351.4 (4)
Ru1—Ru2—As2—C20−89.62 (7)C33—C34—C35—C36−1.4 (4)
Ru3—Ru2—As2—C20−63.69 (8)C34—C35—C36—C370.3 (4)
C48—Ru2—As2—C13−142.72 (10)C35—C36—C37—C320.8 (3)
C47—Ru2—As2—C13125.73 (10)C33—C32—C37—C36−0.8 (3)
C49—Ru2—As2—C13−50.77 (10)P1—C32—C37—C36176.54 (17)
Ru1—Ru2—As2—C1332.21 (7)C26—P1—C38—C39107.4 (2)
Ru3—Ru2—As2—C1358.15 (7)C32—P1—C38—C390.7 (2)
C51—Ru3—P1—C26−95.89 (11)Ru3—P1—C38—C39−124.40 (18)
C50—Ru3—P1—C26−0.29 (11)C26—P1—C38—C43−73.14 (19)
C52—Ru3—P1—C26166.93 (11)C32—P1—C38—C43−179.84 (18)
Ru2—Ru3—P1—C2669.41 (9)Ru3—P1—C38—C4355.06 (19)
C51—Ru3—P1—C38143.46 (11)C43—C38—C39—C400.3 (3)
C50—Ru3—P1—C38−120.94 (11)P1—C38—C39—C40179.77 (19)
C52—Ru3—P1—C3846.28 (10)C38—C39—C40—C410.9 (4)
Ru2—Ru3—P1—C38−51.24 (8)C39—C40—C41—C42−0.9 (4)
C51—Ru3—P1—C3225.31 (11)C40—C41—C42—C43−0.3 (4)
C50—Ru3—P1—C32120.91 (10)C41—C42—C43—C381.5 (4)
C52—Ru3—P1—C32−71.87 (10)C39—C38—C43—C42−1.5 (3)
Ru2—Ru3—P1—C32−169.39 (8)P1—C38—C43—C42179.03 (19)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
C16—H16A···O4i0.932.523.244 (3)135
C29—H29A···O5ii0.932.563.286 (3)135
C5—H5A···Cg1iii0.932.843.668 (2)149
C18—H18A···Cg2iv0.932.953.701 (2)139
C22—H22A···Cg2v0.932.953.787 (2)151
C24—H24A···Cg3iv0.932.813.499 (2)132
Symmetry codes: (i) x−1, y, z; (ii) −x, −y+1, −z+1; (iii) −x, −y, −z; (iv) −x, −y+1, −z; (v) x, y+1, z.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
C16—H16A···O4i0.932.523.244 (3)135
C29—H29A···O5ii0.932.563.286 (3)135
C5—H5A···Cg1iii0.932.843.668 (2)149
C18—H18A···Cg2iv0.932.953.701 (2)139
C22—H22A···Cg2v0.932.953.787 (2)151
C24—H24A···Cg3iv0.932.813.499 (2)132
Symmetry codes: (i) x−1, y, z; (ii) −x, −y+1, −z+1; (iii) −x, −y, −z; (iv) −x, −y+1, −z; (v) x, y+1, z.
Acknowledgements top

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 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
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