Literature DB >> 21579649

[μ-Bis(diphenyl-arsino)methane-1:2κAs:As'][(4-bromo-phen-yl)diphenyl-phosphine-3κP]nona-carbonyl-1κC,2κC,3κC-triangulo-tri-ruthenium(0) chloro-form 0.3-solvate.

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

Abstract

The asymmetric unit of the title triangulo-triruthenium compound, [Ru(3)(C(25)H(22)As(2))(C(18)H(14)BrP)(CO)(9)]·0.3CHCl(3), contains one mol-ecule of the triangulo-triruthenium complex and one partially occupied disordered chloro-form solvent mol-ecule. The bis-(diphenyl-arsino)methane ligand bridges an Ru-Ru bond and the monodentate phosphine ligand bonds to the third Ru atom. Both the arsine and phosphine 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 phosphine-substituted benzene rings make dihedral angles of 67.5 (3), 76.1 (3) and 78.1 (3)° with each other. The dihedral angles between the two benzene rings are 79.0 (4) and 81.4 (3)° for the two diphenyl-arsino groups. In the crystal packing, the mol-ecules are linked into chains along the a axis by inter-molecular C-H⋯O hydrogen bonds.

Entities:  

Year:  2010        PMID: 21579649      PMCID: PMC2979922          DOI: 10.1107/S1600536809055287

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 ▶, 2009 ▶). For the synthesis of μ-bis­(diphenyl­arsino)methane­deca­carbonyl­triruthenium(0), see: Bruce et al. (1983 ▶).

Experimental

Crystal data

[Ru3(C25H22As2)(C18H14BrP)(CO)9]·0.3CHCl3 M = 1404.55 Monoclinic, a = 13.2415 (2) Å b = 16.9463 (3) Å c = 25.2224 (4) Å β = 91.831 (1)° V = 5656.88 (16) Å3 Z = 4 Mo Kα radiation μ = 2.78 mm−1 T = 296 K 0.26 × 0.26 × 0.16 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2005 ▶) T min = 0.537, T max = 0.673 63188 measured reflections 16521 independent reflections 10783 reflections with I > 2σ(I) R int = 0.042

Refinement

R[F 2 > 2σ(F 2)] = 0.048 wR(F 2) = 0.169 S = 1.08 16521 reflections 677 parameters 6 restraints H-atom parameters constrained Δρmax = 1.41 e Å−3 Δρmin = −1.35 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/S1600536809055287/rz2406sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809055287/rz2406Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ru3(C25H22As2)(C18H14BrP)(CO)9]·0.3CHCl3F(000) = 2742
Mr = 1404.55Dx = 1.649 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9923 reflections
a = 13.2415 (2) Åθ = 2.2–27.8°
b = 16.9463 (3) ŵ = 2.78 mm1
c = 25.2224 (4) ÅT = 296 K
β = 91.831 (1)°Block, purple
V = 5656.88 (16) Å30.26 × 0.26 × 0.16 mm
Z = 4
Bruker SMART APEXII CCD area-detector diffractometer16521 independent reflections
Radiation source: fine-focus sealed tube10783 reflections with I > 2σ(I)
graphiteRint = 0.042
φ and ω scansθmax = 30.1°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Bruker, 2005)h = −15→18
Tmin = 0.537, Tmax = 0.673k = −23→23
63188 measured reflectionsl = −34→35
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.169H-atom parameters constrained
S = 1.08w = 1/[σ2(Fo2) + (0.0909P)2 + 1.7904P] where P = (Fo2 + 2Fc2)/3
16521 reflections(Δ/σ)max < 0.001
677 parametersΔρmax = 1.41 e Å3
6 restraintsΔρmin = −1.35 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*/UeqOcc. (<1)
Ru10.23647 (3)0.31292 (2)0.159957 (17)0.03734 (11)
Ru20.04996 (3)0.23846 (2)0.182974 (15)0.03237 (10)
Ru30.19834 (3)0.15122 (2)0.129329 (15)0.03373 (11)
As10.16719 (4)0.44257 (3)0.18017 (2)0.03586 (13)
As2−0.01816 (3)0.34651 (3)0.234290 (19)0.03180 (12)
P10.31671 (10)0.08260 (8)0.07993 (5)0.0391 (3)
Br10.73998 (7)0.26067 (7)0.03555 (5)0.1197 (4)
O10.1908 (4)0.3326 (3)0.04092 (18)0.0692 (13)
O20.4533 (4)0.3563 (4)0.1392 (3)0.128 (3)
O30.2858 (4)0.2977 (3)0.2792 (2)0.0750 (14)
O40.1342 (4)0.1548 (3)0.28246 (18)0.0709 (13)
O5−0.1249 (4)0.1225 (3)0.1762 (2)0.0891 (17)
O6−0.0303 (3)0.3221 (3)0.08269 (17)0.0646 (12)
O70.0669 (4)0.1772 (3)0.02798 (19)0.0770 (14)
O80.0746 (3)0.0079 (3)0.15645 (19)0.0663 (12)
O90.3573 (3)0.1471 (2)0.21969 (19)0.0634 (12)
C10.2604 (4)0.5220 (3)0.2096 (2)0.0463 (13)
C20.2406 (5)0.6013 (4)0.2031 (3)0.0702 (19)
H2A0.18400.61750.18320.084*
C30.3065 (6)0.6578 (4)0.2265 (4)0.089 (3)
H3A0.29340.71140.22220.107*
C40.3881 (6)0.6337 (5)0.2549 (4)0.088 (3)
H4A0.43150.67090.27030.106*
C50.4079 (6)0.5570 (5)0.2613 (4)0.096 (3)
H5A0.46440.54160.28150.115*
C60.3448 (5)0.4995 (4)0.2380 (3)0.080 (2)
H6A0.36040.44630.24190.096*
C70.1009 (4)0.5021 (3)0.1233 (2)0.0451 (12)
C80.0047 (5)0.5283 (5)0.1246 (3)0.076 (2)
H8A−0.03450.51710.15350.091*
C9−0.0355 (7)0.5722 (6)0.0823 (4)0.105 (3)
H9A−0.10210.58940.08370.125*
C100.0150 (8)0.5901 (6)0.0414 (4)0.095 (3)
H10A−0.01500.61980.01410.115*
C110.1142 (8)0.5653 (5)0.0379 (3)0.093 (3)
H11A0.15170.57850.00860.111*
C120.1568 (5)0.5199 (4)0.0791 (3)0.0703 (19)
H12A0.22270.50150.07700.084*
C130.0693 (4)0.4407 (3)0.2370 (2)0.0373 (11)
H13A0.02730.48760.23430.045*
H13B0.10550.44230.27100.045*
C14−0.0395 (4)0.3275 (3)0.30969 (19)0.0376 (11)
C150.0424 (4)0.3164 (4)0.3438 (2)0.0564 (16)
H15A0.10770.31970.33150.068*
C160.0267 (5)0.3004 (5)0.3969 (2)0.069 (2)
H16A0.08200.29270.42000.083*
C17−0.0679 (6)0.2958 (4)0.4156 (3)0.0707 (19)
H17A−0.07700.28530.45130.085*
C18−0.1519 (5)0.3068 (5)0.3813 (3)0.0681 (19)
H18A−0.21710.30370.39380.082*
C19−0.1358 (4)0.3225 (4)0.3283 (2)0.0511 (14)
H19A−0.19090.32970.30500.061*
C20−0.1490 (3)0.3869 (3)0.21020 (19)0.0368 (11)
C21−0.2132 (4)0.3360 (4)0.1828 (3)0.0545 (15)
H21A−0.19240.28480.17550.065*
C22−0.3100 (4)0.3616 (4)0.1660 (3)0.069 (2)
H22A−0.35310.32770.14710.083*
C23−0.3408 (4)0.4376 (4)0.1778 (3)0.0614 (17)
H23A−0.40500.45480.16710.074*
C24−0.2765 (4)0.4878 (3)0.2054 (2)0.0501 (14)
H24A−0.29680.53890.21320.060*
C25−0.1817 (4)0.4617 (3)0.2214 (2)0.0428 (12)
H25A−0.13870.49580.24020.051*
C260.4375 (4)0.1316 (3)0.0694 (2)0.0433 (12)
C270.4367 (5)0.2075 (4)0.0496 (2)0.0574 (15)
H27A0.37550.23320.04280.069*
C280.5284 (5)0.2465 (4)0.0394 (3)0.0693 (19)
H28A0.52810.29680.02480.083*
C290.6169 (5)0.2092 (5)0.0514 (3)0.069 (2)
C300.6201 (5)0.1363 (5)0.0732 (3)0.077 (2)
H30A0.68170.11300.08270.092*
C310.5310 (4)0.0971 (4)0.0813 (3)0.0603 (16)
H31A0.53320.04610.09500.072*
C320.2688 (4)0.0565 (3)0.0135 (2)0.0468 (13)
C330.1857 (5)0.0077 (4)0.0086 (3)0.0665 (18)
H33A0.1581−0.01310.03900.080*
C340.1424 (5)−0.0111 (5)−0.0403 (4)0.086 (3)
H34A0.0866−0.0443−0.04280.103*
C350.1842 (7)0.0212 (5)−0.0873 (3)0.088 (3)
H35A0.15600.0090−0.12060.105*
C360.2638 (7)0.0686 (5)−0.0828 (3)0.084 (2)
H36A0.29100.0898−0.11320.101*
C370.3079 (5)0.0874 (4)−0.0327 (2)0.0645 (17)
H37A0.36360.1207−0.03050.077*
C380.3574 (4)−0.0136 (3)0.1050 (2)0.0433 (12)
C390.3556 (4)−0.0316 (4)0.1587 (2)0.0523 (14)
H39A0.32770.00440.18190.063*
C400.3944 (5)−0.1020 (4)0.1784 (3)0.0623 (17)
H40A0.3925−0.11310.21450.075*
C410.4354 (5)−0.1553 (4)0.1442 (3)0.0685 (19)
H41A0.4647−0.20150.15740.082*
C420.4335 (5)−0.1402 (4)0.0897 (3)0.071 (2)
H42A0.4572−0.17770.06630.085*
C430.3966 (5)−0.0703 (4)0.0715 (2)0.0571 (16)
H43A0.3974−0.06000.03530.069*
C440.2033 (4)0.3203 (3)0.0846 (3)0.0491 (14)
C450.3714 (4)0.3393 (4)0.1466 (3)0.0670 (19)
C460.2647 (5)0.2992 (3)0.2354 (3)0.0525 (14)
C470.1078 (4)0.1867 (3)0.2453 (2)0.0475 (13)
C48−0.0591 (4)0.1669 (3)0.1799 (3)0.0513 (14)
C490.0046 (4)0.2904 (3)0.1191 (2)0.0431 (12)
C500.1146 (4)0.1708 (4)0.0662 (2)0.0481 (13)
C510.1244 (4)0.0604 (3)0.1463 (2)0.0428 (12)
C520.2949 (4)0.1556 (3)0.1875 (2)0.0442 (12)
Cl1A0.3768 (15)0.4277 (14)−0.0348 (9)0.097 (6)0.15
Cl2A0.5082 (16)0.3887 (11)−0.1025 (9)0.118 (7)0.15
Cl3A0.326 (2)0.3053 (11)−0.0909 (11)0.102 (7)0.15
C53A0.393 (2)0.382 (2)−0.0880 (16)0.073 (13)*0.15
H53A0.35970.4163−0.11450.088*0.15
Cl1B0.3361 (12)0.4365 (13)−0.0503 (7)0.084 (5)0.15
Cl2B0.4565 (12)0.3670 (9)−0.1348 (7)0.085 (5)0.15
Cl3B0.3069 (15)0.2742 (9)−0.0856 (6)0.064 (4)0.15
C53B0.348 (2)0.3668 (12)−0.0994 (11)0.042 (8)*0.15
H53B0.29710.3845−0.12600.051*0.15
U11U22U33U12U13U23
Ru10.03017 (19)0.0334 (2)0.0485 (3)−0.00255 (15)0.00296 (16)−0.00460 (18)
Ru20.03149 (19)0.0291 (2)0.0367 (2)−0.00158 (14)0.00485 (15)−0.00434 (16)
Ru30.03338 (19)0.0313 (2)0.0368 (2)0.00096 (15)0.00430 (15)−0.00422 (16)
As10.0338 (2)0.0305 (3)0.0433 (3)−0.00346 (19)0.0004 (2)−0.0003 (2)
As20.0318 (2)0.0296 (3)0.0341 (3)0.00008 (18)0.00137 (19)−0.0033 (2)
P10.0365 (6)0.0405 (7)0.0407 (7)−0.0001 (5)0.0085 (5)−0.0065 (6)
Br10.0793 (6)0.1379 (9)0.1450 (9)−0.0582 (6)0.0501 (6)−0.0405 (7)
O10.082 (3)0.077 (3)0.049 (3)−0.009 (3)0.007 (2)0.007 (2)
O20.047 (3)0.155 (6)0.182 (7)−0.041 (3)0.029 (4)−0.067 (5)
O30.106 (4)0.060 (3)0.058 (3)0.003 (3)−0.017 (3)−0.005 (2)
O40.094 (4)0.061 (3)0.057 (3)0.022 (3)−0.002 (2)0.015 (2)
O50.062 (3)0.061 (3)0.147 (5)−0.029 (2)0.029 (3)−0.022 (3)
O60.054 (2)0.085 (3)0.054 (3)0.009 (2)−0.001 (2)0.010 (2)
O70.090 (3)0.082 (4)0.058 (3)0.016 (3)−0.022 (3)−0.008 (3)
O80.069 (3)0.046 (3)0.084 (3)−0.013 (2)0.006 (2)0.007 (2)
O90.060 (3)0.049 (3)0.080 (3)0.013 (2)−0.027 (2)−0.013 (2)
C10.039 (3)0.040 (3)0.059 (4)−0.010 (2)−0.001 (2)−0.005 (3)
C20.065 (4)0.042 (4)0.102 (6)−0.003 (3)−0.022 (4)−0.005 (4)
C30.077 (5)0.042 (4)0.146 (8)−0.015 (3)−0.027 (5)−0.014 (4)
C40.064 (4)0.060 (5)0.139 (8)−0.016 (4)−0.027 (5)−0.030 (5)
C50.083 (5)0.062 (5)0.138 (8)−0.008 (4)−0.059 (5)−0.002 (5)
C60.071 (4)0.040 (4)0.126 (7)−0.008 (3)−0.044 (4)0.002 (4)
C70.051 (3)0.038 (3)0.046 (3)−0.004 (2)−0.001 (2)0.004 (2)
C80.058 (4)0.095 (6)0.074 (5)0.013 (4)0.001 (3)0.038 (4)
C90.089 (6)0.122 (8)0.100 (7)0.030 (5)−0.021 (5)0.050 (6)
C100.111 (7)0.098 (7)0.075 (6)0.008 (6)−0.026 (5)0.043 (5)
C110.158 (9)0.073 (5)0.048 (4)−0.024 (6)0.005 (5)0.019 (4)
C120.075 (4)0.071 (5)0.065 (4)−0.006 (4)0.008 (3)0.018 (4)
C130.042 (3)0.036 (3)0.035 (3)−0.003 (2)0.002 (2)−0.004 (2)
C140.044 (3)0.033 (3)0.036 (3)−0.002 (2)0.005 (2)−0.003 (2)
C150.047 (3)0.082 (5)0.041 (3)0.008 (3)0.001 (2)−0.002 (3)
C160.062 (4)0.109 (6)0.037 (3)0.005 (4)−0.005 (3)0.009 (3)
C170.083 (5)0.082 (5)0.047 (4)−0.008 (4)0.013 (3)0.007 (4)
C180.064 (4)0.088 (5)0.053 (4)−0.008 (4)0.015 (3)0.005 (4)
C190.042 (3)0.064 (4)0.048 (3)−0.004 (3)0.001 (2)0.004 (3)
C200.034 (2)0.041 (3)0.036 (3)0.002 (2)−0.0006 (19)−0.003 (2)
C210.041 (3)0.049 (3)0.073 (4)0.003 (2)−0.007 (3)−0.019 (3)
C220.036 (3)0.073 (5)0.097 (5)0.004 (3)−0.017 (3)−0.028 (4)
C230.039 (3)0.072 (4)0.073 (4)0.017 (3)−0.009 (3)0.000 (3)
C240.046 (3)0.041 (3)0.063 (4)0.008 (2)−0.006 (3)−0.001 (3)
C250.040 (3)0.038 (3)0.049 (3)−0.001 (2)−0.004 (2)−0.005 (2)
C260.038 (3)0.053 (3)0.039 (3)−0.004 (2)0.005 (2)−0.009 (2)
C270.055 (3)0.055 (4)0.063 (4)−0.004 (3)0.013 (3)−0.002 (3)
C280.072 (4)0.063 (4)0.074 (5)−0.017 (3)0.026 (4)0.001 (3)
C290.045 (3)0.089 (5)0.075 (5)−0.028 (3)0.026 (3)−0.027 (4)
C300.044 (3)0.094 (6)0.094 (6)−0.013 (4)0.012 (3)−0.014 (5)
C310.046 (3)0.066 (4)0.070 (4)0.001 (3)0.001 (3)0.000 (3)
C320.043 (3)0.050 (3)0.047 (3)0.003 (2)0.000 (2)−0.015 (3)
C330.058 (4)0.069 (4)0.073 (5)−0.003 (3)0.002 (3)−0.020 (4)
C340.061 (4)0.085 (6)0.110 (7)−0.001 (4)−0.023 (4)−0.042 (5)
C350.108 (7)0.086 (6)0.068 (5)0.016 (5)−0.029 (5)−0.029 (5)
C360.108 (6)0.091 (6)0.051 (4)0.007 (5)−0.012 (4)−0.011 (4)
C370.065 (4)0.080 (5)0.049 (4)0.003 (3)0.002 (3)−0.010 (3)
C380.040 (3)0.039 (3)0.051 (3)0.003 (2)0.010 (2)−0.004 (2)
C390.057 (3)0.046 (3)0.054 (4)0.008 (3)0.008 (3)−0.008 (3)
C400.077 (4)0.050 (4)0.061 (4)0.011 (3)0.012 (3)0.003 (3)
C410.069 (4)0.044 (4)0.093 (5)0.017 (3)0.016 (4)0.004 (4)
C420.079 (5)0.049 (4)0.087 (5)0.016 (3)0.034 (4)−0.008 (4)
C430.070 (4)0.050 (4)0.053 (4)0.014 (3)0.018 (3)−0.007 (3)
C440.041 (3)0.048 (3)0.058 (4)−0.008 (2)0.011 (3)−0.004 (3)
C450.040 (3)0.069 (4)0.092 (5)−0.011 (3)0.007 (3)−0.020 (4)
C460.060 (4)0.037 (3)0.060 (4)0.006 (3)−0.004 (3)−0.001 (3)
C470.053 (3)0.037 (3)0.053 (4)0.008 (2)0.008 (3)−0.003 (3)
C480.043 (3)0.042 (3)0.070 (4)−0.005 (2)0.014 (3)−0.010 (3)
C490.035 (2)0.051 (3)0.044 (3)0.000 (2)0.001 (2)−0.001 (3)
C500.049 (3)0.051 (3)0.044 (3)0.007 (3)0.000 (3)−0.007 (3)
C510.041 (3)0.041 (3)0.046 (3)0.002 (2)0.001 (2)0.000 (2)
C520.047 (3)0.035 (3)0.051 (3)0.002 (2)−0.002 (2)−0.011 (2)
Cl1A0.087 (13)0.096 (12)0.106 (14)0.037 (11)−0.019 (10)0.010 (10)
Cl2A0.130 (16)0.092 (12)0.136 (17)0.018 (11)0.087 (13)0.028 (12)
Cl3A0.117 (16)0.054 (12)0.135 (17)0.003 (10)−0.007 (12)0.008 (11)
Cl1B0.062 (9)0.110 (13)0.081 (11)0.027 (9)0.012 (8)0.000 (9)
Cl2B0.098 (11)0.060 (8)0.099 (11)0.058 (8)0.034 (8)0.020 (8)
Cl3B0.090 (9)0.046 (9)0.054 (7)−0.010 (7)−0.012 (6)0.027 (7)
Ru1—C451.883 (6)C15—C161.388 (8)
Ru1—C441.940 (7)C15—H15A0.9300
Ru1—C461.942 (7)C16—C171.354 (9)
Ru1—As12.4410 (6)C16—H16A0.9300
Ru1—Ru22.8495 (5)C17—C181.400 (10)
Ru1—Ru32.8870 (6)C17—H17A0.9300
Ru2—C481.885 (6)C18—C191.386 (8)
Ru2—C491.915 (6)C18—H18A0.9300
Ru2—C471.935 (6)C19—H19A0.9300
Ru2—As22.4323 (6)C20—C251.371 (7)
Ru2—Ru32.8366 (5)C20—C211.382 (7)
Ru3—C511.880 (5)C21—C221.405 (8)
Ru3—C521.916 (6)C21—H21A0.9300
Ru3—C501.940 (6)C22—C231.388 (9)
Ru3—P12.3423 (13)C22—H22A0.9300
As1—C71.941 (5)C23—C241.376 (8)
As1—C11.957 (5)C23—H23A0.9300
As1—C131.964 (5)C24—C251.379 (7)
As2—C201.942 (5)C24—H24A0.9300
As2—C141.958 (5)C25—H25A0.9300
As2—C131.972 (5)C26—C271.381 (8)
P1—C381.823 (6)C26—C311.393 (8)
P1—C321.828 (6)C27—C281.412 (8)
P1—C261.828 (5)C27—H27A0.9300
Br1—C291.902 (6)C28—C291.358 (10)
O1—C441.129 (7)C28—H28A0.9300
O2—C451.143 (7)C29—C301.352 (11)
O3—C461.132 (7)C30—C311.375 (9)
O4—C471.130 (7)C30—H30A0.9300
O5—C481.153 (7)C31—H31A0.9300
O6—C491.149 (6)C32—C331.380 (8)
O7—C501.140 (7)C32—C371.390 (8)
O8—C511.142 (6)C33—C341.381 (10)
O9—C521.149 (6)C33—H33A0.9300
C1—C61.362 (8)C34—C351.433 (12)
C1—C21.378 (8)C34—H34A0.9300
C2—C31.412 (9)C35—C361.326 (11)
C2—H2A0.9300C35—H35A0.9300
C3—C41.342 (10)C36—C371.412 (9)
C3—H3A0.9300C36—H36A0.9300
C4—C51.333 (11)C37—H37A0.9300
C4—H4A0.9300C38—C391.390 (8)
C5—C61.401 (9)C38—C431.390 (7)
C5—H5A0.9300C39—C401.385 (8)
C6—H6A0.9300C39—H39A0.9300
C7—C81.349 (8)C40—C411.372 (9)
C7—C121.390 (8)C40—H40A0.9300
C8—C91.393 (10)C41—C421.397 (10)
C8—H8A0.9300C41—H41A0.9300
C9—C101.283 (12)C42—C431.356 (9)
C9—H9A0.9300C42—H42A0.9300
C10—C111.385 (12)C43—H43A0.9300
C10—H10A0.9300Cl1A—C53A1.57 (2)
C11—C121.398 (10)Cl2A—C53A1.58 (2)
C11—H11A0.9300Cl3A—C53A1.58 (2)
C12—H12A0.9300C53A—H53A0.9800
C13—H13A0.9700Cl1B—C53B1.721 (17)
C13—H13B0.9700Cl2B—C53B1.720 (16)
C14—C151.375 (7)Cl3B—C53B1.699 (16)
C14—C191.376 (7)C53B—H53B0.9800
C45—Ru1—C4489.8 (3)C14—C15—C16119.4 (6)
C45—Ru1—C4692.9 (3)C14—C15—H15A120.3
C44—Ru1—C46176.3 (2)C16—C15—H15A120.3
C45—Ru1—As1100.9 (2)C17—C16—C15121.0 (6)
C44—Ru1—As194.12 (17)C17—C16—H16A119.5
C46—Ru1—As187.98 (17)C15—C16—H16A119.5
C45—Ru1—Ru2167.2 (2)C16—C17—C18120.2 (6)
C44—Ru1—Ru293.30 (15)C16—C17—H17A119.9
C46—Ru1—Ru283.58 (18)C18—C17—H17A119.9
As1—Ru1—Ru291.263 (18)C19—C18—C17118.5 (6)
C45—Ru1—Ru3109.7 (2)C19—C18—H18A120.7
C44—Ru1—Ru376.52 (17)C17—C18—H18A120.7
C46—Ru1—Ru3100.10 (17)C14—C19—C18120.9 (6)
As1—Ru1—Ru3147.83 (2)C14—C19—H19A119.5
Ru2—Ru1—Ru359.268 (13)C18—C19—H19A119.5
C48—Ru2—C4992.4 (3)C25—C20—C21119.1 (5)
C48—Ru2—C4791.4 (3)C25—C20—As2123.1 (4)
C49—Ru2—C47175.0 (2)C21—C20—As2117.7 (4)
C48—Ru2—As2102.07 (17)C20—C21—C22119.9 (5)
C49—Ru2—As289.41 (16)C20—C21—H21A120.0
C47—Ru2—As293.03 (16)C22—C21—H21A120.0
C48—Ru2—Ru3100.77 (17)C23—C22—C21119.6 (6)
C49—Ru2—Ru392.41 (15)C23—C22—H22A120.2
C47—Ru2—Ru383.63 (15)C21—C22—H22A120.2
As2—Ru2—Ru3156.99 (2)C24—C23—C22120.1 (5)
C48—Ru2—Ru1160.77 (17)C24—C23—H23A120.0
C49—Ru2—Ru182.88 (15)C22—C23—H23A120.0
C47—Ru2—Ru192.46 (17)C23—C24—C25119.5 (5)
As2—Ru2—Ru196.525 (18)C23—C24—H24A120.2
Ru3—Ru2—Ru161.024 (13)C25—C24—H24A120.2
C51—Ru3—C52101.4 (2)C20—C25—C24121.8 (5)
C51—Ru3—C5092.2 (2)C20—C25—H25A119.1
C52—Ru3—C50166.3 (2)C24—C25—H25A119.1
C51—Ru3—P194.43 (16)C27—C26—C31117.7 (5)
C52—Ru3—P189.15 (16)C27—C26—P1118.6 (4)
C50—Ru3—P191.29 (16)C31—C26—P1123.6 (5)
C51—Ru3—Ru286.79 (16)C26—C27—C28120.3 (6)
C52—Ru3—Ru294.01 (15)C26—C27—H27A119.8
C50—Ru3—Ru285.20 (16)C28—C27—H27A119.8
P1—Ru3—Ru2176.33 (4)C29—C28—C27118.9 (7)
C51—Ru3—Ru1143.46 (16)C29—C28—H28A120.5
C52—Ru3—Ru169.60 (16)C27—C28—H28A120.5
C50—Ru3—Ru198.52 (18)C30—C29—C28122.1 (6)
P1—Ru3—Ru1119.95 (4)C30—C29—Br1119.3 (6)
Ru2—Ru3—Ru159.708 (13)C28—C29—Br1118.6 (6)
C7—As1—C1100.8 (2)C29—C30—C31119.1 (7)
C7—As1—C13104.7 (2)C29—C30—H30A120.4
C1—As1—C1399.0 (2)C31—C30—H30A120.4
C7—As1—Ru1118.55 (17)C30—C31—C26121.7 (7)
C1—As1—Ru1117.51 (16)C30—C31—H31A119.1
C13—As1—Ru1113.54 (15)C26—C31—H31A119.1
C20—As2—C14102.0 (2)C33—C32—C37117.9 (6)
C20—As2—C13104.0 (2)C33—C32—P1118.6 (5)
C14—As2—C13101.7 (2)C37—C32—P1123.3 (5)
C20—As2—Ru2116.18 (14)C32—C33—C34121.7 (7)
C14—As2—Ru2117.40 (15)C32—C33—H33A119.2
C13—As2—Ru2113.62 (14)C34—C33—H33A119.2
C38—P1—C32101.1 (3)C33—C34—C35119.4 (7)
C38—P1—C26101.9 (3)C33—C34—H34A120.3
C32—P1—C26104.9 (2)C35—C34—H34A120.3
C38—P1—Ru3117.08 (17)C36—C35—C34119.1 (7)
C32—P1—Ru3112.92 (17)C36—C35—H35A120.4
C26—P1—Ru3117.05 (18)C34—C35—H35A120.4
C6—C1—C2119.0 (5)C35—C36—C37121.2 (8)
C6—C1—As1120.3 (5)C35—C36—H36A119.4
C2—C1—As1120.7 (4)C37—C36—H36A119.4
C1—C2—C3119.9 (6)C32—C37—C36120.7 (7)
C1—C2—H2A120.0C32—C37—H37A119.7
C3—C2—H2A120.0C36—C37—H37A119.7
C4—C3—C2119.5 (7)C39—C38—C43117.3 (5)
C4—C3—H3A120.2C39—C38—P1121.3 (4)
C2—C3—H3A120.2C43—C38—P1121.3 (4)
C5—C4—C3120.9 (7)C40—C39—C38121.4 (5)
C5—C4—H4A119.6C40—C39—H39A119.3
C3—C4—H4A119.6C38—C39—H39A119.3
C4—C5—C6121.0 (7)C41—C40—C39119.4 (6)
C4—C5—H5A119.5C41—C40—H40A120.3
C6—C5—H5A119.5C39—C40—H40A120.3
C1—C6—C5119.6 (6)C40—C41—C42120.1 (6)
C1—C6—H6A120.2C40—C41—H41A119.9
C5—C6—H6A120.2C42—C41—H41A119.9
C8—C7—C12118.3 (6)C43—C42—C41119.3 (6)
C8—C7—As1123.9 (5)C43—C42—H42A120.4
C12—C7—As1117.7 (5)C41—C42—H42A120.4
C7—C8—C9119.7 (7)C42—C43—C38122.3 (6)
C7—C8—H8A120.1C42—C43—H43A118.8
C9—C8—H8A120.1C38—C43—H43A118.8
C10—C9—C8123.0 (9)O1—C44—Ru1171.8 (5)
C10—C9—H9A118.5O2—C45—Ru1178.8 (7)
C8—C9—H9A118.5O3—C46—Ru1173.6 (6)
C9—C10—C11119.9 (8)O4—C47—Ru2174.7 (5)
C9—C10—H10A120.0O5—C48—Ru2177.5 (6)
C11—C10—H10A120.0O6—C49—Ru2174.3 (5)
C10—C11—C12118.7 (7)O7—C50—Ru3175.4 (5)
C10—C11—H11A120.7O8—C51—Ru3176.1 (5)
C12—C11—H11A120.7O9—C52—Ru3169.5 (5)
C7—C12—C11120.2 (7)Cl1A—C53A—Cl3A111 (2)
C7—C12—H12A119.9Cl1A—C53A—Cl2A109 (2)
C11—C12—H12A119.9Cl3A—C53A—Cl2A127 (2)
As1—C13—As2112.8 (2)Cl1A—C53A—H53A102.5
As1—C13—H13A109.0Cl3A—C53A—H53A102.5
As2—C13—H13A109.0Cl2A—C53A—H53A102.5
As1—C13—H13B109.0Cl3B—C53B—Cl2B112.6 (15)
As2—C13—H13B109.0Cl3B—C53B—Cl1B116.8 (16)
H13A—C13—H13B107.8Cl2B—C53B—Cl1B117.9 (14)
C15—C14—C19119.9 (5)Cl3B—C53B—H53B102.0
C15—C14—As2119.7 (4)Cl2B—C53B—H53B102.0
C19—C14—As2120.4 (4)Cl1B—C53B—H53B102.0
C45—Ru1—Ru2—C48−51.6 (12)C13—As1—C1—C695.6 (6)
C44—Ru1—Ru2—C4852.1 (6)Ru1—As1—C1—C6−27.0 (6)
C46—Ru1—Ru2—C48−125.9 (6)C7—As1—C1—C224.0 (6)
As1—Ru1—Ru2—C48146.3 (6)C13—As1—C1—C2−83.0 (6)
Ru3—Ru1—Ru2—C48−20.1 (6)Ru1—As1—C1—C2154.4 (5)
C45—Ru1—Ru2—C49−128.2 (10)C6—C1—C2—C3−1.2 (11)
C44—Ru1—Ru2—C49−24.6 (2)As1—C1—C2—C3177.4 (6)
C46—Ru1—Ru2—C49157.5 (2)C1—C2—C3—C40.1 (13)
As1—Ru1—Ru2—C4969.63 (17)C2—C3—C4—C50.0 (15)
Ru3—Ru1—Ru2—C49−96.76 (17)C3—C4—C5—C60.8 (16)
C45—Ru1—Ru2—C4749.9 (10)C2—C1—C6—C52.1 (12)
C44—Ru1—Ru2—C47153.5 (2)As1—C1—C6—C5−176.5 (7)
C46—Ru1—Ru2—C47−24.5 (2)C4—C5—C6—C1−1.9 (15)
As1—Ru1—Ru2—C47−112.29 (16)C1—As1—C7—C8−107.4 (6)
Ru3—Ru1—Ru2—C4781.33 (16)C13—As1—C7—C8−5.0 (6)
C45—Ru1—Ru2—As2143.2 (10)Ru1—As1—C7—C8122.8 (6)
C44—Ru1—Ru2—As2−113.15 (17)C1—As1—C7—C1271.4 (5)
C46—Ru1—Ru2—As268.87 (17)C13—As1—C7—C12173.8 (5)
As1—Ru1—Ru2—As2−18.95 (2)Ru1—As1—C7—C12−58.3 (5)
Ru3—Ru1—Ru2—As2174.66 (2)C12—C7—C8—C9−0.3 (12)
C45—Ru1—Ru2—Ru3−31.5 (10)As1—C7—C8—C9178.5 (7)
C44—Ru1—Ru2—Ru372.19 (17)C7—C8—C9—C10−0.5 (16)
C46—Ru1—Ru2—Ru3−105.79 (17)C8—C9—C10—C110.3 (17)
As1—Ru1—Ru2—Ru3166.39 (2)C9—C10—C11—C120.8 (15)
C48—Ru2—Ru3—C51−21.9 (3)C8—C7—C12—C111.4 (10)
C49—Ru2—Ru3—C51−114.8 (2)As1—C7—C12—C11−177.5 (6)
C47—Ru2—Ru3—C5168.3 (2)C10—C11—C12—C7−1.6 (12)
As2—Ru2—Ru3—C51151.05 (17)C7—As1—C13—As292.9 (3)
Ru1—Ru2—Ru3—C51164.73 (17)C1—As1—C13—As2−163.3 (3)
C48—Ru2—Ru3—C52−123.1 (3)Ru1—As1—C13—As2−37.9 (3)
C49—Ru2—Ru3—C52144.0 (2)C20—As2—C13—As1−107.9 (3)
C47—Ru2—Ru3—C52−32.8 (2)C14—As2—C13—As1146.4 (3)
As2—Ru2—Ru3—C5249.86 (17)Ru2—As2—C13—As119.3 (3)
Ru1—Ru2—Ru3—C5263.54 (17)C20—As2—C14—C15−164.4 (5)
C48—Ru2—Ru3—C5070.6 (3)C13—As2—C14—C15−57.1 (5)
C49—Ru2—Ru3—C50−22.3 (2)Ru2—As2—C14—C1567.5 (5)
C47—Ru2—Ru3—C50160.8 (2)C20—As2—C14—C1917.8 (5)
As2—Ru2—Ru3—C50−116.46 (19)C13—As2—C14—C19125.1 (5)
Ru1—Ru2—Ru3—C50−102.79 (18)Ru2—As2—C14—C19−110.3 (4)
C48—Ru2—Ru3—Ru1173.4 (2)C19—C14—C15—C16−0.1 (10)
C49—Ru2—Ru3—Ru180.49 (16)As2—C14—C15—C16−177.9 (5)
C47—Ru2—Ru3—Ru1−96.39 (17)C14—C15—C16—C17−0.3 (11)
As2—Ru2—Ru3—Ru1−13.68 (5)C15—C16—C17—C180.4 (12)
C45—Ru1—Ru3—C51146.7 (4)C16—C17—C18—C19−0.1 (11)
C44—Ru1—Ru3—C51−128.4 (3)C15—C14—C19—C180.3 (9)
C46—Ru1—Ru3—C5150.0 (3)As2—C14—C19—C18178.2 (5)
As1—Ru1—Ru3—C51−52.4 (3)C17—C18—C19—C14−0.3 (10)
Ru2—Ru1—Ru3—C51−26.2 (3)C14—As2—C20—C2574.7 (5)
C45—Ru1—Ru3—C5265.3 (3)C13—As2—C20—C25−30.7 (5)
C44—Ru1—Ru3—C52150.1 (2)Ru2—As2—C20—C25−156.4 (4)
C46—Ru1—Ru3—C52−31.4 (3)C14—As2—C20—C21−102.1 (5)
As1—Ru1—Ru3—C52−133.90 (18)C13—As2—C20—C21152.5 (4)
Ru2—Ru1—Ru3—C52−107.67 (17)Ru2—As2—C20—C2126.8 (5)
C45—Ru1—Ru3—C50−107.7 (3)C25—C20—C21—C221.0 (9)
C44—Ru1—Ru3—C50−22.9 (2)As2—C20—C21—C22177.9 (5)
C46—Ru1—Ru3—C50155.5 (2)C20—C21—C22—C23−0.9 (11)
As1—Ru1—Ru3—C5053.08 (17)C21—C22—C23—C240.6 (11)
Ru2—Ru1—Ru3—C5079.31 (16)C22—C23—C24—C25−0.3 (10)
C45—Ru1—Ru3—P1−11.3 (3)C21—C20—C25—C24−0.8 (8)
C44—Ru1—Ru3—P173.58 (16)As2—C20—C25—C24−177.5 (4)
C46—Ru1—Ru3—P1−107.99 (19)C23—C24—C25—C200.5 (9)
As1—Ru1—Ru3—P1149.55 (6)C38—P1—C26—C27179.3 (5)
Ru2—Ru1—Ru3—P1175.78 (5)C32—P1—C26—C2774.3 (5)
C45—Ru1—Ru3—Ru2173.0 (3)Ru3—P1—C26—C27−51.7 (5)
C44—Ru1—Ru3—Ru2−102.20 (16)C38—P1—C26—C31−1.9 (5)
C46—Ru1—Ru3—Ru276.23 (18)C32—P1—C26—C31−106.8 (5)
As1—Ru1—Ru3—Ru2−26.23 (4)Ru3—P1—C26—C31127.2 (5)
C45—Ru1—As1—C794.2 (3)C31—C26—C27—C283.0 (9)
C44—Ru1—As1—C73.7 (2)P1—C26—C27—C28−178.1 (5)
C46—Ru1—As1—C7−173.3 (3)C26—C27—C28—C29−2.5 (10)
Ru2—Ru1—As1—C7−89.72 (18)C27—C28—C29—C30−0.6 (11)
Ru3—Ru1—As1—C7−67.39 (19)C27—C28—C29—Br1178.0 (5)
C45—Ru1—As1—C1−27.4 (3)C28—C29—C30—C313.1 (11)
C44—Ru1—As1—C1−118.0 (2)Br1—C29—C30—C31−175.5 (5)
C46—Ru1—As1—C165.1 (3)C29—C30—C31—C26−2.5 (11)
Ru2—Ru1—As1—C1148.64 (19)C27—C26—C31—C30−0.5 (9)
Ru3—Ru1—As1—C1170.97 (19)P1—C26—C31—C30−179.3 (5)
C45—Ru1—As1—C13−142.2 (3)C38—P1—C32—C3364.5 (5)
C44—Ru1—As1—C13127.2 (2)C26—P1—C32—C33170.1 (5)
C46—Ru1—As1—C13−49.7 (2)Ru3—P1—C32—C33−61.4 (5)
Ru2—Ru1—As1—C1333.83 (16)C38—P1—C32—C37−119.7 (5)
Ru3—Ru1—As1—C1356.16 (17)C26—P1—C32—C37−14.1 (6)
C48—Ru2—As2—C20−50.9 (3)Ru3—P1—C32—C37114.4 (5)
C49—Ru2—As2—C2041.4 (2)C37—C32—C33—C340.6 (10)
C47—Ru2—As2—C20−143.0 (2)P1—C32—C33—C34176.6 (5)
Ru3—Ru2—As2—C20136.14 (17)C32—C33—C34—C35−0.3 (11)
Ru1—Ru2—As2—C20124.12 (16)C33—C34—C35—C36−0.1 (12)
C48—Ru2—As2—C1470.0 (3)C34—C35—C36—C370.3 (13)
C49—Ru2—As2—C14162.3 (2)C33—C32—C37—C36−0.4 (10)
C47—Ru2—As2—C14−22.1 (2)P1—C32—C37—C36−176.2 (5)
Ru3—Ru2—As2—C14−102.88 (17)C35—C36—C37—C32−0.1 (12)
Ru1—Ru2—As2—C14−114.89 (17)C32—P1—C38—C39−149.9 (5)
C48—Ru2—As2—C13−171.6 (3)C26—P1—C38—C39102.2 (5)
C49—Ru2—As2—C13−79.3 (2)Ru3—P1—C38—C39−26.8 (5)
C47—Ru2—As2—C1396.3 (2)C32—P1—C38—C4333.6 (5)
Ru3—Ru2—As2—C1315.51 (18)C26—P1—C38—C43−74.4 (5)
Ru1—Ru2—As2—C133.49 (17)Ru3—P1—C38—C43156.6 (4)
C51—Ru3—P1—C38−38.5 (3)C43—C38—C39—C402.2 (9)
C52—Ru3—P1—C3862.9 (3)P1—C38—C39—C40−174.5 (5)
C50—Ru3—P1—C38−130.8 (3)C38—C39—C40—C410.0 (10)
Ru1—Ru3—P1—C38128.6 (2)C39—C40—C41—C42−3.2 (11)
C51—Ru3—P1—C3278.3 (3)C40—C41—C42—C434.2 (11)
C52—Ru3—P1—C32179.6 (3)C41—C42—C43—C38−2.0 (11)
C50—Ru3—P1—C32−14.1 (3)C39—C38—C43—C42−1.1 (9)
Ru1—Ru3—P1—C32−114.7 (2)P1—C38—C43—C42175.5 (5)
C51—Ru3—P1—C26−159.8 (3)C51—Ru3—C52—O960 (3)
C52—Ru3—P1—C26−58.5 (3)C50—Ru3—C52—O9−127 (3)
C50—Ru3—P1—C26107.8 (3)P1—Ru3—C52—O9−35 (3)
Ru1—Ru3—P1—C267.2 (2)Ru2—Ru3—C52—O9147 (3)
C7—As1—C1—C6−157.4 (6)Ru1—Ru3—C52—O9−157 (3)
D—H···AD—HH···AD···AD—H···A
C23—H23A···O2i0.932.593.180 (8)122
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
C23—H23A⋯O2i0.932.593.180 (8)122

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-arsino)methane-1:2κAs:As']nona-carbonyl-1κC,2κC,3κC-[tris-(4-fluoro-phen-yl)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

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