Literature DB >> 21579935

[μ-Bis(diphenyl-arsino)methane-1:2κAs:As']nona-carbonyl-1κC,2κC,3κC-[tris-(4-methyl-phen-yl)-phosphine-3κP]-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(21)H(21)P)(CO)(9)], the bis-(diphenyl-arsino)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 Ru(3) triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three phenyl rings of the phosphine make dihedral angles of 86.89 (19), 82.1 (2) and 63.0 (2)° with each other. The dihedral angles between the two phenyl rings are 73.8 (2) and 82.2 (3)° for the two diphenyl-arsino groups. An intra-molecular C-H⋯O hydrogen bond stabilizes the mol-ecular structure. In the crystal packing, mol-ecules are linked into chains down the b axis via inter-molecular C-H⋯O hydrogen bonds.

Entities:  

Year:  2009        PMID: 21579935      PMCID: PMC2980046          DOI: 10.1107/S1600536809049940

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 in the data collection, see: Cosier & Glazer (1986 ▶).

Experimental

Crystal data

[Ru3(C25H22As2)(C21H21P)(CO)9] M = 1331.91 Monoclinic, a = 16.2585 (2) Å b = 16.9247 (2) Å c = 19.6900 (2) Å β = 98.680 (1)° V = 5356.05 (11) Å3 Z = 4 Mo Kα radiation μ = 2.15 mm−1 T = 296 K 0.21 × 0.21 × 0.03 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer Absorption correction: multi-scan (; Bruker, 2005 ▶) T min = 0.665, T max = 0.933 63277 measured reflections 15703 independent reflections 9536 reflections with I > 2σ(I) R int = 0.063

Refinement

R[F 2 > 2σ(F 2)] = 0.049 wR(F 2) = 0.096 S = 1.00 15703 reflections 634 parameters H-atom parameters constrained Δρmax = 0.60 e Å−3 Δρmin = −0.41 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/S1600536809049940/sj2681sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809049940/sj2681Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ru3(C25H22As2)(C21H21P)(CO)9]F(000) = 2632
Mr = 1331.91Dx = 1.652 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9940 reflections
a = 16.2585 (2) Åθ = 2.3–26.0°
b = 16.9247 (2) ŵ = 2.15 mm1
c = 19.6900 (2) ÅT = 296 K
β = 98.680 (1)°Plate, red
V = 5356.05 (11) Å30.21 × 0.21 × 0.03 mm
Z = 4
Bruker SMART APEXII CCD area-detector diffractometer15703 independent reflections
Radiation source: fine-focus sealed tube9536 reflections with I > 2σ(I)
graphiteRint = 0.063
φ and ω scansθmax = 30.1°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Bruker, 2005)h = −22→22
Tmin = 0.665, Tmax = 0.933k = −18→23
63277 measured reflectionsl = −27→27
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.096H-atom parameters constrained
S = 1.00w = 1/[σ2(Fo2) + (0.0397P)2] where P = (Fo2 + 2Fc2)/3
15703 reflections(Δ/σ)max < 0.001
634 parametersΔρmax = 0.60 e Å3
0 restraintsΔρmin = −0.40 e Å3
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
Ru10.234430 (18)0.082258 (18)0.290394 (17)0.03903 (8)
Ru20.095682 (17)0.005658 (17)0.211088 (16)0.03574 (8)
Ru30.250620 (18)−0.075182 (17)0.238649 (17)0.03759 (8)
As10.16874 (2)0.21116 (2)0.26830 (2)0.03705 (10)
As2−0.00352 (2)0.11309 (2)0.21734 (2)0.03700 (10)
P10.38304 (6)−0.13329 (6)0.26418 (5)0.0402 (2)
O10.3348 (2)0.10979 (19)0.17289 (18)0.0784 (10)
O20.3831 (2)0.1220 (2)0.3968 (2)0.0934 (12)
O30.1375 (2)0.05987 (18)0.41083 (17)0.0741 (10)
O40.0457 (2)−0.08636 (18)0.33265 (19)0.0782 (11)
O5−0.0027 (2)−0.1159 (2)0.1199 (2)0.0924 (12)
O60.1513 (2)0.09138 (18)0.08889 (17)0.0699 (9)
O70.2824 (2)−0.0409 (2)0.09116 (17)0.0756 (10)
O80.1550 (2)−0.22473 (19)0.19949 (19)0.0814 (11)
O90.2461 (2)−0.08632 (17)0.39289 (17)0.0697 (9)
C10.1912 (2)0.2681 (2)0.1877 (2)0.0445 (10)
C20.2732 (3)0.2890 (3)0.1858 (3)0.0652 (13)
H2A0.31410.27530.22210.078*
C30.2948 (4)0.3300 (3)0.1304 (3)0.0791 (16)
H3A0.35000.34360.12960.095*
C40.2357 (4)0.3504 (3)0.0775 (3)0.0845 (18)
H4A0.25040.37850.04060.101*
C50.1538 (4)0.3297 (3)0.0780 (3)0.0817 (16)
H5A0.11320.34300.04120.098*
C60.1326 (3)0.2889 (3)0.1338 (2)0.0616 (12)
H6A0.07730.27550.13450.074*
C70.1927 (2)0.2926 (2)0.3382 (2)0.0405 (9)
C80.2062 (3)0.2709 (2)0.4064 (2)0.0538 (11)
H8A0.20580.21760.41770.065*
C90.2204 (3)0.3265 (3)0.4583 (2)0.0671 (14)
H9A0.22890.31070.50410.081*
C100.2217 (3)0.4046 (3)0.4418 (3)0.0668 (14)
H10A0.23140.44250.47630.080*
C110.2086 (3)0.4272 (3)0.3744 (3)0.0675 (14)
H11A0.20990.48060.36340.081*
C120.1936 (3)0.3718 (2)0.3225 (2)0.0578 (12)
H12A0.18410.38810.27690.069*
C130.0474 (2)0.2089 (2)0.2622 (2)0.0416 (9)
H13A0.02430.25480.23670.050*
H13B0.03300.21230.30820.050*
C14−0.0632 (2)0.1517 (2)0.1305 (2)0.0448 (10)
C15−0.0724 (3)0.1023 (3)0.0737 (3)0.0661 (13)
H15A−0.05080.05130.07790.079*
C16−0.1131 (4)0.1278 (4)0.0115 (3)0.0925 (19)
H16A−0.11930.0936−0.02590.111*
C17−0.1448 (4)0.2033 (4)0.0036 (3)0.0920 (19)
H17A−0.17150.2206−0.03900.110*
C18−0.1363 (3)0.2525 (3)0.0599 (3)0.0763 (15)
H18A−0.15720.30370.05540.092*
C19−0.0973 (3)0.2266 (3)0.1227 (2)0.0560 (11)
H19A−0.09370.25990.16050.067*
C20−0.0938 (2)0.0935 (2)0.2700 (2)0.0501 (11)
C21−0.1754 (3)0.0953 (3)0.2391 (3)0.0676 (14)
H21A−0.18860.11110.19350.081*
C22−0.2379 (3)0.0736 (4)0.2756 (4)0.095 (2)
H22A−0.29310.07420.25450.114*
C23−0.2189 (4)0.0514 (4)0.3419 (4)0.113 (3)
H23A−0.26120.03520.36570.136*
C24−0.1385 (4)0.0523 (4)0.3747 (4)0.123 (3)
H24A−0.12610.03900.42090.148*
C25−0.0748 (3)0.0737 (3)0.3370 (3)0.0853 (18)
H25A−0.01970.07430.35830.102*
C260.3884 (2)−0.2298 (2)0.3075 (2)0.0416 (9)
C270.3279 (2)−0.2538 (2)0.3465 (2)0.0529 (11)
H27A0.2810−0.22260.34740.064*
C280.3370 (3)−0.3233 (2)0.3841 (2)0.0581 (12)
H28A0.2967−0.33700.41080.070*
C290.4040 (3)−0.3724 (2)0.3827 (2)0.0545 (11)
C300.4632 (3)−0.3498 (2)0.3433 (2)0.0584 (12)
H30A0.5088−0.38250.34120.070*
C310.4564 (3)−0.2794 (2)0.3066 (2)0.0520 (11)
H31A0.4979−0.26520.28120.062*
C320.4366 (2)−0.1552 (2)0.1903 (2)0.0434 (9)
C330.3920 (3)−0.1915 (2)0.1337 (2)0.0546 (11)
H33A0.3360−0.20280.13330.066*
C340.4297 (3)−0.2114 (3)0.0773 (2)0.0644 (13)
H34A0.3983−0.23530.03940.077*
C350.5131 (3)−0.1962 (3)0.0764 (2)0.0579 (12)
C360.5573 (3)−0.1617 (3)0.1335 (2)0.0596 (12)
H36A0.6138−0.15190.13440.072*
C370.5202 (2)−0.1409 (2)0.1898 (2)0.0533 (11)
H37A0.5519−0.11710.22760.064*
C380.4591 (2)−0.0747 (2)0.3211 (2)0.0416 (9)
C390.4872 (3)−0.0032 (2)0.2982 (2)0.0546 (11)
H39A0.46910.01300.25330.065*
C400.5415 (3)0.0441 (3)0.3412 (3)0.0585 (12)
H40A0.56030.09110.32440.070*
C410.5683 (3)0.0229 (3)0.4083 (2)0.0578 (12)
C420.5398 (3)−0.0477 (3)0.4309 (2)0.0592 (12)
H42A0.5572−0.06350.47600.071*
C430.4858 (2)−0.0957 (2)0.3878 (2)0.0491 (11)
H43A0.4675−0.14290.40450.059*
C440.2951 (3)0.0928 (2)0.2144 (2)0.0522 (11)
C450.3291 (3)0.1071 (3)0.3549 (3)0.0582 (12)
C460.1713 (3)0.0653 (2)0.3637 (2)0.0518 (11)
C470.0670 (2)−0.0503 (2)0.2894 (2)0.0499 (11)
C480.0325 (2)−0.0683 (3)0.1537 (2)0.0525 (11)
C490.1344 (2)0.0597 (2)0.1357 (2)0.0475 (10)
C500.2690 (3)−0.0515 (2)0.1462 (2)0.0494 (10)
C510.1925 (2)−0.1692 (3)0.2141 (2)0.0505 (11)
C520.2446 (3)−0.0733 (2)0.3344 (2)0.0505 (11)
C530.4136 (3)−0.4481 (3)0.4251 (3)0.0830 (16)
H53A0.4712−0.45580.44330.124*
H53B0.3940−0.49210.39640.124*
H53C0.3818−0.44390.46220.124*
C540.5545 (3)−0.2172 (3)0.0149 (2)0.0850 (18)
H54A0.6021−0.25000.02940.127*
H54B0.5718−0.1698−0.00560.127*
H54C0.5157−0.2452−0.01820.127*
C550.6253 (3)0.0748 (3)0.4567 (3)0.095 (2)
H55A0.65570.10920.43070.142*
H55B0.66350.04240.48650.142*
H55C0.59280.10590.48370.142*
U11U22U33U12U13U23
Ru10.03420 (15)0.03399 (18)0.04736 (19)−0.00229 (13)0.00114 (15)−0.00603 (15)
Ru20.02854 (13)0.03101 (17)0.04748 (18)−0.00082 (12)0.00511 (13)−0.00357 (14)
Ru30.03213 (15)0.03246 (17)0.04644 (19)0.00260 (12)0.00032 (14)−0.00174 (14)
As10.0377 (2)0.0325 (2)0.0409 (2)−0.00439 (16)0.00575 (18)−0.00314 (17)
As20.03049 (18)0.0332 (2)0.0480 (2)0.00017 (16)0.00820 (18)−0.00228 (18)
P10.0329 (5)0.0406 (6)0.0455 (6)0.0030 (4)0.0012 (5)0.0006 (5)
O10.072 (2)0.079 (2)0.093 (3)−0.0106 (18)0.041 (2)−0.008 (2)
O20.070 (2)0.104 (3)0.093 (3)0.004 (2)−0.031 (2)−0.038 (2)
O30.093 (3)0.068 (2)0.066 (2)−0.0084 (18)0.028 (2)−0.0057 (17)
O40.085 (2)0.064 (2)0.091 (3)−0.0072 (18)0.031 (2)0.0289 (19)
O50.074 (2)0.076 (3)0.120 (3)−0.017 (2)−0.006 (2)−0.046 (2)
O60.074 (2)0.075 (2)0.064 (2)0.0058 (17)0.0215 (19)0.0193 (18)
O70.097 (3)0.076 (2)0.057 (2)0.0244 (19)0.020 (2)0.0140 (18)
O80.079 (2)0.048 (2)0.109 (3)−0.0221 (18)−0.014 (2)−0.005 (2)
O90.099 (3)0.056 (2)0.053 (2)0.0103 (17)0.008 (2)0.0068 (16)
C10.050 (2)0.033 (2)0.051 (3)−0.0051 (18)0.012 (2)−0.0029 (19)
C20.060 (3)0.072 (3)0.065 (3)−0.016 (2)0.014 (3)0.006 (3)
C30.086 (4)0.078 (4)0.079 (4)−0.027 (3)0.034 (4)0.002 (3)
C40.122 (5)0.074 (4)0.065 (4)−0.022 (4)0.039 (4)0.007 (3)
C50.114 (5)0.069 (4)0.059 (3)0.005 (3)0.001 (3)0.017 (3)
C60.060 (3)0.062 (3)0.062 (3)−0.001 (2)0.007 (3)0.011 (3)
C70.043 (2)0.032 (2)0.045 (2)−0.0035 (17)0.0051 (19)−0.0045 (18)
C80.076 (3)0.035 (2)0.049 (3)−0.006 (2)0.006 (2)−0.005 (2)
C90.104 (4)0.054 (3)0.044 (3)−0.008 (3)0.014 (3)−0.012 (2)
C100.088 (4)0.055 (3)0.060 (3)−0.014 (3)0.016 (3)−0.023 (3)
C110.099 (4)0.037 (3)0.067 (3)−0.011 (2)0.016 (3)−0.007 (2)
C120.079 (3)0.040 (3)0.054 (3)−0.003 (2)0.007 (3)−0.004 (2)
C130.0393 (19)0.039 (2)0.047 (2)0.0029 (16)0.0079 (19)−0.0054 (18)
C140.0347 (19)0.050 (3)0.049 (2)0.0002 (18)0.0025 (19)−0.001 (2)
C150.061 (3)0.070 (3)0.062 (3)0.019 (2)−0.009 (3)−0.016 (3)
C160.090 (4)0.123 (5)0.057 (3)0.032 (4)−0.014 (3)−0.028 (4)
C170.092 (4)0.116 (5)0.062 (4)0.035 (4)−0.006 (3)0.006 (4)
C180.074 (3)0.071 (4)0.076 (4)0.020 (3)−0.013 (3)0.010 (3)
C190.055 (3)0.048 (3)0.062 (3)0.008 (2)−0.002 (2)−0.006 (2)
C200.044 (2)0.041 (2)0.070 (3)0.0045 (18)0.023 (2)0.004 (2)
C210.042 (2)0.067 (3)0.097 (4)−0.006 (2)0.024 (3)−0.005 (3)
C220.047 (3)0.115 (5)0.128 (6)−0.013 (3)0.029 (4)−0.005 (4)
C230.088 (5)0.119 (5)0.151 (7)0.018 (4)0.077 (5)0.040 (5)
C240.099 (5)0.164 (7)0.120 (6)0.044 (5)0.060 (5)0.069 (5)
C250.057 (3)0.122 (5)0.082 (4)0.021 (3)0.027 (3)0.033 (3)
C260.040 (2)0.034 (2)0.048 (2)0.0044 (16)−0.0027 (19)−0.0037 (18)
C270.039 (2)0.044 (3)0.074 (3)0.0042 (19)0.004 (2)0.010 (2)
C280.047 (2)0.046 (3)0.079 (3)−0.004 (2)0.004 (2)0.012 (2)
C290.058 (3)0.036 (2)0.064 (3)−0.004 (2)−0.010 (2)0.001 (2)
C300.059 (3)0.046 (3)0.066 (3)0.022 (2)−0.002 (2)−0.003 (2)
C310.049 (2)0.053 (3)0.054 (3)0.010 (2)0.008 (2)0.000 (2)
C320.044 (2)0.042 (2)0.042 (2)0.0084 (18)0.0006 (19)0.0015 (19)
C330.048 (2)0.054 (3)0.060 (3)0.008 (2)0.000 (2)−0.005 (2)
C340.073 (3)0.061 (3)0.056 (3)0.015 (2)−0.002 (3)−0.011 (2)
C350.066 (3)0.059 (3)0.049 (3)0.023 (2)0.007 (2)0.007 (2)
C360.050 (2)0.073 (3)0.056 (3)0.012 (2)0.009 (2)0.004 (3)
C370.045 (2)0.063 (3)0.050 (3)0.006 (2)0.002 (2)−0.001 (2)
C380.0327 (18)0.044 (2)0.049 (2)0.0033 (16)0.0085 (18)−0.0028 (19)
C390.046 (2)0.056 (3)0.059 (3)−0.008 (2)0.002 (2)0.000 (2)
C400.044 (2)0.057 (3)0.076 (3)−0.014 (2)0.013 (2)−0.010 (3)
C410.041 (2)0.074 (3)0.061 (3)0.000 (2)0.012 (2)−0.024 (3)
C420.058 (3)0.073 (3)0.045 (3)0.007 (2)0.002 (2)−0.012 (2)
C430.050 (2)0.053 (3)0.046 (2)0.005 (2)0.012 (2)−0.002 (2)
C440.043 (2)0.049 (3)0.063 (3)−0.0051 (19)0.003 (2)−0.013 (2)
C450.047 (2)0.057 (3)0.067 (3)0.002 (2)−0.003 (2)−0.016 (2)
C460.058 (3)0.040 (3)0.056 (3)−0.0021 (19)0.005 (2)−0.004 (2)
C470.042 (2)0.038 (2)0.070 (3)0.0010 (18)0.008 (2)0.000 (2)
C480.040 (2)0.047 (3)0.069 (3)0.0006 (19)0.005 (2)−0.010 (2)
C490.040 (2)0.046 (3)0.057 (3)0.0082 (18)0.006 (2)−0.005 (2)
C500.047 (2)0.042 (2)0.056 (3)0.0095 (19)−0.001 (2)−0.002 (2)
C510.042 (2)0.043 (3)0.064 (3)0.0014 (19)−0.003 (2)0.004 (2)
C520.050 (2)0.049 (3)0.052 (3)0.0040 (19)0.005 (2)−0.005 (2)
C530.092 (4)0.047 (3)0.104 (4)−0.001 (3)−0.003 (4)0.017 (3)
C540.103 (4)0.103 (4)0.052 (3)0.046 (3)0.020 (3)0.009 (3)
C550.073 (4)0.121 (5)0.092 (4)−0.037 (3)0.017 (3)−0.057 (4)
Ru1—C451.890 (5)C16—C171.378 (7)
Ru1—C461.915 (4)C16—H16A0.9300
Ru1—C441.922 (4)C17—C181.378 (7)
Ru1—As12.4391 (5)C17—H17A0.9300
Ru1—Ru22.8539 (4)C18—C191.373 (6)
Ru1—Ru32.8790 (4)C18—H18A0.9300
Ru2—C481.884 (5)C19—H19A0.9300
Ru2—C471.925 (4)C20—C251.352 (7)
Ru2—C491.929 (4)C20—C211.374 (6)
Ru2—As22.4460 (4)C21—C221.380 (6)
Ru2—Ru32.8460 (4)C21—H21A0.9300
Ru3—C511.876 (5)C22—C231.348 (9)
Ru3—C521.904 (4)C22—H22A0.9300
Ru3—C501.931 (5)C23—C241.368 (10)
Ru3—P12.3513 (10)C23—H23A0.9300
As1—C11.938 (4)C24—C251.410 (7)
As1—C71.946 (4)C24—H24A0.9300
As1—C131.958 (3)C25—H25A0.9300
As2—C141.947 (4)C26—C311.390 (5)
As2—C201.948 (3)C26—C271.397 (5)
As2—C131.968 (4)C27—C281.386 (5)
P1—C381.831 (4)C27—H27A0.9300
P1—C261.839 (4)C28—C291.374 (6)
P1—C321.842 (4)C28—H28A0.9300
O1—C441.151 (5)C29—C301.379 (6)
O2—C451.138 (5)C29—C531.523 (6)
O3—C461.151 (4)C30—C311.389 (5)
O4—C471.144 (5)C30—H30A0.9300
O5—C481.141 (5)C31—H31A0.9300
O6—C491.135 (5)C32—C331.379 (6)
O7—C501.151 (5)C32—C371.382 (5)
O8—C511.134 (5)C33—C341.389 (6)
O9—C521.168 (5)C33—H33A0.9300
C1—C61.362 (6)C34—C351.383 (6)
C1—C21.385 (5)C34—H34A0.9300
C2—C31.381 (6)C35—C361.370 (6)
C2—H2A0.9300C35—C541.514 (6)
C3—C41.350 (7)C36—C371.385 (5)
C3—H3A0.9300C36—H36A0.9300
C4—C51.379 (8)C37—H37A0.9300
C4—H4A0.9300C38—C431.366 (5)
C5—C61.384 (6)C38—C391.392 (5)
C5—H5A0.9300C39—C401.383 (6)
C6—H6A0.9300C39—H39A0.9300
C7—C121.376 (5)C40—C411.374 (6)
C7—C81.376 (5)C40—H40A0.9300
C8—C91.383 (6)C41—C421.379 (6)
C8—H8A0.9300C41—C551.508 (6)
C9—C101.363 (6)C42—C431.388 (6)
C9—H9A0.9300C42—H42A0.9300
C10—C111.366 (6)C43—H43A0.9300
C10—H10A0.9300C53—H53A0.9600
C11—C121.381 (6)C53—H53B0.9600
C11—H11A0.9300C53—H53C0.9600
C12—H12A0.9300C54—H54A0.9600
C13—H13A0.9700C54—H54B0.9600
C13—H13B0.9700C54—H54C0.9600
C14—C191.382 (5)C55—H55A0.9600
C14—C151.386 (6)C55—H55B0.9600
C15—C161.372 (7)C55—H55C0.9600
C15—H15A0.9300
C45—Ru1—C4690.09 (19)C15—C16—C17121.0 (5)
C45—Ru1—C4492.37 (18)C15—C16—H16A119.5
C46—Ru1—C44176.30 (17)C17—C16—H16A119.5
C45—Ru1—As1102.18 (14)C16—C17—C18118.7 (5)
C46—Ru1—As189.88 (12)C16—C17—H17A120.7
C44—Ru1—As192.30 (12)C18—C17—H17A120.7
C45—Ru1—Ru2164.91 (15)C19—C18—C17120.5 (5)
C46—Ru1—Ru282.81 (13)C19—C18—H18A119.8
C44—Ru1—Ru294.15 (13)C17—C18—H18A119.8
As1—Ru1—Ru291.150 (15)C18—C19—C14121.2 (4)
C45—Ru1—Ru3109.60 (13)C18—C19—H19A119.4
C46—Ru1—Ru3102.50 (12)C14—C19—H19A119.4
C44—Ru1—Ru374.06 (12)C25—C20—C21120.1 (4)
As1—Ru1—Ru3145.659 (18)C25—C20—As2118.8 (3)
Ru2—Ru1—Ru359.526 (10)C21—C20—As2121.0 (4)
C48—Ru2—C4788.73 (18)C20—C21—C22120.1 (5)
C48—Ru2—C4993.74 (18)C20—C21—H21A120.0
C47—Ru2—C49174.99 (17)C22—C21—H21A120.0
C48—Ru2—As2102.71 (12)C23—C22—C21120.0 (6)
C47—Ru2—As294.85 (11)C23—C22—H22A120.0
C49—Ru2—As288.86 (11)C21—C22—H22A120.0
C48—Ru2—Ru3100.48 (12)C22—C23—C24121.1 (5)
C47—Ru2—Ru385.69 (12)C22—C23—H23A119.5
C49—Ru2—Ru389.58 (11)C24—C23—H23A119.5
As2—Ru2—Ru3156.811 (17)C23—C24—C25118.7 (6)
C48—Ru2—Ru1160.83 (12)C23—C24—H24A120.6
C47—Ru2—Ru192.99 (13)C25—C24—H24A120.6
C49—Ru2—Ru183.26 (13)C20—C25—C24120.0 (5)
As2—Ru2—Ru196.175 (14)C20—C25—H25A120.0
Ru3—Ru2—Ru160.675 (11)C24—C25—H25A120.0
C51—Ru3—C5299.79 (18)C31—C26—C27117.3 (4)
C51—Ru3—C5094.40 (18)C31—C26—P1120.9 (3)
C52—Ru3—C50165.73 (17)C27—C26—P1121.6 (3)
C51—Ru3—P196.29 (12)C28—C27—C26120.9 (4)
C52—Ru3—P188.70 (13)C28—C27—H27A119.6
C50—Ru3—P191.23 (12)C26—C27—H27A119.6
C51—Ru3—Ru287.81 (12)C29—C28—C27121.6 (4)
C52—Ru3—Ru290.27 (12)C29—C28—H28A119.2
C50—Ru3—Ru288.79 (12)C27—C28—H28A119.2
P1—Ru3—Ru2175.88 (3)C28—C29—C30117.8 (4)
C51—Ru3—Ru1143.77 (12)C28—C29—C53120.9 (4)
C52—Ru3—Ru167.23 (12)C30—C29—C53121.2 (4)
C50—Ru3—Ru1100.20 (12)C29—C30—C31121.5 (4)
P1—Ru3—Ru1116.18 (3)C29—C30—H30A119.2
Ru2—Ru3—Ru159.798 (10)C31—C30—H30A119.2
C1—As1—C7100.67 (16)C30—C31—C26120.8 (4)
C1—As1—C13105.80 (17)C30—C31—H31A119.6
C7—As1—C1398.57 (15)C26—C31—H31A119.6
C1—As1—Ru1117.32 (11)C33—C32—C37118.0 (4)
C7—As1—Ru1118.18 (12)C33—C32—P1118.3 (3)
C13—As1—Ru1113.78 (11)C37—C32—P1123.6 (3)
C14—As2—C20102.02 (17)C32—C33—C34120.9 (4)
C14—As2—C13103.76 (17)C32—C33—H33A119.6
C20—As2—C13101.59 (16)C34—C33—H33A119.6
C14—As2—Ru2116.77 (11)C35—C34—C33121.1 (5)
C20—As2—Ru2117.12 (12)C35—C34—H34A119.4
C13—As2—Ru2113.51 (11)C33—C34—H34A119.4
C38—P1—C26102.54 (18)C36—C35—C34117.6 (4)
C38—P1—C32103.69 (17)C36—C35—C54121.1 (4)
C26—P1—C32101.05 (16)C34—C35—C54121.4 (5)
C38—P1—Ru3114.60 (12)C35—C36—C37121.8 (4)
C26—P1—Ru3116.66 (12)C35—C36—H36A119.1
C32—P1—Ru3116.26 (13)C37—C36—H36A119.1
C6—C1—C2118.4 (4)C32—C37—C36120.6 (4)
C6—C1—As1124.8 (3)C32—C37—H37A119.7
C2—C1—As1116.8 (3)C36—C37—H37A119.7
C3—C2—C1120.7 (5)C43—C38—C39117.8 (4)
C3—C2—H2A119.7C43—C38—P1122.3 (3)
C1—C2—H2A119.7C39—C38—P1119.8 (3)
C4—C3—C2120.1 (5)C40—C39—C38121.0 (4)
C4—C3—H3A120.0C40—C39—H39A119.5
C2—C3—H3A120.0C38—C39—H39A119.5
C3—C4—C5120.4 (5)C41—C40—C39121.1 (4)
C3—C4—H4A119.8C41—C40—H40A119.4
C5—C4—H4A119.8C39—C40—H40A119.4
C4—C5—C6119.2 (6)C40—C41—C42117.6 (4)
C4—C5—H5A120.4C40—C41—C55122.0 (5)
C6—C5—H5A120.4C42—C41—C55120.3 (5)
C1—C6—C5121.3 (5)C41—C42—C43121.4 (4)
C1—C6—H6A119.4C41—C42—H42A119.3
C5—C6—H6A119.4C43—C42—H42A119.3
C12—C7—C8118.3 (4)C38—C43—C42121.0 (4)
C12—C7—As1122.6 (3)C38—C43—H43A119.5
C8—C7—As1119.1 (3)C42—C43—H43A119.5
C7—C8—C9121.6 (4)O1—C44—Ru1170.0 (4)
C7—C8—H8A119.2O2—C45—Ru1175.8 (4)
C9—C8—H8A119.2O3—C46—Ru1174.2 (4)
C10—C9—C8119.3 (4)O4—C47—Ru2175.0 (4)
C10—C9—H9A120.4O5—C48—Ru2176.5 (4)
C8—C9—H9A120.4O6—C49—Ru2174.9 (4)
C9—C10—C11119.9 (4)O7—C50—Ru3176.5 (4)
C9—C10—H10A120.1O8—C51—Ru3177.7 (4)
C11—C10—H10A120.1O9—C52—Ru3167.5 (4)
C10—C11—C12120.9 (4)C29—C53—H53A109.5
C10—C11—H11A119.6C29—C53—H53B109.5
C12—C11—H11A119.6H53A—C53—H53B109.5
C7—C12—C11120.0 (4)C29—C53—H53C109.5
C7—C12—H12A120.0H53A—C53—H53C109.5
C11—C12—H12A120.0H53B—C53—H53C109.5
As1—C13—As2113.29 (16)C35—C54—H54A109.5
As1—C13—H13A108.9C35—C54—H54B109.5
As2—C13—H13A108.9H54A—C54—H54B109.5
As1—C13—H13B108.9C35—C54—H54C109.5
As2—C13—H13B108.9H54A—C54—H54C109.5
H13A—C13—H13B107.7H54B—C54—H54C109.5
C19—C14—C15118.0 (4)C41—C55—H55A109.5
C19—C14—As2123.0 (3)C41—C55—H55B109.5
C15—C14—As2119.0 (3)H55A—C55—H55B109.5
C16—C15—C14120.6 (5)C41—C55—H55C109.5
C16—C15—H15A119.7H55A—C55—H55C109.5
C14—C15—H15A119.7H55B—C55—H55C109.5
C45—Ru1—Ru2—C48−58.0 (6)Ru1—As1—C1—C2−62.2 (3)
C46—Ru1—Ru2—C48−120.5 (4)C6—C1—C2—C30.0 (7)
C44—Ru1—Ru2—C4857.4 (4)As1—C1—C2—C3−179.6 (4)
As1—Ru1—Ru2—C48149.8 (4)C1—C2—C3—C40.2 (8)
Ru3—Ru1—Ru2—C48−11.4 (4)C2—C3—C4—C5−0.7 (9)
C45—Ru1—Ru2—C4736.8 (5)C3—C4—C5—C61.0 (8)
C46—Ru1—Ru2—C47−25.75 (17)C2—C1—C6—C50.3 (7)
C44—Ru1—Ru2—C47152.12 (17)As1—C1—C6—C5180.0 (4)
As1—Ru1—Ru2—C47−115.48 (11)C4—C5—C6—C1−0.8 (8)
Ru3—Ru1—Ru2—C4783.36 (11)C1—As1—C7—C1220.0 (4)
C45—Ru1—Ru2—C49−139.9 (5)C13—As1—C7—C12−88.0 (3)
C46—Ru1—Ru2—C49157.58 (16)Ru1—As1—C7—C12149.1 (3)
C44—Ru1—Ru2—C49−24.55 (17)C1—As1—C7—C8−162.4 (3)
As1—Ru1—Ru2—C4967.84 (11)C13—As1—C7—C889.6 (3)
Ru3—Ru1—Ru2—C49−93.32 (11)Ru1—As1—C7—C8−33.3 (4)
C45—Ru1—Ru2—As2132.0 (5)C12—C7—C8—C90.1 (6)
C46—Ru1—Ru2—As269.46 (12)As1—C7—C8—C9−177.5 (3)
C44—Ru1—Ru2—As2−112.67 (12)C7—C8—C9—C10−0.6 (7)
As1—Ru1—Ru2—As2−20.274 (16)C8—C9—C10—C110.3 (8)
Ru3—Ru1—Ru2—As2178.567 (15)C9—C10—C11—C120.4 (8)
C45—Ru1—Ru2—Ru3−46.6 (5)C8—C7—C12—C110.6 (6)
C46—Ru1—Ru2—Ru3−109.10 (12)As1—C7—C12—C11178.2 (3)
C44—Ru1—Ru2—Ru368.77 (12)C10—C11—C12—C7−0.9 (7)
As1—Ru1—Ru2—Ru3161.159 (15)C1—As1—C13—As293.4 (2)
C48—Ru2—Ru3—C51−20.78 (19)C7—As1—C13—As2−162.9 (2)
C47—Ru2—Ru3—C5167.13 (18)Ru1—As1—C13—As2−36.8 (2)
C49—Ru2—Ru3—C51−114.50 (18)C14—As2—C13—As1−110.8 (2)
As2—Ru2—Ru3—C51159.38 (14)C20—As2—C13—As1143.6 (2)
Ru1—Ru2—Ru3—C51163.00 (13)Ru2—As2—C13—As116.9 (2)
C48—Ru2—Ru3—C52−120.56 (19)C20—As2—C14—C1974.5 (3)
C47—Ru2—Ru3—C52−32.66 (18)C13—As2—C14—C19−30.8 (3)
C49—Ru2—Ru3—C52145.72 (18)Ru2—As2—C14—C19−156.5 (3)
As2—Ru2—Ru3—C5259.59 (13)C20—As2—C14—C15−105.4 (3)
Ru1—Ru2—Ru3—C5263.21 (13)C13—As2—C14—C15149.3 (3)
C48—Ru2—Ru3—C5073.68 (18)Ru2—As2—C14—C1523.6 (4)
C47—Ru2—Ru3—C50161.58 (18)C19—C14—C15—C161.0 (7)
C49—Ru2—Ru3—C50−20.05 (18)As2—C14—C15—C16−179.1 (4)
As2—Ru2—Ru3—C50−106.17 (13)C14—C15—C16—C170.8 (8)
Ru1—Ru2—Ru3—C50−102.55 (12)C15—C16—C17—C18−1.2 (9)
C48—Ru2—Ru3—Ru1176.22 (13)C16—C17—C18—C19−0.3 (9)
C47—Ru2—Ru3—Ru1−95.87 (13)C17—C18—C19—C142.2 (8)
C49—Ru2—Ru3—Ru182.50 (12)C15—C14—C19—C18−2.5 (6)
As2—Ru2—Ru3—Ru1−3.62 (4)As2—C14—C19—C18177.6 (3)
C45—Ru1—Ru3—C51138.8 (3)C14—As2—C20—C25−172.9 (4)
C46—Ru1—Ru3—C5144.2 (3)C13—As2—C20—C25−66.0 (4)
C44—Ru1—Ru3—C51−134.4 (3)Ru2—As2—C20—C2558.3 (4)
As1—Ru1—Ru3—C51−64.5 (2)C14—As2—C20—C2110.7 (4)
Ru2—Ru1—Ru3—C51−29.6 (2)C13—As2—C20—C21117.7 (4)
C45—Ru1—Ru3—C5263.9 (2)Ru2—As2—C20—C21−118.1 (3)
C46—Ru1—Ru3—C52−30.7 (2)C25—C20—C21—C22−2.8 (7)
C44—Ru1—Ru3—C52150.7 (2)As2—C20—C21—C22173.5 (4)
As1—Ru1—Ru3—C52−139.41 (14)C20—C21—C22—C230.7 (9)
Ru2—Ru1—Ru3—C52−104.50 (14)C21—C22—C23—C242.0 (11)
C45—Ru1—Ru3—C50−109.03 (19)C22—C23—C24—C25−2.6 (11)
C46—Ru1—Ru3—C50156.34 (19)C21—C20—C25—C242.2 (8)
C44—Ru1—Ru3—C50−22.24 (18)As2—C20—C25—C24−174.2 (5)
As1—Ru1—Ru3—C5047.64 (13)C23—C24—C25—C200.5 (10)
Ru2—Ru1—Ru3—C5082.55 (13)C38—P1—C26—C31−73.2 (4)
C45—Ru1—Ru3—P1−12.55 (15)C32—P1—C26—C3133.7 (4)
C46—Ru1—Ru3—P1−107.18 (14)Ru3—P1—C26—C31160.7 (3)
C44—Ru1—Ru3—P174.23 (14)C38—P1—C26—C27102.0 (4)
As1—Ru1—Ru3—P1144.11 (4)C32—P1—C26—C27−151.1 (3)
Ru2—Ru1—Ru3—P1179.02 (3)Ru3—P1—C26—C27−24.1 (4)
C45—Ru1—Ru3—Ru2168.42 (15)C31—C26—C27—C281.5 (6)
C46—Ru1—Ru3—Ru273.79 (14)P1—C26—C27—C28−173.9 (4)
C44—Ru1—Ru3—Ru2−104.80 (14)C26—C27—C28—C29−2.1 (7)
As1—Ru1—Ru3—Ru2−34.91 (2)C27—C28—C29—C301.0 (7)
C45—Ru1—As1—C197.1 (2)C27—C28—C29—C53179.1 (4)
C46—Ru1—As1—C1−172.78 (19)C28—C29—C30—C310.7 (7)
C44—Ru1—As1—C14.23 (19)C53—C29—C30—C31−177.4 (4)
Ru2—Ru1—As1—C1−89.97 (14)C29—C30—C31—C26−1.2 (7)
Ru3—Ru1—As1—C1−60.41 (14)C27—C26—C31—C300.1 (6)
C45—Ru1—As1—C7−23.72 (18)P1—C26—C31—C30175.5 (3)
C46—Ru1—As1—C766.35 (18)C38—P1—C32—C33−172.6 (3)
C44—Ru1—As1—C7−116.65 (17)C26—P1—C32—C3381.4 (3)
Ru2—Ru1—As1—C7149.15 (11)Ru3—P1—C32—C33−45.9 (4)
Ru3—Ru1—As1—C7178.72 (11)C38—P1—C32—C3710.7 (4)
C45—Ru1—As1—C13−138.62 (18)C26—P1—C32—C37−95.3 (4)
C46—Ru1—As1—C13−48.55 (18)Ru3—P1—C32—C37137.4 (3)
C44—Ru1—As1—C13128.46 (18)C37—C32—C33—C34−1.4 (6)
Ru2—Ru1—As1—C1334.26 (12)P1—C32—C33—C34−178.3 (3)
Ru3—Ru1—As1—C1363.83 (13)C32—C33—C34—C350.7 (7)
C48—Ru2—As2—C14−50.20 (18)C33—C34—C35—C360.7 (7)
C47—Ru2—As2—C14−139.99 (18)C33—C34—C35—C54−179.6 (4)
C49—Ru2—As2—C1443.38 (18)C34—C35—C36—C37−1.3 (7)
Ru3—Ru2—As2—C14129.64 (13)C54—C35—C36—C37179.0 (4)
Ru1—Ru2—As2—C14126.47 (12)C33—C32—C37—C360.8 (6)
C48—Ru2—As2—C2071.2 (2)P1—C32—C37—C36177.5 (3)
C47—Ru2—As2—C20−18.6 (2)C35—C36—C37—C320.6 (7)
C49—Ru2—As2—C20164.7 (2)C26—P1—C38—C43−19.2 (3)
Ru3—Ru2—As2—C20−108.99 (16)C32—P1—C38—C43−124.1 (3)
Ru1—Ru2—As2—C20−112.17 (16)Ru3—P1—C38—C43108.2 (3)
C48—Ru2—As2—C13−170.87 (18)C26—P1—C38—C39165.4 (3)
C47—Ru2—As2—C1399.34 (18)C32—P1—C38—C3960.5 (3)
C49—Ru2—As2—C13−77.29 (17)Ru3—P1—C38—C39−67.3 (3)
Ru3—Ru2—As2—C138.97 (13)C43—C38—C39—C401.3 (6)
Ru1—Ru2—As2—C135.80 (12)P1—C38—C39—C40176.9 (3)
C51—Ru3—P1—C38−158.16 (19)C38—C39—C40—C41−1.3 (6)
C52—Ru3—P1—C38−58.46 (18)C39—C40—C41—C420.8 (6)
C50—Ru3—P1—C38107.27 (18)C39—C40—C41—C55−177.9 (4)
Ru1—Ru3—P1—C385.28 (14)C40—C41—C42—C43−0.2 (6)
C51—Ru3—P1—C26−38.36 (19)C55—C41—C42—C43178.5 (4)
C52—Ru3—P1—C2661.34 (19)C39—C38—C43—C42−0.7 (5)
C50—Ru3—P1—C26−132.93 (19)P1—C38—C43—C42−176.2 (3)
Ru1—Ru3—P1—C26125.07 (14)C41—C42—C43—C380.2 (6)
C51—Ru3—P1—C3280.77 (19)C45—Ru1—C44—O1−52 (2)
C52—Ru3—P1—C32−179.52 (19)As1—Ru1—C44—O150 (2)
C50—Ru3—P1—C32−13.79 (19)Ru2—Ru1—C44—O1141 (2)
Ru1—Ru3—P1—C32−115.79 (14)Ru3—Ru1—C44—O1−162 (2)
C7—As1—C1—C6−112.1 (4)C51—Ru3—C52—O949.9 (18)
C13—As1—C1—C6−9.9 (4)C50—Ru3—C52—O9−136.1 (16)
Ru1—As1—C1—C6118.2 (3)P1—Ru3—C52—O9−46.3 (18)
C7—As1—C1—C267.5 (3)Ru2—Ru3—C52—O9137.7 (18)
C13—As1—C1—C2169.7 (3)Ru1—Ru3—C52—O9−165.5 (19)
D—H···AD—HH···AD···AD—H···A
C27—H27A···O90.932.573.317 (5)138
C54—H54A···O2i0.962.603.306 (6)131
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
C27—H27A⋯O90.932.573.317 (5)138
C54—H54A⋯O2i0.962.603.306 (6)131

Symmetry code: (i) .

  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-phosphino)methane-1:2κP:P']nonacarbonyl-1κC,2κC,3κC-[tris-(4-methyl-phen-yl)arsine-3κAs]-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

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