Literature DB >> 21522853

[μ-Bis(diphenyl-arsanyl)methane-1:2κAs:As']nona-carbonyl-1κC,2κC,3κC-[(4-methyl-sulfanylphen-yl)diphenyl-phosphane-3κP]-triangulo-triruthenium(0).

Omar Bin Shawkataly, Imthyaz Ahmed Khan, H A Hafiz Malik, Chin Sing Yeap, Hoong-Kun Fun.   

Abstract

In the title triangulo-triruthenium compound, [Ru(3)(C(25)H(22)As(2))(C(19)H(17)PS)(CO)(9)], the bis-(diphenyl-arsanyl)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 Ru(3) 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 diphenyl-arsanyl groups. In the crystal, mol-ecules are linked into a three-dimensional framework by inter-molecular C-H⋯O hydrogen bonds. Weak inter-molecular C-H⋯π inter-actions stabilize the crystal structure.

Entities:  

Year:  2011        PMID: 21522853      PMCID: PMC3051533          DOI: 10.1107/S1600536810054206

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


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 = 1335.92 Monoclinic, 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[F 2 > 2σ(F 2)] = 0.032 wR(F 2) = 0.081 S = 1.02 14623 reflections 623 parameters H-atom parameters constrained Δρmax = 1.24 e Å−3 Δρmin = −0.97 e Å−3 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 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810054206/sj5088sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810054206/sj5088Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ru3(C25H22As2)(C19H17PS)(CO)9]F(000) = 2632
Mr = 1335.92Dx = 1.761 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9884 reflections
a = 16.1070 (11) Åθ = 2.8–30.0°
b = 16.7244 (12) ŵ = 2.32 mm1
c = 24.3147 (13) ÅT = 100 K
β = 129.712 (3)°Needle, brown
V = 5038.6 (6) Å30.19 × 0.07 × 0.03 mm
Z = 4
Bruker APEXII DUO CCD area-detector diffractometer14623 independent reflections
Radiation source: fine-focus sealed tube11553 reflections with I > 2σ(I)
graphiteRint = 0.036
φ and ω scansθmax = 30.0°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2009)h = −22→22
Tmin = 0.660, Tmax = 0.927k = −22→23
41559 measured reflectionsl = −34→30
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H-atom parameters constrained
S = 1.02w = 1/[σ2(Fo2) + (0.043P)2 + 0.5735P] where P = (Fo2 + 2Fc2)/3
14623 reflections(Δ/σ)max = 0.002
623 parametersΔρmax = 1.24 e Å3
0 restraintsΔρmin = −0.97 e Å3
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.
xyzUiso*/Ueq
Ru10.298134 (17)0.831631 (12)0.779202 (12)0.01628 (5)
Ru20.366549 (16)0.752105 (11)0.710419 (11)0.01393 (5)
Ru30.229637 (16)0.671585 (12)0.727742 (11)0.01448 (5)
As10.34320 (2)0.961468 (15)0.760642 (15)0.01670 (6)
As20.48023 (2)0.861583 (15)0.726315 (14)0.01358 (6)
S10.29520 (7)0.30382 (5)0.94198 (5)0.03403 (18)
P10.11515 (5)0.61875 (4)0.74696 (4)0.01794 (13)
O10.06273 (17)0.85680 (13)0.64359 (13)0.0332 (5)
O20.2509 (2)0.88001 (16)0.87696 (15)0.0481 (7)
O30.53465 (17)0.81202 (12)0.91484 (12)0.0290 (5)
O40.55898 (18)0.66694 (12)0.84723 (12)0.0305 (5)
O50.3699 (2)0.62869 (13)0.62036 (14)0.0384 (6)
O60.17484 (18)0.83165 (13)0.57129 (12)0.0314 (5)
O70.03756 (19)0.70147 (14)0.56881 (12)0.0384 (5)
O80.2900 (2)0.52208 (12)0.69080 (13)0.0350 (5)
O90.40236 (17)0.65945 (12)0.89112 (11)0.0274 (4)
C10.2316 (2)1.01511 (17)0.67165 (17)0.0258 (6)
C20.2373 (3)1.02328 (19)0.61772 (18)0.0327 (7)
H2A0.29771.00490.62440.039*
C30.1528 (3)1.0589 (2)0.5532 (2)0.0501 (10)
H3A0.15641.06280.51660.060*
C40.0652 (3)1.0880 (3)0.5430 (2)0.0597 (12)
H4A0.01011.11300.50020.072*
C50.0581 (3)1.0804 (2)0.5963 (3)0.0587 (12)
H5A−0.00181.10060.58930.070*
C60.1400 (3)1.0425 (2)0.6607 (2)0.0422 (9)
H6A0.13361.03550.69590.051*
C70.3912 (2)1.04386 (16)0.83213 (16)0.0214 (5)
C80.3521 (3)1.12121 (19)0.8150 (2)0.0395 (8)
H8A0.30081.13630.76740.047*
C90.3895 (4)1.1766 (2)0.8691 (2)0.0472 (10)
H9A0.36131.22820.85740.057*
C100.4683 (3)1.15544 (19)0.9401 (2)0.0368 (8)
H10A0.49331.19270.97610.044*
C110.5094 (3)1.07953 (19)0.95709 (18)0.0331 (7)
H11A0.56401.06551.00460.040*
C120.4693 (2)1.02319 (18)0.90326 (17)0.0286 (6)
H12A0.49550.97110.91530.034*
C130.4691 (2)0.96050 (15)0.76505 (15)0.0188 (5)
H13A0.53410.96670.81440.023*
H13B0.46471.00580.73830.023*
C140.4548 (2)0.89586 (15)0.63982 (14)0.0168 (5)
C150.4669 (2)0.97424 (16)0.62777 (15)0.0212 (5)
H15A0.49111.01290.66260.025*
C160.4429 (2)0.99524 (17)0.56330 (16)0.0257 (6)
H16A0.44791.04830.55430.031*
C170.4117 (2)0.93731 (17)0.51296 (15)0.0259 (6)
H17A0.39570.95130.47010.031*
C180.4044 (2)0.85851 (17)0.52652 (16)0.0263 (6)
H18A0.38680.81910.49360.032*
C190.4231 (2)0.83779 (16)0.58862 (15)0.0214 (5)
H19A0.41450.78500.59620.026*
C200.6352 (2)0.84273 (15)0.79266 (14)0.0172 (5)
C210.6878 (3)0.8239 (2)0.76698 (18)0.0362 (8)
H21A0.64990.82290.71790.043*
C220.7977 (3)0.8064 (3)0.8140 (2)0.0511 (11)
H22A0.83290.79370.79630.061*
C230.8542 (3)0.8079 (2)0.8867 (2)0.0410 (8)
H23A0.92710.79450.91800.049*
C240.8029 (3)0.8291 (2)0.91276 (18)0.0397 (8)
H24A0.84160.83230.96180.048*
C250.6924 (2)0.8461 (2)0.86547 (17)0.0328 (7)
H25A0.65730.85970.88320.039*
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)
H27A0.03970.53170.62360.039*
C28−0.1211 (3)0.5126 (2)0.5550 (2)0.0440 (9)
H28A−0.12270.48270.52210.053*
C29−0.2153 (3)0.5280 (2)0.5434 (2)0.0475 (10)
H29A−0.28100.50970.50200.057*
C30−0.2115 (3)0.5704 (2)0.5933 (2)0.0500 (10)
H30A−0.27490.57990.58580.060*
C31−0.1137 (2)0.5997 (2)0.6553 (2)0.0367 (8)
H31A−0.11220.62820.68870.044*
C320.0890 (2)0.68742 (16)0.79316 (16)0.0210 (5)
C330.0218 (2)0.75348 (16)0.75643 (17)0.0260 (6)
H33A−0.01350.76010.70800.031*
C340.0078 (3)0.80941 (18)0.79248 (19)0.0320 (7)
H34A−0.03830.85260.76780.038*
C350.0627 (3)0.80081 (19)0.8652 (2)0.0336 (7)
H35A0.05410.83880.88910.040*
C360.1295 (3)0.73659 (19)0.90170 (19)0.0341 (7)
H36A0.16570.73100.95030.041*
C370.1433 (2)0.67957 (17)0.86618 (17)0.0268 (6)
H37A0.18890.63620.89130.032*
C380.1634 (2)0.52798 (15)0.80201 (15)0.0191 (5)
C390.2553 (2)0.48814 (16)0.82327 (15)0.0209 (5)
H39A0.29320.50770.80910.025*
C400.2921 (2)0.41979 (16)0.86515 (15)0.0223 (5)
H40A0.35320.39370.87790.027*
C410.2383 (2)0.38980 (15)0.88827 (15)0.0206 (5)
C420.1459 (2)0.42901 (17)0.86758 (16)0.0240 (6)
H42A0.10930.41020.88290.029*
C430.1082 (2)0.49637 (16)0.82400 (16)0.0236 (6)
H43A0.04500.52090.80920.028*
C440.1501 (2)0.84081 (16)0.69206 (17)0.0242 (6)
C450.2641 (2)0.86080 (18)0.83811 (17)0.0274 (6)
C460.4472 (2)0.81506 (15)0.86264 (16)0.0211 (5)
C470.4857 (2)0.69993 (16)0.79802 (16)0.0215 (5)
C480.3713 (2)0.67561 (16)0.65498 (16)0.0231 (6)
C490.2428 (2)0.80292 (16)0.62486 (15)0.0211 (5)
C500.1099 (2)0.69369 (17)0.62778 (16)0.0246 (6)
C510.2650 (2)0.57719 (16)0.70502 (15)0.0216 (5)
C520.3425 (2)0.67135 (15)0.83039 (15)0.0194 (5)
C530.2174 (3)0.2842 (2)0.9688 (2)0.0429 (9)
H53A0.24530.23770.99900.064*
H53B0.14360.27490.92730.064*
H53C0.22100.32930.99470.064*
U11U22U33U12U13U23
Ru10.01661 (10)0.01670 (10)0.01801 (11)−0.00152 (7)0.01220 (9)−0.00249 (8)
Ru20.01341 (9)0.01460 (9)0.01386 (10)−0.00012 (7)0.00875 (8)−0.00023 (7)
Ru30.01278 (9)0.01571 (10)0.01328 (10)−0.00109 (7)0.00754 (8)0.00002 (7)
As10.01609 (12)0.01591 (12)0.01858 (14)0.00069 (9)0.01129 (12)−0.00089 (10)
As20.01239 (12)0.01535 (12)0.01197 (12)0.00032 (9)0.00731 (10)0.00076 (9)
S10.0378 (4)0.0299 (4)0.0409 (5)0.0113 (3)0.0281 (4)0.0160 (3)
P10.0141 (3)0.0199 (3)0.0190 (3)0.0006 (2)0.0102 (3)0.0025 (3)
O10.0187 (11)0.0406 (13)0.0310 (13)0.0015 (9)0.0116 (10)−0.0017 (10)
O20.0478 (16)0.0701 (18)0.0462 (16)−0.0237 (13)0.0392 (15)−0.0314 (14)
O30.0225 (11)0.0317 (11)0.0220 (11)0.0001 (9)0.0092 (10)0.0004 (9)
O40.0251 (11)0.0290 (11)0.0265 (12)0.0067 (9)0.0113 (10)0.0087 (9)
O50.0584 (17)0.0286 (12)0.0450 (15)−0.0044 (11)0.0407 (15)−0.0102 (10)
O60.0223 (11)0.0380 (12)0.0222 (11)0.0046 (9)0.0088 (10)0.0073 (9)
O70.0273 (12)0.0419 (13)0.0180 (11)−0.0101 (10)0.0014 (10)0.0039 (10)
O80.0475 (15)0.0246 (11)0.0422 (15)0.0024 (10)0.0329 (13)−0.0018 (10)
O90.0277 (11)0.0290 (11)0.0170 (10)−0.0040 (8)0.0105 (10)0.0027 (8)
C10.0174 (13)0.0218 (13)0.0274 (16)0.0036 (10)0.0094 (13)0.0018 (12)
C20.0225 (15)0.0345 (17)0.0273 (17)0.0013 (13)0.0095 (14)0.0065 (13)
C30.035 (2)0.056 (2)0.029 (2)0.0036 (17)0.0070 (17)0.0167 (17)
C40.034 (2)0.056 (3)0.044 (3)0.0121 (18)0.004 (2)0.023 (2)
C50.0236 (18)0.053 (2)0.063 (3)0.0188 (17)0.011 (2)0.008 (2)
C60.0255 (17)0.047 (2)0.049 (2)0.0115 (15)0.0211 (18)0.0067 (17)
C70.0244 (14)0.0220 (13)0.0240 (14)−0.0030 (10)0.0183 (13)−0.0060 (11)
C80.062 (2)0.0271 (16)0.0338 (19)0.0045 (16)0.033 (2)−0.0005 (14)
C90.086 (3)0.0215 (16)0.047 (2)0.0041 (17)0.048 (3)−0.0027 (15)
C100.055 (2)0.0294 (16)0.039 (2)−0.0137 (15)0.036 (2)−0.0135 (14)
C110.0319 (17)0.0369 (17)0.0244 (16)−0.0085 (13)0.0151 (15)−0.0105 (13)
C120.0245 (15)0.0258 (15)0.0299 (17)−0.0049 (12)0.0148 (14)−0.0103 (12)
C130.0159 (12)0.0213 (13)0.0181 (13)−0.0016 (10)0.0104 (11)−0.0027 (10)
C140.0162 (12)0.0202 (12)0.0132 (12)0.0012 (9)0.0090 (11)0.0030 (10)
C150.0221 (13)0.0212 (13)0.0174 (13)−0.0008 (10)0.0112 (12)0.0011 (10)
C160.0282 (15)0.0235 (14)0.0226 (15)−0.0015 (11)0.0150 (13)0.0051 (11)
C170.0263 (15)0.0326 (15)0.0142 (13)−0.0034 (12)0.0108 (12)0.0029 (11)
C180.0295 (16)0.0286 (15)0.0178 (14)−0.0033 (12)0.0137 (13)−0.0027 (12)
C190.0259 (14)0.0176 (12)0.0195 (14)−0.0026 (10)0.0139 (13)−0.0002 (10)
C200.0107 (11)0.0191 (12)0.0166 (13)0.0003 (9)0.0063 (11)0.0024 (10)
C210.0195 (15)0.061 (2)0.0220 (16)0.0041 (14)0.0104 (14)−0.0085 (15)
C220.0197 (16)0.094 (3)0.034 (2)0.0078 (18)0.0144 (16)−0.014 (2)
C230.0148 (14)0.058 (2)0.036 (2)0.0091 (14)0.0097 (15)0.0066 (17)
C240.0187 (15)0.070 (2)0.0204 (16)0.0041 (15)0.0077 (14)0.0133 (16)
C250.0183 (14)0.059 (2)0.0199 (15)0.0046 (14)0.0118 (13)0.0092 (14)
C260.0163 (13)0.0242 (14)0.0252 (15)−0.0027 (10)0.0093 (12)0.0055 (11)
C270.0253 (15)0.0383 (17)0.0255 (16)−0.0085 (13)0.0125 (14)−0.0021 (13)
C280.041 (2)0.045 (2)0.0294 (19)−0.0199 (17)0.0149 (17)−0.0050 (16)
C290.0271 (18)0.045 (2)0.034 (2)−0.0156 (15)0.0027 (16)0.0013 (17)
C300.0155 (15)0.046 (2)0.062 (3)0.0002 (14)0.0127 (18)0.007 (2)
C310.0185 (15)0.0367 (18)0.045 (2)−0.0029 (13)0.0161 (16)−0.0007 (15)
C320.0205 (13)0.0220 (13)0.0254 (15)0.0002 (10)0.0169 (13)0.0009 (11)
C330.0262 (15)0.0267 (15)0.0257 (15)0.0045 (11)0.0168 (14)0.0047 (12)
C340.0325 (17)0.0277 (15)0.0396 (19)0.0074 (13)0.0248 (16)0.0037 (14)
C350.0383 (18)0.0324 (16)0.045 (2)−0.0012 (14)0.0336 (18)−0.0054 (15)
C360.0415 (19)0.0359 (17)0.0312 (18)−0.0007 (14)0.0262 (17)−0.0003 (14)
C370.0256 (15)0.0283 (15)0.0280 (16)0.0031 (12)0.0178 (14)0.0023 (12)
C380.0154 (12)0.0199 (12)0.0179 (13)−0.0025 (10)0.0088 (11)0.0005 (10)
C390.0222 (13)0.0217 (13)0.0210 (14)0.0008 (10)0.0147 (12)0.0015 (11)
C400.0212 (13)0.0234 (13)0.0213 (14)0.0022 (10)0.0131 (12)0.0000 (11)
C410.0225 (13)0.0163 (12)0.0179 (13)−0.0001 (10)0.0106 (12)0.0021 (10)
C420.0233 (14)0.0252 (14)0.0251 (15)−0.0031 (11)0.0162 (13)0.0030 (11)
C430.0179 (13)0.0247 (14)0.0272 (15)0.0006 (10)0.0139 (13)0.0043 (12)
C440.0229 (14)0.0240 (14)0.0284 (16)−0.0032 (11)0.0177 (14)−0.0060 (12)
C450.0242 (14)0.0319 (15)0.0303 (16)−0.0087 (12)0.0193 (14)−0.0101 (13)
C460.0264 (14)0.0171 (12)0.0229 (14)−0.0017 (10)0.0172 (13)−0.0007 (10)
C470.0220 (13)0.0209 (13)0.0252 (15)−0.0018 (11)0.0167 (13)−0.0004 (11)
C480.0296 (15)0.0198 (13)0.0257 (15)−0.0010 (11)0.0204 (14)−0.0005 (11)
C490.0175 (13)0.0234 (13)0.0203 (14)−0.0026 (10)0.0112 (12)−0.0021 (11)
C500.0210 (14)0.0227 (14)0.0229 (15)−0.0045 (11)0.0107 (13)0.0013 (11)
C510.0192 (13)0.0235 (13)0.0204 (14)−0.0003 (10)0.0118 (12)0.0002 (11)
C520.0205 (13)0.0190 (12)0.0202 (14)−0.0041 (10)0.0138 (12)−0.0015 (10)
C530.0381 (19)0.051 (2)0.044 (2)0.0112 (16)0.0284 (19)0.0252 (17)
Ru1—C451.895 (3)C13—H13B0.9700
Ru1—C461.932 (3)C14—C151.384 (3)
Ru1—C441.934 (3)C14—C191.394 (4)
Ru1—As12.4217 (3)C15—C161.398 (4)
Ru1—Ru22.8522 (3)C15—H15A0.9300
Ru1—Ru32.8606 (3)C16—C171.380 (4)
Ru2—C481.895 (3)C16—H16A0.9300
Ru2—C491.930 (3)C17—C181.382 (4)
Ru2—C471.938 (3)C17—H17A0.9300
Ru2—As22.4393 (3)C18—C191.382 (4)
Ru2—Ru32.8357 (3)C18—H18A0.9300
Ru3—C511.878 (3)C19—H19A0.9300
Ru3—C521.933 (3)C20—C211.372 (4)
Ru3—C501.943 (3)C20—C251.379 (4)
Ru3—P12.3453 (7)C21—C221.393 (4)
As1—C11.936 (3)C21—H21A0.9300
As1—C71.950 (3)C22—C231.377 (5)
As1—C131.962 (2)C22—H22A0.9300
As2—C201.946 (3)C23—C241.372 (5)
As2—C141.954 (2)C23—H23A0.9300
As2—C131.967 (3)C24—C251.399 (4)
S1—C411.756 (3)C24—H24A0.9300
S1—C531.775 (3)C25—H25A0.9300
P1—C321.834 (3)C26—C271.383 (4)
P1—C381.836 (3)C26—C311.395 (4)
P1—C261.839 (3)C27—C281.392 (5)
O1—C441.150 (4)C27—H27A0.9300
O2—C451.140 (3)C28—C291.379 (6)
O3—C461.146 (4)C28—H28A0.9300
O4—C471.151 (3)C29—C301.374 (6)
O5—C481.140 (3)C29—H29A0.9300
O6—C491.142 (3)C30—C311.399 (5)
O7—C501.138 (4)C30—H30A0.9300
O8—C511.144 (3)C31—H31A0.9300
O9—C521.153 (3)C32—C371.397 (4)
C1—C21.378 (4)C32—C331.398 (4)
C1—C61.400 (4)C33—C341.395 (4)
C2—C31.394 (5)C33—H33A0.9300
C2—H2A0.9300C34—C351.389 (5)
C3—C41.358 (6)C34—H34A0.9300
C3—H3A0.9300C35—C361.371 (5)
C4—C51.377 (7)C35—H35A0.9300
C4—H4A0.9300C36—C371.397 (4)
C5—C61.399 (6)C36—H36A0.9300
C5—H5A0.9300C37—H37A0.9300
C6—H6A0.9300C38—C391.388 (4)
C7—C81.381 (4)C38—C431.401 (3)
C7—C121.383 (4)C39—C401.387 (4)
C8—C91.392 (5)C39—H39A0.9300
C8—H8A0.9300C40—C411.394 (4)
C9—C101.385 (6)C40—H40A0.9300
C9—H9A0.9300C41—C421.393 (4)
C10—C111.368 (5)C42—C431.392 (4)
C10—H10A0.9300C42—H42A0.9300
C11—C121.392 (4)C43—H43A0.9300
C11—H11A0.9300C53—H53A0.9600
C12—H12A0.9300C53—H53B0.9600
C13—H13A0.9700C53—H53C0.9600
C45—Ru1—C4690.51 (13)C15—C14—C19119.4 (2)
C45—Ru1—C4493.36 (13)C15—C14—As2123.0 (2)
C46—Ru1—C44175.24 (11)C19—C14—As2117.54 (19)
C45—Ru1—As1100.13 (9)C14—C15—C16120.0 (3)
C46—Ru1—As190.28 (8)C14—C15—H15A120.0
C44—Ru1—As191.78 (8)C16—C15—H15A120.0
C45—Ru1—Ru2165.84 (10)C17—C16—C15120.1 (3)
C46—Ru1—Ru282.08 (8)C17—C16—H16A120.0
C44—Ru1—Ru293.56 (8)C15—C16—H16A120.0
As1—Ru1—Ru291.991 (10)C16—C17—C18119.8 (3)
C45—Ru1—Ru3110.76 (9)C16—C17—H17A120.1
C46—Ru1—Ru3101.44 (8)C18—C17—H17A120.1
C44—Ru1—Ru374.58 (8)C17—C18—C19120.5 (3)
As1—Ru1—Ru3146.643 (11)C17—C18—H18A119.7
Ru2—Ru1—Ru359.519 (7)C19—C18—H18A119.7
C48—Ru2—C4990.79 (12)C18—C19—C14120.1 (2)
C48—Ru2—C4790.92 (12)C18—C19—H19A120.0
C49—Ru2—C47176.61 (11)C14—C19—H19A120.0
C48—Ru2—As2104.59 (8)C21—C20—C25119.6 (3)
C49—Ru2—As289.66 (8)C21—C20—As2119.9 (2)
C47—Ru2—As292.75 (8)C25—C20—As2120.5 (2)
C48—Ru2—Ru3100.01 (8)C20—C21—C22120.3 (3)
C49—Ru2—Ru390.21 (8)C20—C21—H21A119.8
C47—Ru2—Ru386.61 (7)C22—C21—H21A119.8
As2—Ru2—Ru3155.395 (11)C23—C22—C21120.1 (3)
C48—Ru2—Ru1159.76 (8)C23—C22—H22A120.0
C49—Ru2—Ru184.66 (8)C21—C22—H22A120.0
C47—Ru2—Ru192.74 (8)C24—C23—C22119.9 (3)
As2—Ru2—Ru195.117 (10)C24—C23—H23A120.1
Ru3—Ru2—Ru160.388 (8)C22—C23—H23A120.1
C51—Ru3—C5299.57 (12)C23—C24—C25119.9 (3)
C51—Ru3—C5092.14 (12)C23—C24—H24A120.0
C52—Ru3—C50168.17 (12)C25—C24—H24A120.0
C51—Ru3—P199.62 (8)C20—C25—C24120.1 (3)
C52—Ru3—P187.27 (8)C20—C25—H25A119.9
C50—Ru3—P192.44 (8)C24—C25—H25A119.9
C51—Ru3—Ru286.81 (8)C27—C26—C31118.7 (3)
C52—Ru3—Ru290.79 (7)C27—C26—P1117.8 (2)
C50—Ru3—Ru288.19 (8)C31—C26—P1123.4 (3)
P1—Ru3—Ru2173.506 (19)C26—C27—C28121.3 (3)
C51—Ru3—Ru1144.16 (8)C26—C27—H27A119.3
C52—Ru3—Ru169.84 (8)C28—C27—H27A119.3
C50—Ru3—Ru199.57 (8)C29—C28—C27119.8 (4)
P1—Ru3—Ru1113.452 (19)C29—C28—H28A120.1
Ru2—Ru3—Ru160.093 (7)C27—C28—H28A120.1
C1—As1—C7103.01 (12)C30—C29—C28119.6 (3)
C1—As1—C13104.72 (12)C30—C29—H29A120.2
C7—As1—C1398.63 (11)C28—C29—H29A120.2
C1—As1—Ru1116.68 (9)C29—C30—C31121.1 (3)
C7—As1—Ru1117.57 (8)C29—C30—H30A119.5
C13—As1—Ru1113.89 (8)C31—C30—H30A119.5
C20—As2—C14102.46 (11)C26—C31—C30119.5 (4)
C20—As2—C13101.54 (11)C26—C31—H31A120.2
C14—As2—C13104.34 (11)C30—C31—H31A120.2
C20—As2—Ru2116.43 (7)C37—C32—C33119.1 (3)
C14—As2—Ru2115.44 (8)C37—C32—P1121.2 (2)
C13—As2—Ru2114.74 (7)C33—C32—P1119.4 (2)
C41—S1—C53105.61 (15)C34—C33—C32119.9 (3)
C32—P1—C38103.11 (12)C34—C33—H33A120.1
C32—P1—C26105.57 (13)C32—C33—H33A120.1
C38—P1—C26101.02 (12)C35—C34—C33120.2 (3)
C32—P1—Ru3113.81 (9)C35—C34—H34A119.9
C38—P1—Ru3115.89 (8)C33—C34—H34A119.9
C26—P1—Ru3115.78 (9)C36—C35—C34120.2 (3)
C2—C1—C6119.4 (3)C36—C35—H35A119.9
C2—C1—As1122.1 (2)C34—C35—H35A119.9
C6—C1—As1118.5 (3)C35—C36—C37120.2 (3)
C1—C2—C3120.2 (3)C35—C36—H36A119.9
C1—C2—H2A119.9C37—C36—H36A119.9
C3—C2—H2A119.9C36—C37—C32120.3 (3)
C4—C3—C2120.8 (4)C36—C37—H37A119.9
C4—C3—H3A119.6C32—C37—H37A119.9
C2—C3—H3A119.6C39—C38—C43117.6 (2)
C3—C4—C5119.8 (4)C39—C38—P1121.46 (19)
C3—C4—H4A120.1C43—C38—P1120.9 (2)
C5—C4—H4A120.1C40—C39—C38121.5 (2)
C4—C5—C6120.7 (4)C40—C39—H39A119.3
C4—C5—H5A119.7C38—C39—H39A119.3
C6—C5—H5A119.7C39—C40—C41120.6 (2)
C5—C6—C1119.1 (4)C39—C40—H40A119.7
C5—C6—H6A120.5C41—C40—H40A119.7
C1—C6—H6A120.5C42—C41—C40118.8 (2)
C8—C7—C12119.1 (3)C42—C41—S1125.7 (2)
C8—C7—As1123.3 (2)C40—C41—S1115.5 (2)
C12—C7—As1117.6 (2)C43—C42—C41120.1 (2)
C7—C8—C9120.0 (3)C43—C42—H42A119.9
C7—C8—H8A120.0C41—C42—H42A119.9
C9—C8—H8A120.0C42—C43—C38121.4 (2)
C10—C9—C8120.4 (3)C42—C43—H43A119.3
C10—C9—H9A119.8C38—C43—H43A119.3
C8—C9—H9A119.8O1—C44—Ru1170.4 (2)
C11—C10—C9119.7 (3)O2—C45—Ru1175.3 (3)
C11—C10—H10A120.2O3—C46—Ru1173.1 (2)
C9—C10—H10A120.2O4—C47—Ru2174.8 (2)
C10—C11—C12120.0 (3)O5—C48—Ru2177.1 (3)
C10—C11—H11A120.0O6—C49—Ru2172.8 (2)
C12—C11—H11A120.0O7—C50—Ru3175.4 (2)
C7—C12—C11120.7 (3)O8—C51—Ru3176.4 (2)
C7—C12—H12A119.6O9—C52—Ru3168.7 (2)
C11—C12—H12A119.6S1—C53—H53A109.5
As1—C13—As2112.81 (12)S1—C53—H53B109.5
As1—C13—H13A109.0H53A—C53—H53B109.5
As2—C13—H13A109.0S1—C53—H53C109.5
As1—C13—H13B109.0H53A—C53—H53C109.5
As2—C13—H13B109.0H53B—C53—H53C109.5
H13A—C13—H13B107.8
C45—Ru1—Ru2—C4864.9 (5)Ru1—As1—C1—C2−108.3 (2)
C46—Ru1—Ru2—C48123.9 (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—C668.2 (3)
Ru3—Ru1—Ru2—C4815.6 (3)C6—C1—C2—C30.4 (5)
C45—Ru1—Ru2—C49142.6 (4)As1—C1—C2—C3176.9 (3)
C46—Ru1—Ru2—C49−158.40 (11)C1—C2—C3—C41.8 (6)
C44—Ru1—Ru2—C4923.51 (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—C4993.29 (8)C4—C5—C6—C12.5 (6)
C45—Ru1—Ru2—C47−35.2 (4)C2—C1—C6—C5−2.5 (5)
C46—Ru1—Ru2—C4723.78 (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—C47113.78 (8)C13—As1—C7—C8103.9 (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—C12177.4 (2)
C46—Ru1—Ru2—As2−69.22 (8)C13—As1—C7—C12−75.2 (2)
C44—Ru1—Ru2—As2112.68 (8)Ru1—As1—C7—C1247.5 (2)
As1—Ru1—Ru2—As220.778 (12)C12—C7—C8—C9−1.5 (5)
Ru3—Ru1—Ru2—As2−177.538 (11)As1—C7—C8—C9179.4 (3)
C45—Ru1—Ru2—Ru349.3 (4)C7—C8—C9—C102.0 (6)
C46—Ru1—Ru2—Ru3108.32 (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—C5119.80 (13)As1—C7—C12—C11178.4 (2)
C49—Ru2—Ru3—C51110.64 (12)C10—C11—C12—C72.7 (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—As2160.20 (14)
Ru1—Ru2—Ru3—C51−165.63 (9)Ru1—As1—C13—As234.79 (15)
C48—Ru2—Ru3—C52119.35 (12)C20—As2—C13—As1−141.11 (13)
C49—Ru2—Ru3—C52−149.81 (11)C14—As2—C13—As1112.66 (14)
C47—Ru2—Ru3—C5229.01 (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—C1520.4 (2)
C48—Ru2—Ru3—C50−72.44 (13)Ru2—As2—C14—C15147.2 (2)
C49—Ru2—Ru3—C5018.40 (12)C20—As2—C14—C1994.7 (2)
C47—Ru2—Ru3—C50−162.78 (12)C13—As2—C14—C19−159.7 (2)
As2—Ru2—Ru3—C50108.03 (9)Ru2—As2—C14—C19−32.9 (2)
Ru1—Ru2—Ru3—C50102.13 (9)C19—C14—C15—C162.8 (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—Ru195.09 (8)C15—C16—C17—C180.0 (5)
As2—Ru2—Ru3—Ru15.90 (3)C16—C17—C18—C193.1 (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—C180.2 (4)
C44—Ru1—Ru3—C51128.75 (17)As2—C14—C19—C18−179.7 (2)
As1—Ru1—Ru3—C5159.88 (15)C14—As2—C20—C21−25.6 (3)
Ru2—Ru1—Ru3—C5125.04 (15)C13—As2—C20—C21−133.3 (2)
C45—Ru1—Ru3—C52−65.38 (13)Ru2—As2—C20—C21101.4 (2)
C46—Ru1—Ru3—C5229.57 (11)C14—As2—C20—C25156.1 (2)
C44—Ru1—Ru3—C52−153.11 (12)C13—As2—C20—C2548.4 (3)
As1—Ru1—Ru3—C52138.01 (8)Ru2—As2—C20—C25−76.9 (2)
Ru2—Ru1—Ru3—C52103.18 (8)C25—C20—C21—C221.6 (5)
C45—Ru1—Ru3—C50109.14 (14)As2—C20—C21—C22−176.8 (3)
C46—Ru1—Ru3—C50−155.90 (12)C20—C21—C22—C230.0 (6)
C44—Ru1—Ru3—C5021.41 (12)C21—C22—C23—C24−2.1 (6)
As1—Ru1—Ru3—C50−47.46 (9)C22—C23—C24—C252.6 (6)
Ru2—Ru1—Ru3—C50−82.30 (9)C21—C20—C25—C24−1.0 (5)
C45—Ru1—Ru3—P112.24 (11)As2—C20—C25—C24177.3 (3)
C46—Ru1—Ru3—P1107.19 (8)C23—C24—C25—C20−1.0 (5)
C44—Ru1—Ru3—P1−75.49 (9)C32—P1—C26—C27171.3 (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—C2744.4 (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—C3195.2 (3)
C44—Ru1—Ru3—Ru2103.71 (8)Ru3—P1—C26—C31−138.8 (2)
As1—Ru1—Ru3—Ru234.83 (2)C31—C26—C27—C280.9 (5)
C45—Ru1—As1—C1−98.91 (14)P1—C26—C27—C28177.9 (3)
C46—Ru1—As1—C1170.52 (12)C26—C27—C28—C290.5 (5)
C44—Ru1—As1—C1−5.19 (13)C27—C28—C29—C30−1.6 (6)
Ru2—Ru1—As1—C188.44 (10)C28—C29—C30—C311.2 (6)
Ru3—Ru1—As1—C158.93 (10)C27—C26—C31—C30−1.3 (5)
C45—Ru1—As1—C724.23 (14)P1—C26—C31—C30−178.1 (3)
C46—Ru1—As1—C7−66.34 (12)C29—C30—C31—C260.3 (6)
C44—Ru1—As1—C7117.95 (12)C38—P1—C32—C3725.6 (3)
Ru2—Ru1—As1—C7−148.42 (9)C26—P1—C32—C37131.2 (2)
Ru3—Ru1—As1—C7−177.93 (9)Ru3—P1—C32—C37−100.8 (2)
C45—Ru1—As1—C13138.84 (13)C38—P1—C32—C33−160.9 (2)
C46—Ru1—As1—C1348.28 (12)C26—P1—C32—C33−55.3 (2)
C44—Ru1—As1—C13−127.43 (12)Ru3—P1—C32—C3372.7 (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—C351.7 (5)
C49—Ru2—As2—C20−164.28 (12)C33—C34—C35—C36−1.1 (5)
C47—Ru2—As2—C2018.12 (12)C34—C35—C36—C370.3 (5)
Ru3—Ru2—As2—C20105.97 (9)C35—C36—C37—C32−0.2 (5)
Ru1—Ru2—As2—C20111.12 (9)C33—C32—C37—C360.8 (4)
C48—Ru2—As2—C1446.67 (13)P1—C32—C37—C36174.3 (2)
C49—Ru2—As2—C14−44.06 (11)C32—P1—C38—C39−132.6 (2)
C47—Ru2—As2—C14138.34 (11)C26—P1—C38—C39118.4 (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—C4347.5 (3)
C48—Ru2—As2—C13168.08 (13)C26—P1—C38—C43−61.5 (3)
C49—Ru2—As2—C1377.35 (12)Ru3—P1—C38—C43172.5 (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—C40179.7 (2)
Ru1—Ru2—As2—C13−7.25 (9)C38—C39—C40—C41−1.1 (4)
C51—Ru3—P1—C32164.97 (14)C39—C40—C41—C421.0 (4)
C52—Ru3—P1—C3265.71 (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—C40175.6 (2)
C51—Ru3—P1—C3845.64 (13)C40—C41—C42—C430.7 (4)
C52—Ru3—P1—C38−53.62 (13)S1—C41—C42—C43−179.2 (2)
C50—Ru3—P1—C38138.22 (13)C41—C42—C43—C38−2.3 (5)
Ru1—Ru3—P1—C38−120.25 (10)C39—C38—C43—C422.1 (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—C2620.16 (13)C50—Ru3—C52—O9127.4 (11)
Ru1—Ru3—P1—C26121.69 (10)P1—Ru3—C52—O938.5 (12)
C7—As1—C1—C2121.3 (3)Ru2—Ru3—C52—O9−147.7 (12)
C13—As1—C1—C218.6 (3)Ru1—Ru3—C52—O9154.8 (12)
Cg1, Cg2 and Cg3 are the centroids of the C7–C12, C38–C43 and C14–C19 benzene rings, respectively.
D—H···AD—HH···AD···AD—H···A
C4—H4A···O6i0.932.483.278 (6)144
C24—H24A···O7ii0.932.563.259 (5)132
C42—H42A···O1iii0.932.573.414 (5)151
C30—H30A···Cg1iii0.933.003.890 (6)161
C34—H34A···Cg2iv0.932.893.785 (4)163
C40—H40A···Cg3v0.932.883.672 (4)144
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⋯AD—HH⋯ADAD—H⋯A
C4—H4A⋯O6i0.932.483.278 (6)144
C24—H24A⋯O7ii0.932.563.259 (5)132
C42—H42A⋯O1iii0.932.573.414 (5)151
C30—H30ACg1iii0.933.003.890 (6)161
C34—H34ACg2iv0.932.893.785 (4)163
C40—H40ACg3v0.932.883.672 (4)144

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

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1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Bis{[μ-bis-(diphenyl-arsino)methane-1:2κAs:As']nona-carbonyl-1κC,2κC,3κC-[tris-(4-methoxy-phen-yl)arsine-3κAs]-triangulo-triruthenium(0)} dichloro-methane solvate.

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; Chin Sing Yeap; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-01-16

3.  Bis{[μ-bis-(diphenyl-phosphino)methane-1:2κP:P']nona-carbonyl-1κC,2κC,3κC-[tris-(4-methoxy-phen-yl)arsine-3κAs]-triangulo-triruthenium(0)} dichloro-methane solvate.

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; Chin Sing Yeap; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-12-09

4.  Structure validation in chemical crystallography.

Authors:  Anthony L Spek
Journal:  Acta Crystallogr D Biol Crystallogr       Date:  2009-01-20
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1.  Undeca-carbon-yl[(4-methyl-sulfanylphen-yl)di-phenyl-phosphane]triruthenium(0): crystal structure and Hirshfeld surface analysis.

Authors:  Omar Bin Shawkataly; Hafiz Malik Hussien Abdelnasir; Siti Syaida Sirat; Mukesh M Jotani; Edward R T Tiekink
Journal:  Acta Crystallogr E Crystallogr Commun       Date:  2018-05-15
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