Literature DB >> 21579984

[μ-Bis(diphenyl-arsino)methane-1:2κAs:As']nona-carbonyl-1κC,2κC,3κC-[triphenyl-stibine-3κSb]-triangulo-triruthenium(0).

Omar Bin Shawkataly, Imthyaz Ahmed Khan, Chin Sing Yeap, Hoong-Kun Fun.   

Abstract

In the title triangulo-triruthenium compound, [Ru(3)(C(25)H(22)As(2))(C(18)H(15)Sb)(CO)(9)], the bis-(diphenyl-arsino)methane ligand bridges an Ru-Ru bond and the monodentate stibine ligand bonds to the third Ru atom. Both the stibine and arsine ligands are equatorial with respect to the Ru(3) triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three stibine-substituted phenyl rings make dihedral angles of 84.3 (3), 80.4 (3) and 70.5 (3)° with each other. The dihedral angles between the two phenyl rings are 85.9 (3) and 75.2 (3)° for the two diphenyl-arsine groups. In the crystal packing, mol-ecules are linked into chains down the c axis via inter-molecular C-H⋯O hydrogen bonds. Weak inter-molecular C-H⋯π inter-actions further stabilize the crystal structure.

Entities:  

Year:  2009        PMID: 21579984      PMCID: PMC2980229          DOI: 10.1107/S1600536809049927

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 ▶); Shawkataly et al. (1998 ▶, 2004 ▶, 2009 ▶). For related structures, see: Shawkataly et al. (2009 ▶). For the synthesis of μ-bis­(diphenylarsino)methanedecacarbonyl­triruthenium(0), see: Bruce et al. (1983 ▶). For the stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986 ▶).

Experimental

Crystal data

[Ru3(C25H22As2)(C18H15Sb)(CO)9] M = 1380.62 Monoclinic, a = 42.3464 (6) Å b = 11.6246 (2) Å c = 20.1185 (3) Å β = 91.823 (1)° V = 9898.5 (3) Å3 Z = 8 Mo Kα radiation μ = 2.82 mm−1 T = 100 K 0.36 × 0.15 × 0.09 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer Absorption correction: multi-scan (; Bruker, 2005 ▶) T min = 0.428, T max = 0.796 55374 measured reflections 11349 independent reflections 8669 reflections with I > 2σ(I) R int = 0.042

Refinement

R[F 2 > 2σ(F 2)] = 0.037 wR(F 2) = 0.096 S = 1.08 11349 reflections 605 parameters H-atom parameters constrained Δρmax = 1.45 e Å−3 Δρmin = −1.24 e Å−3 Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT (Bruker, 2005 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809049927/sj2682sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809049927/sj2682Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ru3(C25H22As2)(C18H15Sb)(CO)9]F(000) = 5360
Mr = 1380.62Dx = 1.853 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 9674 reflections
a = 42.3464 (6) Åθ = 2.3–30.6°
b = 11.6246 (2) ŵ = 2.82 mm1
c = 20.1185 (3) ÅT = 100 K
β = 91.823 (1)°Block, red
V = 9898.5 (3) Å30.36 × 0.15 × 0.09 mm
Z = 8
Bruker SMART APEXII CCD area-detector diffractometer11349 independent reflections
Radiation source: fine-focus sealed tube8669 reflections with I > 2σ(I)
graphiteRint = 0.042
φ and ω scansθmax = 27.5°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2005)h = −54→50
Tmin = 0.428, Tmax = 0.796k = −14→15
55374 measured reflectionsl = −25→26
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.096H-atom parameters constrained
S = 1.08w = 1/[σ2(Fo2) + (0.027P)2 + 103.4772P] where P = (Fo2 + 2Fc2)/3
11349 reflections(Δ/σ)max = 0.001
605 parametersΔρmax = 1.45 e Å3
0 restraintsΔρmin = −1.24 e Å3
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.
xyzUiso*/Ueq
Sb10.084142 (8)0.82926 (3)0.122293 (17)0.02485 (8)
Ru10.111861 (9)0.69580 (3)−0.05368 (2)0.02414 (10)
Ru20.173966 (9)0.62369 (3)−0.01095 (2)0.02287 (9)
Ru30.132574 (9)0.71467 (3)0.08382 (2)0.02524 (10)
As10.124706 (12)0.65958 (4)−0.16939 (3)0.02403 (11)
As20.185533 (11)0.52317 (4)−0.11339 (3)0.02262 (11)
O10.04220 (10)0.7484 (5)−0.0798 (2)0.0569 (13)
O20.09819 (10)0.4372 (3)−0.0433 (2)0.0431 (10)
O30.12504 (9)0.9554 (3)−0.04611 (18)0.0311 (8)
O40.15850 (10)0.3916 (3)0.0537 (2)0.0409 (10)
O50.23787 (10)0.6078 (4)0.0599 (2)0.0491 (11)
O60.19089 (9)0.8586 (3)−0.0700 (2)0.0355 (9)
O70.09752 (10)0.4866 (3)0.1062 (2)0.0467 (11)
O80.16762 (9)0.6817 (4)0.2157 (2)0.0432 (10)
O90.17354 (9)0.9301 (3)0.06805 (19)0.0338 (9)
C10.08858 (12)0.6283 (4)−0.2287 (3)0.0268 (11)
C20.07734 (14)0.7137 (5)−0.2713 (3)0.0382 (13)
H2A0.08870.7816−0.27530.046*
C30.04930 (15)0.6994 (5)−0.3082 (3)0.0422 (15)
H3A0.04160.7582−0.33560.051*
C40.03303 (14)0.5975 (6)−0.3038 (3)0.0388 (14)
H4A0.01430.5876−0.32840.047*
C50.04410 (13)0.5110 (5)−0.2639 (3)0.0398 (14)
H5A0.03320.4417−0.26220.048*
C60.07193 (13)0.5261 (5)−0.2253 (3)0.0341 (13)
H6A0.07920.4673−0.19750.041*
C70.14865 (12)0.7655 (5)−0.2226 (3)0.0279 (11)
C80.14999 (14)0.8819 (5)−0.2059 (3)0.0351 (13)
H8A0.13930.9089−0.16930.042*
C90.16728 (15)0.9577 (5)−0.2442 (3)0.0400 (14)
H9A0.16791.0354−0.23340.048*
C100.18329 (14)0.9184 (5)−0.2973 (3)0.0374 (14)
H10A0.19570.9689−0.32120.045*
C110.18129 (15)0.8051 (6)−0.3158 (3)0.0441 (15)
H11A0.19140.7796−0.35340.053*
C120.16402 (14)0.7281 (5)−0.2780 (3)0.0367 (13)
H12A0.16290.6511−0.29030.044*
C130.14903 (12)0.5166 (4)−0.1756 (3)0.0268 (11)
H13A0.13580.4515−0.16490.032*
H13B0.15610.5068−0.22060.032*
C140.19684 (12)0.3618 (4)−0.1015 (3)0.0259 (11)
C150.17403 (14)0.2789 (5)−0.0939 (4)0.0428 (15)
H15A0.15280.2983−0.09890.051*
C160.18254 (15)0.1664 (5)−0.0788 (4)0.0462 (16)
H16A0.16700.1107−0.07470.055*
C170.21371 (15)0.1370 (5)−0.0699 (3)0.0377 (13)
H17A0.21930.0617−0.05910.045*
C180.23675 (14)0.2198 (5)−0.0770 (3)0.0353 (13)
H18A0.25790.2003−0.07110.042*
C190.22837 (12)0.3321 (4)−0.0930 (3)0.0297 (11)
H19A0.24400.3874−0.09800.036*
C200.21906 (11)0.5759 (4)−0.1697 (3)0.0238 (10)
C210.22437 (12)0.5219 (5)−0.2302 (3)0.0311 (12)
H21A0.21230.4584−0.24310.037*
C220.24741 (12)0.5623 (5)−0.2708 (3)0.0317 (12)
H22A0.25090.5258−0.31100.038*
C230.26547 (12)0.6576 (5)−0.2520 (3)0.0324 (12)
H23A0.28070.6860−0.28000.039*
C240.26066 (12)0.7096 (5)−0.1917 (3)0.0327 (12)
H24A0.27300.7724−0.17860.039*
C250.23753 (12)0.6687 (4)−0.1502 (3)0.0285 (11)
H25A0.23450.7039−0.10940.034*
C260.08319 (14)0.8791 (5)0.2245 (3)0.0362 (13)
C270.06664 (18)0.9775 (6)0.2432 (3)0.0527 (18)
H27A0.05801.02500.21010.063*
C280.0626 (2)1.0070 (6)0.3096 (4)0.062 (2)
H28A0.05131.07220.32090.074*
C290.07591 (19)0.9367 (8)0.3582 (4)0.062 (2)
H29A0.07320.95410.40270.074*
C300.09304 (15)0.8420 (8)0.3418 (3)0.060 (2)
H30A0.10250.79740.37520.072*
C310.09648 (14)0.8112 (7)0.2746 (3)0.0491 (17)
H31A0.10770.74530.26390.059*
C320.03824 (12)0.7518 (4)0.1172 (3)0.0266 (11)
C330.01478 (13)0.7924 (5)0.1571 (3)0.0355 (13)
H33A0.01880.85550.18450.043*
C34−0.01436 (13)0.7407 (5)0.1569 (3)0.0391 (14)
H34A−0.02990.76780.18460.047*
C35−0.02059 (13)0.6480 (6)0.1154 (3)0.0424 (15)
H35A−0.04060.61460.11390.051*
C360.00261 (16)0.6057 (6)0.0767 (3)0.0480 (17)
H36A−0.00140.54130.05030.058*
C370.03201 (13)0.6578 (5)0.0764 (3)0.0350 (13)
H37A0.04750.62990.04890.042*
C380.07462 (13)0.9943 (4)0.0789 (3)0.0278 (11)
C390.04575 (14)1.0187 (5)0.0475 (3)0.0376 (14)
H39A0.03010.96240.04430.045*
C400.04024 (16)1.1274 (5)0.0207 (3)0.0445 (15)
H40A0.02081.14430.00010.053*
C410.06361 (15)1.2100 (5)0.0246 (3)0.0416 (14)
H41A0.06011.28210.00580.050*
C420.09210 (14)1.1861 (5)0.0562 (3)0.0377 (14)
H42A0.10771.24230.05910.045*
C430.09760 (13)1.0786 (5)0.0837 (3)0.0328 (12)
H43A0.11681.06290.10550.039*
C440.06855 (14)0.7302 (5)−0.0681 (3)0.0366 (13)
C450.10430 (13)0.5344 (5)−0.0440 (3)0.0335 (12)
C460.12143 (12)0.8580 (5)−0.0476 (3)0.0281 (11)
C470.16233 (13)0.4801 (5)0.0298 (3)0.0313 (12)
C480.21364 (13)0.6139 (5)0.0330 (3)0.0320 (12)
C490.18295 (12)0.7728 (4)−0.0483 (3)0.0274 (11)
C500.11020 (13)0.5703 (5)0.0947 (3)0.0360 (13)
C510.15435 (12)0.6939 (5)0.1651 (3)0.0312 (12)
C520.15780 (13)0.8488 (5)0.0705 (3)0.0290 (11)
U11U22U33U12U13U23
Sb10.02101 (17)0.02523 (17)0.02838 (18)−0.00263 (13)0.00167 (13)0.00197 (14)
Ru10.0184 (2)0.0245 (2)0.0297 (2)−0.00163 (15)0.00413 (16)0.00320 (16)
Ru20.01783 (19)0.02012 (19)0.0308 (2)−0.00182 (15)0.00339 (16)−0.00040 (16)
Ru30.0209 (2)0.0246 (2)0.0304 (2)−0.00150 (16)0.00461 (16)0.00228 (17)
As10.0213 (3)0.0211 (2)0.0299 (3)−0.00367 (19)0.0037 (2)0.0000 (2)
As20.0189 (2)0.0165 (2)0.0326 (3)−0.00326 (18)0.0048 (2)−0.0012 (2)
O10.027 (2)0.087 (4)0.057 (3)0.008 (2)0.003 (2)0.015 (3)
O20.043 (2)0.032 (2)0.054 (3)−0.0134 (18)−0.001 (2)0.0059 (19)
O30.038 (2)0.0244 (19)0.031 (2)0.0034 (16)0.0047 (17)0.0020 (15)
O40.042 (2)0.030 (2)0.052 (3)−0.0002 (18)0.011 (2)0.0113 (19)
O50.033 (2)0.046 (3)0.068 (3)0.0054 (19)−0.014 (2)−0.013 (2)
O60.028 (2)0.0215 (19)0.057 (3)−0.0020 (15)0.0103 (18)0.0024 (17)
O70.051 (3)0.027 (2)0.064 (3)−0.0077 (19)0.024 (2)0.002 (2)
O80.031 (2)0.053 (3)0.046 (3)−0.0016 (19)−0.0013 (19)0.020 (2)
O90.039 (2)0.0269 (19)0.035 (2)−0.0100 (17)0.0042 (17)−0.0029 (16)
C10.023 (3)0.027 (3)0.031 (3)−0.003 (2)0.006 (2)−0.004 (2)
C20.041 (3)0.032 (3)0.041 (3)−0.008 (3)0.000 (3)0.001 (3)
C30.041 (3)0.042 (3)0.043 (4)−0.010 (3)−0.010 (3)0.009 (3)
C40.029 (3)0.054 (4)0.033 (3)−0.008 (3)−0.004 (2)−0.002 (3)
C50.031 (3)0.037 (3)0.051 (4)−0.012 (2)0.000 (3)0.001 (3)
C60.030 (3)0.032 (3)0.041 (3)−0.009 (2)0.002 (2)0.005 (2)
C70.024 (3)0.030 (3)0.030 (3)−0.005 (2)0.003 (2)0.002 (2)
C80.046 (3)0.030 (3)0.031 (3)−0.009 (2)0.011 (3)−0.004 (2)
C90.049 (4)0.031 (3)0.041 (3)−0.016 (3)0.006 (3)−0.001 (3)
C100.037 (3)0.042 (3)0.033 (3)−0.014 (3)0.000 (3)0.012 (3)
C110.044 (4)0.047 (4)0.042 (4)0.006 (3)0.019 (3)0.006 (3)
C120.041 (3)0.032 (3)0.038 (3)0.000 (2)0.010 (3)−0.001 (2)
C130.024 (3)0.020 (2)0.036 (3)−0.0026 (19)0.000 (2)−0.005 (2)
C140.028 (3)0.020 (2)0.030 (3)−0.002 (2)0.006 (2)−0.002 (2)
C150.029 (3)0.024 (3)0.076 (5)−0.002 (2)0.002 (3)0.002 (3)
C160.041 (4)0.023 (3)0.075 (5)−0.012 (3)0.002 (3)0.003 (3)
C170.051 (4)0.021 (3)0.041 (3)0.001 (2)0.002 (3)−0.002 (2)
C180.036 (3)0.032 (3)0.037 (3)0.006 (2)0.003 (3)0.001 (2)
C190.028 (3)0.023 (2)0.039 (3)−0.002 (2)0.006 (2)0.000 (2)
C200.019 (2)0.016 (2)0.036 (3)−0.0029 (18)0.003 (2)0.002 (2)
C210.027 (3)0.026 (3)0.040 (3)−0.005 (2)0.003 (2)−0.003 (2)
C220.027 (3)0.035 (3)0.034 (3)0.001 (2)0.005 (2)−0.001 (2)
C230.024 (3)0.027 (3)0.046 (3)−0.001 (2)0.008 (2)0.005 (2)
C240.024 (3)0.027 (3)0.048 (3)−0.004 (2)0.010 (2)−0.001 (2)
C250.023 (3)0.023 (2)0.040 (3)−0.001 (2)0.005 (2)−0.004 (2)
C260.036 (3)0.045 (3)0.028 (3)−0.017 (3)0.000 (2)0.004 (3)
C270.081 (5)0.040 (4)0.038 (4)−0.012 (3)0.011 (3)−0.005 (3)
C280.100 (6)0.042 (4)0.044 (4)−0.016 (4)0.014 (4)−0.009 (3)
C290.061 (5)0.086 (6)0.038 (4)−0.034 (5)0.001 (3)−0.013 (4)
C300.025 (3)0.116 (7)0.037 (4)−0.010 (4)−0.004 (3)0.026 (4)
C310.022 (3)0.081 (5)0.044 (4)0.002 (3)0.001 (3)0.010 (3)
C320.027 (3)0.024 (2)0.030 (3)−0.003 (2)0.001 (2)0.010 (2)
C330.027 (3)0.032 (3)0.048 (4)0.004 (2)0.001 (3)0.001 (3)
C340.025 (3)0.041 (3)0.052 (4)0.006 (2)0.008 (3)0.005 (3)
C350.021 (3)0.061 (4)0.044 (4)−0.013 (3)−0.005 (3)0.017 (3)
C360.049 (4)0.062 (4)0.033 (3)−0.026 (3)0.003 (3)−0.008 (3)
C370.032 (3)0.041 (3)0.033 (3)−0.007 (2)0.010 (2)−0.004 (2)
C380.032 (3)0.025 (3)0.027 (3)−0.002 (2)0.005 (2)0.002 (2)
C390.042 (3)0.034 (3)0.037 (3)−0.015 (3)−0.008 (3)0.010 (2)
C400.047 (4)0.041 (3)0.044 (4)−0.008 (3)−0.015 (3)0.014 (3)
C410.053 (4)0.031 (3)0.041 (3)−0.007 (3)0.000 (3)0.007 (3)
C420.039 (3)0.029 (3)0.046 (4)−0.012 (2)0.009 (3)−0.002 (3)
C430.025 (3)0.026 (3)0.047 (3)−0.002 (2)0.003 (2)−0.003 (2)
C440.029 (3)0.045 (3)0.037 (3)0.003 (3)0.007 (2)0.006 (3)
C450.025 (3)0.039 (3)0.036 (3)−0.009 (2)0.000 (2)0.002 (2)
C460.023 (3)0.035 (3)0.026 (3)0.001 (2)0.003 (2)0.000 (2)
C470.030 (3)0.027 (3)0.037 (3)0.002 (2)0.004 (2)0.001 (2)
C480.030 (3)0.027 (3)0.039 (3)0.001 (2)0.000 (2)−0.008 (2)
C490.018 (2)0.028 (3)0.036 (3)0.000 (2)0.006 (2)−0.003 (2)
C500.031 (3)0.030 (3)0.048 (4)0.003 (2)0.014 (3)0.000 (3)
C510.020 (3)0.036 (3)0.038 (3)0.003 (2)0.003 (2)0.013 (2)
C520.032 (3)0.030 (3)0.025 (3)0.010 (2)−0.001 (2)−0.003 (2)
Sb1—C262.138 (6)C13—H13B0.9700
Sb1—C382.141 (5)C14—C151.377 (7)
Sb1—C322.142 (5)C14—C191.385 (7)
Sb1—Ru32.5847 (5)C15—C161.387 (8)
Ru1—C441.891 (6)C15—H15A0.9300
Ru1—C451.914 (6)C16—C171.370 (9)
Ru1—C461.932 (6)C16—H16A0.9300
Ru1—As12.4439 (7)C17—C181.382 (8)
Ru1—Ru22.8661 (6)C17—H17A0.9300
Ru1—Ru32.8838 (6)C18—C191.387 (7)
Ru2—C481.876 (6)C18—H18A0.9300
Ru2—C471.930 (5)C19—H19A0.9300
Ru2—C491.932 (5)C20—C251.382 (7)
Ru2—As22.4325 (6)C20—C211.394 (7)
Ru2—Ru32.8354 (6)C21—C221.375 (7)
Ru3—C511.866 (6)C21—H21A0.9300
Ru3—C521.914 (6)C22—C231.392 (7)
Ru3—C501.942 (6)C22—H22A0.9300
As1—C71.939 (5)C23—C241.377 (8)
As1—C11.944 (5)C23—H23A0.9300
As1—C131.961 (5)C24—C251.390 (7)
As2—C201.943 (5)C24—H24A0.9300
As2—C141.948 (5)C25—H25A0.9300
As2—C131.959 (5)C26—C311.385 (9)
O1—C441.153 (7)C26—C271.399 (9)
O2—C451.160 (7)C27—C281.396 (9)
O3—C461.143 (6)C27—H27A0.9300
O4—C471.150 (6)C28—C291.380 (11)
O5—C481.148 (6)C28—H28A0.9300
O6—C491.143 (6)C29—C301.364 (11)
O7—C501.139 (7)C29—H29A0.9300
O8—C511.156 (7)C30—C311.411 (10)
O9—C521.158 (6)C30—H30A0.9300
C1—C61.385 (7)C31—H31A0.9300
C1—C21.386 (8)C32—C331.380 (8)
C2—C31.391 (8)C32—C371.387 (7)
C2—H2A0.9300C33—C341.373 (8)
C3—C41.374 (8)C33—H33A0.9300
C3—H3A0.9300C34—C351.382 (9)
C4—C51.361 (8)C34—H34A0.9300
C4—H4A0.9300C35—C361.364 (9)
C5—C61.401 (8)C35—H35A0.9300
C5—H5A0.9300C36—C371.385 (8)
C6—H6A0.9300C36—H36A0.9300
C7—C121.379 (8)C37—H37A0.9300
C7—C81.395 (7)C38—C431.382 (7)
C8—C91.393 (7)C38—C391.388 (8)
C8—H8A0.9300C39—C401.391 (8)
C9—C101.362 (8)C39—H39A0.9300
C9—H9A0.9300C40—C411.380 (8)
C10—C111.371 (9)C40—H40A0.9300
C10—H10A0.9300C41—C421.374 (9)
C11—C121.396 (8)C41—H41A0.9300
C11—H11A0.9300C42—C431.384 (8)
C12—H12A0.9300C42—H42A0.9300
C13—H13A0.9700C43—H43A0.9300
C26—Sb1—C3898.0 (2)As2—C13—H13B109.8
C26—Sb1—C3296.6 (2)As1—C13—H13B109.8
C38—Sb1—C32101.44 (19)H13A—C13—H13B108.2
C26—Sb1—Ru3117.84 (17)C15—C14—C19119.2 (5)
C38—Sb1—Ru3118.75 (14)C15—C14—As2121.2 (4)
C32—Sb1—Ru3119.78 (14)C19—C14—As2119.2 (4)
C44—Ru1—C4593.4 (2)C14—C15—C16120.4 (6)
C44—Ru1—C4690.2 (2)C14—C15—H15A119.8
C45—Ru1—C46170.3 (2)C16—C15—H15A119.8
C44—Ru1—As197.71 (18)C17—C16—C15120.5 (5)
C45—Ru1—As188.34 (17)C17—C16—H16A119.8
C46—Ru1—As1100.15 (15)C15—C16—H16A119.8
C44—Ru1—Ru2169.88 (17)C16—C17—C18119.5 (5)
C45—Ru1—Ru280.65 (16)C16—C17—H17A120.3
C46—Ru1—Ru294.46 (15)C18—C17—H17A120.3
As1—Ru1—Ru290.310 (19)C17—C18—C19120.2 (5)
C44—Ru1—Ru3113.30 (18)C17—C18—H18A119.9
C45—Ru1—Ru391.36 (17)C19—C18—H18A119.9
C46—Ru1—Ru378.92 (16)C14—C19—C18120.1 (5)
As1—Ru1—Ru3148.95 (2)C14—C19—H19A119.9
Ru2—Ru1—Ru359.090 (14)C18—C19—H19A119.9
C48—Ru2—C4789.1 (2)C25—C20—C21119.6 (5)
C48—Ru2—C4993.0 (2)C25—C20—As2119.9 (4)
C47—Ru2—C49175.6 (2)C21—C20—As2120.5 (4)
C48—Ru2—As299.70 (16)C22—C21—C20120.2 (5)
C47—Ru2—As290.30 (17)C22—C21—H21A119.9
C49—Ru2—As293.09 (16)C20—C21—H21A119.9
C48—Ru2—Ru3105.62 (17)C21—C22—C23120.3 (5)
C47—Ru2—Ru382.27 (16)C21—C22—H22A119.8
C49—Ru2—Ru393.47 (15)C23—C22—H22A119.9
As2—Ru2—Ru3153.43 (2)C24—C23—C22119.5 (5)
C48—Ru2—Ru1163.36 (16)C24—C23—H23A120.2
C47—Ru2—Ru197.82 (16)C22—C23—H23A120.2
C49—Ru2—Ru179.10 (15)C23—C24—C25120.4 (5)
As2—Ru2—Ru195.39 (2)C23—C24—H24A119.8
Ru3—Ru2—Ru160.766 (14)C25—C24—H24A119.8
C51—Ru3—C5288.0 (2)C20—C25—C24120.0 (5)
C51—Ru3—C5091.1 (2)C20—C25—H25A120.0
C52—Ru3—C50174.8 (2)C24—C25—H25A120.0
C51—Ru3—Sb1100.32 (17)C31—C26—C27117.8 (6)
C52—Ru3—Sb194.24 (15)C31—C26—Sb1121.7 (5)
C50—Ru3—Sb190.98 (16)C27—C26—Sb1120.3 (5)
C51—Ru3—Ru2103.99 (17)C28—C27—C26122.3 (7)
C52—Ru3—Ru281.37 (15)C28—C27—H27A118.8
C50—Ru3—Ru293.86 (16)C26—C27—H27A118.8
Sb1—Ru3—Ru2155.09 (2)C29—C28—C27118.3 (8)
C51—Ru3—Ru1163.12 (17)C29—C28—H28A120.9
C52—Ru3—Ru194.69 (16)C27—C28—H28A120.9
C50—Ru3—Ru184.69 (19)C30—C29—C28121.0 (7)
Sb1—Ru3—Ru196.108 (17)C30—C29—H29A119.5
Ru2—Ru3—Ru160.144 (14)C28—C29—H29A119.5
C7—As1—C1101.2 (2)C29—C30—C31120.6 (7)
C7—As1—C13102.6 (2)C29—C30—H30A119.7
C1—As1—C13102.0 (2)C31—C30—H30A119.7
C7—As1—Ru1123.55 (16)C26—C31—C30120.0 (7)
C1—As1—Ru1114.97 (15)C26—C31—H31A120.0
C13—As1—Ru1109.85 (16)C30—C31—H31A120.0
C20—As2—C14101.2 (2)C33—C32—C37119.1 (5)
C20—As2—C13102.5 (2)C33—C32—Sb1119.8 (4)
C14—As2—C13103.1 (2)C37—C32—Sb1121.0 (4)
C20—As2—Ru2120.83 (15)C34—C33—C32120.8 (6)
C14—As2—Ru2114.44 (15)C34—C33—H33A119.6
C13—As2—Ru2112.55 (15)C32—C33—H33A119.6
C6—C1—C2118.7 (5)C33—C34—C35119.8 (6)
C6—C1—As1121.5 (4)C33—C34—H34A120.1
C2—C1—As1119.6 (4)C35—C34—H34A120.1
C1—C2—C3121.0 (5)C36—C35—C34119.9 (5)
C1—C2—H2A119.5C36—C35—H35A120.1
C3—C2—H2A119.5C34—C35—H35A120.1
C4—C3—C2119.3 (6)C35—C36—C37120.6 (6)
C4—C3—H3A120.3C35—C36—H36A119.7
C2—C3—H3A120.3C37—C36—H36A119.7
C5—C4—C3120.7 (5)C36—C37—C32119.7 (5)
C5—C4—H4A119.6C36—C37—H37A120.1
C3—C4—H4A119.6C32—C37—H37A120.1
C4—C5—C6120.1 (5)C43—C38—C39119.7 (5)
C4—C5—H5A119.9C43—C38—Sb1118.9 (4)
C6—C5—H5A119.9C39—C38—Sb1121.3 (4)
C1—C6—C5120.1 (5)C38—C39—C40119.8 (5)
C1—C6—H6A120.0C38—C39—H39A120.1
C5—C6—H6A120.0C40—C39—H39A120.1
C12—C7—C8118.9 (5)C41—C40—C39119.9 (6)
C12—C7—As1121.0 (4)C41—C40—H40A120.0
C8—C7—As1120.1 (4)C39—C40—H40A120.0
C9—C8—C7119.9 (5)C42—C41—C40120.3 (6)
C9—C8—H8A120.0C42—C41—H41A119.9
C7—C8—H8A120.0C40—C41—H41A119.9
C10—C9—C8120.4 (5)C41—C42—C43120.1 (5)
C10—C9—H9A119.8C41—C42—H42A120.0
C8—C9—H9A119.8C43—C42—H42A120.0
C9—C10—C11120.5 (5)C38—C43—C42120.2 (5)
C9—C10—H10A119.8C38—C43—H43A119.9
C11—C10—H10A119.8C42—C43—H43A119.9
C10—C11—C12119.8 (6)O1—C44—Ru1176.7 (6)
C10—C11—H11A120.1O2—C45—Ru1174.0 (5)
C12—C11—H11A120.1O3—C46—Ru1175.1 (5)
C7—C12—C11120.5 (5)O4—C47—Ru2173.2 (5)
C7—C12—H12A119.8O5—C48—Ru2179.8 (6)
C11—C12—H12A119.8O6—C49—Ru2174.2 (4)
As2—C13—As1109.4 (2)O7—C50—Ru3174.7 (6)
As2—C13—H13A109.8O8—C51—Ru3179.3 (5)
As1—C13—H13A109.8O9—C52—Ru3174.4 (5)
C44—Ru1—Ru2—C48−80.4 (13)Ru1—Ru2—As2—C14−123.40 (17)
C45—Ru1—Ru2—C48−134.6 (6)C48—Ru2—As2—C13−179.1 (2)
C46—Ru1—Ru2—C4836.9 (6)C47—Ru2—As2—C1391.8 (2)
As1—Ru1—Ru2—C48137.1 (6)C49—Ru2—As2—C13−85.4 (2)
Ru3—Ru1—Ru2—C48−37.4 (6)Ru3—Ru2—As2—C1318.65 (17)
C44—Ru1—Ru2—C4733.5 (11)Ru1—Ru2—As2—C13−6.11 (16)
C45—Ru1—Ru2—C47−20.7 (2)C7—As1—C1—C6153.1 (4)
C46—Ru1—Ru2—C47150.8 (2)C13—As1—C1—C647.5 (5)
As1—Ru1—Ru2—C47−108.97 (17)Ru1—As1—C1—C6−71.3 (5)
Ru3—Ru1—Ru2—C4776.56 (17)C7—As1—C1—C2−32.7 (5)
C44—Ru1—Ru2—C49−143.3 (11)C13—As1—C1—C2−138.4 (4)
C45—Ru1—Ru2—C49162.5 (2)Ru1—As1—C1—C2102.8 (4)
C46—Ru1—Ru2—C49−26.0 (2)C6—C1—C2—C32.4 (9)
As1—Ru1—Ru2—C4974.19 (16)As1—C1—C2—C3−171.9 (5)
Ru3—Ru1—Ru2—C49−100.27 (16)C1—C2—C3—C4−2.0 (10)
C44—Ru1—Ru2—As2124.6 (11)C2—C3—C4—C5−0.1 (10)
C45—Ru1—Ru2—As270.34 (17)C3—C4—C5—C61.7 (10)
C46—Ru1—Ru2—As2−118.13 (15)C2—C1—C6—C5−0.8 (8)
As1—Ru1—Ru2—As2−17.93 (2)As1—C1—C6—C5173.3 (4)
Ru3—Ru1—Ru2—As2167.61 (2)C4—C5—C6—C1−1.2 (9)
C44—Ru1—Ru2—Ru3−43.0 (11)C1—As1—C7—C12−71.1 (5)
C45—Ru1—Ru2—Ru3−97.27 (17)C13—As1—C7—C1234.1 (5)
C46—Ru1—Ru2—Ru374.26 (15)Ru1—As1—C7—C12158.5 (4)
As1—Ru1—Ru2—Ru3174.47 (2)C1—As1—C7—C8107.6 (5)
C26—Sb1—Ru3—C514.8 (2)C13—As1—C7—C8−147.3 (5)
C38—Sb1—Ru3—C51122.8 (2)Ru1—As1—C7—C8−22.8 (5)
C32—Sb1—Ru3—C51−112.1 (2)C12—C7—C8—C9−1.5 (9)
C26—Sb1—Ru3—C52−84.0 (2)As1—C7—C8—C9179.8 (5)
C38—Sb1—Ru3—C5234.1 (2)C7—C8—C9—C10−0.9 (9)
C32—Sb1—Ru3—C52159.2 (2)C8—C9—C10—C113.3 (10)
C26—Sb1—Ru3—C5096.1 (3)C9—C10—C11—C12−3.2 (10)
C38—Sb1—Ru3—C50−145.9 (2)C8—C7—C12—C111.6 (9)
C32—Sb1—Ru3—C50−20.8 (2)As1—C7—C12—C11−179.8 (5)
C26—Sb1—Ru3—Ru2−162.55 (17)C10—C11—C12—C70.7 (10)
C38—Sb1—Ru3—Ru2−44.51 (17)C20—As2—C13—As1−95.8 (3)
C32—Sb1—Ru3—Ru280.56 (16)C14—As2—C13—As1159.4 (2)
C26—Sb1—Ru3—Ru1−179.14 (17)Ru2—As2—C13—As135.6 (3)
C38—Sb1—Ru3—Ru1−61.10 (16)C7—As1—C13—As280.0 (3)
C32—Sb1—Ru3—Ru163.97 (15)C1—As1—C13—As2−175.5 (2)
C48—Ru2—Ru3—C51−16.7 (2)Ru1—As1—C13—As2−53.1 (3)
C47—Ru2—Ru3—C5170.2 (2)C20—As2—C14—C15−148.2 (5)
C49—Ru2—Ru3—C51−110.8 (2)C13—As2—C14—C15−42.4 (5)
As2—Ru2—Ru3—C51145.19 (18)Ru2—As2—C14—C1580.2 (5)
Ru1—Ru2—Ru3—C51173.73 (17)C20—As2—C14—C1939.2 (5)
C48—Ru2—Ru3—C5269.1 (2)C13—As2—C14—C19145.1 (4)
C47—Ru2—Ru3—C52156.0 (2)Ru2—As2—C14—C19−92.3 (4)
C49—Ru2—Ru3—C52−25.0 (2)C19—C14—C15—C16−0.9 (9)
As2—Ru2—Ru3—C52−129.05 (16)As2—C14—C15—C16−173.5 (5)
Ru1—Ru2—Ru3—C52−100.51 (16)C14—C15—C16—C171.4 (11)
C48—Ru2—Ru3—C50−108.8 (3)C15—C16—C17—C18−1.0 (10)
C47—Ru2—Ru3—C50−21.9 (3)C16—C17—C18—C190.1 (9)
C49—Ru2—Ru3—C50157.1 (2)C15—C14—C19—C180.0 (8)
As2—Ru2—Ru3—C5053.08 (19)As2—C14—C19—C18172.7 (4)
Ru1—Ru2—Ru3—C5081.62 (19)C17—C18—C19—C140.4 (9)
C48—Ru2—Ru3—Sb1150.50 (18)C14—As2—C20—C25−124.8 (4)
C47—Ru2—Ru3—Sb1−122.60 (18)C13—As2—C20—C25128.9 (4)
C49—Ru2—Ru3—Sb156.36 (16)Ru2—As2—C20—C252.7 (5)
As2—Ru2—Ru3—Sb1−47.65 (8)C14—As2—C20—C2156.2 (5)
Ru1—Ru2—Ru3—Sb1−19.11 (4)C13—As2—C20—C21−50.2 (5)
C48—Ru2—Ru3—Ru1169.61 (18)Ru2—As2—C20—C21−176.3 (4)
C47—Ru2—Ru3—Ru1−103.49 (17)C25—C20—C21—C22−1.3 (8)
C49—Ru2—Ru3—Ru175.47 (16)As2—C20—C21—C22177.7 (4)
As2—Ru2—Ru3—Ru1−28.54 (5)C20—C21—C22—C23−0.3 (8)
C44—Ru1—Ru3—C51151.1 (6)C21—C22—C23—C241.6 (8)
C45—Ru1—Ru3—C5156.9 (6)C22—C23—C24—C25−1.2 (8)
C46—Ru1—Ru3—C51−123.5 (6)C21—C20—C25—C241.7 (8)
As1—Ru1—Ru3—C51−32.2 (6)As2—C20—C25—C24−177.3 (4)
Ru2—Ru1—Ru3—C51−21.4 (6)C23—C24—C25—C20−0.4 (8)
C44—Ru1—Ru3—C52−110.3 (3)C38—Sb1—C26—C31−161.8 (5)
C45—Ru1—Ru3—C52155.5 (2)C32—Sb1—C26—C3195.6 (5)
C46—Ru1—Ru3—C52−24.8 (2)Ru3—Sb1—C26—C31−33.2 (5)
As1—Ru1—Ru3—C5266.47 (16)C38—Sb1—C26—C2723.6 (5)
Ru2—Ru1—Ru3—C5277.25 (15)C32—Sb1—C26—C27−79.0 (5)
C44—Ru1—Ru3—C5074.9 (3)Ru3—Sb1—C26—C27152.2 (4)
C45—Ru1—Ru3—C50−19.3 (2)C31—C26—C27—C28−1.6 (10)
C46—Ru1—Ru3—C50160.4 (2)Sb1—C26—C27—C28173.3 (5)
As1—Ru1—Ru3—C50−108.33 (17)C26—C27—C28—C290.9 (11)
Ru2—Ru1—Ru3—C50−97.55 (16)C27—C28—C29—C301.2 (11)
C44—Ru1—Ru3—Sb1−15.5 (2)C28—C29—C30—C31−2.6 (11)
C45—Ru1—Ru3—Sb1−109.71 (17)C27—C26—C31—C300.1 (9)
C46—Ru1—Ru3—Sb169.94 (15)Sb1—C26—C31—C30−174.6 (5)
As1—Ru1—Ru3—Sb1161.25 (4)C29—C30—C31—C261.9 (10)
Ru2—Ru1—Ru3—Sb1172.030 (19)C26—Sb1—C32—C3330.1 (5)
C44—Ru1—Ru3—Ru2172.5 (2)C38—Sb1—C32—C33−69.5 (4)
C45—Ru1—Ru3—Ru278.26 (17)Ru3—Sb1—C32—C33157.6 (4)
C46—Ru1—Ru3—Ru2−102.09 (15)C26—Sb1—C32—C37−147.0 (4)
As1—Ru1—Ru3—Ru2−10.78 (4)C38—Sb1—C32—C37113.4 (4)
C44—Ru1—As1—C7106.0 (3)Ru3—Sb1—C32—C37−19.6 (5)
C45—Ru1—As1—C7−160.8 (3)C37—C32—C33—C340.2 (8)
C46—Ru1—As1—C714.4 (2)Sb1—C32—C33—C34−177.0 (4)
Ru2—Ru1—As1—C7−80.15 (19)C32—C33—C34—C35−1.1 (9)
Ru3—Ru1—As1—C7−70.92 (19)C33—C34—C35—C362.5 (9)
C44—Ru1—As1—C1−18.5 (3)C34—C35—C36—C37−2.8 (10)
C45—Ru1—As1—C174.7 (2)C35—C36—C37—C321.9 (10)
C46—Ru1—As1—C1−110.1 (2)C33—C32—C37—C36−0.5 (8)
Ru2—Ru1—As1—C1155.33 (17)Sb1—C32—C37—C36176.6 (5)
Ru3—Ru1—As1—C1164.56 (17)C26—Sb1—C38—C4370.3 (4)
C44—Ru1—As1—C13−132.8 (2)C32—Sb1—C38—C43168.8 (4)
C45—Ru1—As1—C13−39.6 (2)Ru3—Sb1—C38—C43−57.6 (5)
C46—Ru1—As1—C13135.6 (2)C26—Sb1—C38—C39−108.5 (5)
Ru2—Ru1—As1—C1341.03 (15)C32—Sb1—C38—C39−10.0 (5)
Ru3—Ru1—As1—C1350.27 (16)Ru3—Sb1—C38—C39123.6 (4)
C48—Ru2—As2—C20−57.7 (2)C43—C38—C39—C400.3 (9)
C47—Ru2—As2—C20−146.8 (2)Sb1—C38—C39—C40179.1 (5)
C49—Ru2—As2—C2036.0 (2)C38—C39—C40—C411.0 (10)
Ru3—Ru2—As2—C20140.05 (17)C39—C40—C41—C42−1.5 (10)
Ru1—Ru2—As2—C20115.29 (17)C40—C41—C42—C430.6 (10)
C48—Ru2—As2—C1463.6 (2)C39—C38—C43—C42−1.2 (8)
C47—Ru2—As2—C14−25.5 (2)Sb1—C38—C43—C42−180.0 (4)
C49—Ru2—As2—C14157.3 (2)C41—C42—C43—C380.7 (9)
Ru3—Ru2—As2—C14−98.65 (17)
D—H···AD—HH···AD···AD—H···A
C13—H13B···O8i0.972.593.290 (7)129
C23—H23A···Cg1ii0.932.883.686 (6)146
C34—H34A···Cg2iii0.932.723.564 (6)151
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
C13—H13B⋯O8i0.972.593.290 (7)129
C23—H23ACg1ii0.932.883.686 (6)146
C34—H34ACg2iii0.932.723.564 (6)151

Symmetry codes: (i) ; (ii) ; (iii) . Cg1 and Cg2 are the centroids of the C14–C19 and C26–C31phenyl rings, respectively.

  3 in total

1.  A short history of SHELX.

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

2.  [μ-Bis(diphenyl-arsino)methane-1:2κAs:As']nona-carbonyl-1κC,2κC,3κC-tricyclo-hexyl-phosphine-3κP-triangulo-triruthenium(0).

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; Chin Sing Yeap; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-11-21

3.  Structure validation in chemical crystallography.

Authors:  Anthony L Spek
Journal:  Acta Crystallogr D Biol Crystallogr       Date:  2009-01-20
  3 in total
  7 in total

1.  [μ-Bis(di-o-tolyl-phosphan-yl)methane-1:2κP:P']nona-carbonyl-1κC,2κC,3κC-[diphen-yl(phenyl-sulfanylmeth-yl)phosphane-3κP]-triangulo-triruthenium(0) dichloro-methane 0.25-solvate.

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; H A Hafiz Malik; Chin Sing Yeap; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-01-15

2.  [μ-Bis(di-o-tolyl-phosphan-yl)methane-1:2κP:P']deca-carbonyl-1κC,2κC,3κC-triangulo-triruthenium(0)-methanol (8/1).

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; H A Hafiz Malik; Chin Sing Yeap; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-01-15

3.  [μ-Bis(diphenyl-arsan-yl)methane-1:2κAs:As']nona-carbonyl-1κC,2κC,3κC-[tris-(biphenyl-4-yl)arsane-3κAs]-triangulo-triruthenium(0).

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; Siti Syaida Sirat; Chin Sing Yeap; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-01-15

4.  [μ-Bis(diphenyl-phosphan-yl)ethane-1:2κP:P']nona-carbonyl-1κC,2κC,3κC-(triphenyl-stibine-3κSb)-triangulo-triruthenium(0).

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; Siti Syaida Sirat; Chin Sing Yeap; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2011-01-15

5.  [μ-Bis(di-o-tolyl-phosphan-yl)methane-1:2κ(2)P:P']nona-carbonyl-1κ(3)C,2κ(3)C,3κ(3)C-[tris-(2-chloro-eth-yl) phosphite-3κP]-triangulo-triruthenium(0).

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; Siti Syaida Sirat; Ching Kheng Quah; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-05-31

6.  [μ-Bis(di-o-tolyl-phosphan-yl)methane-1:2κ(2)P:P']nona-carbonyl-1κ(3)C,2κ(3)C,3κ(3)C-(triphenyl phosphite-3κP)-triangulo-triruthenium(0) chloro-form disolvate.

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; Siti Syaida Sirat; Ching Kheng Quah; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-05-26

7.  [μ-Bis(diphenyl-arsino)methane-1:2κ(2)As:As]deca-carbonyl-1κ(3)C,2κ(3)C,3κ(4)C-triangulo-triosmium(0).

Authors:  Omar Bin Shawkataly; Imthyaz Ahmed Khan; Siti Syaida Sirat; Ching Kheng Quah; Hoong-Kun Fun
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2012-07-25
  7 in total

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