metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890
Volume 65| Part 11| November 2009| Pages m1371-m1372

cis,fac-Di­chlorido{N-[3,5-di-tert-butyl-2-(tri­methyl­silyl­­oxy)benz­yl]-N,N-bis­­(2-pyridylmeth­yl)amine}(di­methyl sulfoxide)ruthenium(II) di­chloro­methane disolvate

aChemistry Department, Macalester College, 1600 Grand Avenue, Saint Paul, MN 55105, USA, and bChemistry Department, University of California, Berkeley, CA 94720-1460, USA
*Correspondence e-mail: fischer@macalester.edu

(Received 7 October 2009; accepted 9 October 2009; online 17 October 2009)

Reaction of dichloridotetra­kis(dimethyl sulfoxide)ruthenium(II) and N-[3,5-di-tert-butyl-2-(trimethyl­silyl­oxy)benz­yl]-N,N-bis­(2-pyridylmeth­yl)amine (BPPA-TMS) affords the thermodynamic product cis,fac-[RuCl2(BPPA-TMS)(DMSO)] and kinetic product trans,mer-[RuCl2(BPPA-TMS)(DMSO)]. The title complex, [RuCl2(C30H43N3OSi)(C2H6OS)]·2CH2Cl2, crystallizes as a dichloro­methane disolvate, with two formula units in the asymmetric unit. The complex exhibits a distorted-octa­hedral geometry about the low spin d6 RuII center. The BPPA-TMS ligand is coordinated in a facial fashion, with the DMSO ligand cis to the aliphatic nitro­gen atom of the BPPA-TMS ligand. One of the two dichloromethane solvate molecules is disordered over two positions in a 0.695:0.305 ratio.

Related literature

The application of tetra­dentate monoanionic (TDMA) ligands for stabilizing reactive metal complexes motivates ligand design efforts (Chomitz & Arnold, 2009[Chomitz, W. A. & Arnold, J. (2009). Chem. Eur. J. 15, 2020-2030.]). The TDMA precursor N,N-bis-(2-pyridylmeth­yl)(2-hydr­oxy-3,5-di-tert-butyl­benz­yl)amine (HBPPA) has been employed to prepare main group, transition metal and actinide BPPA complexes (Chomitz et al., 2007[Chomitz, W. A., Minasian, S. G., Sutton, A. D. & Arnold, J. (2007). Inorg. Chem. 46, 7199-7209.]; Marinescu et al., 2007[Marinescu, S. C., Agapie, T., Day, M. W. & Bercaw, J. E. (2007). Organometallics, 26, 1178-1190.]) but Ru(BPPA) complexes have not been reported. Coordination complexes of ruthenium that contain chlorido, DMSO, and pyridylic ligands demonstrate promising applications as chemotherapeutic agents (Velders et al., 2004[Velders, A. H., Bergamo, A., Alessio, E., Zangrando, E., Haasnoot, J. G., Casarsa, C., Cocchietto, M., Zorzet, S. & Sava, G. (2004). J. Med. Chem. 47, 1110-1121.]; Bratsos et al., 2007[Bratsos, I., Serli, B., Zangrando, E., Katsaros, N. & Alessio, E. (2007). Inorg. Chem., 46, 975-992.]). Substitution mechanisms for related complexes have been studied, see: Mola et al. (2007[Mola, J., Romero, I., Rodriguez, M., Bozoglian, F., Poater, A., Sola, M., Parella, T., Benet-Buchholz, J., Fontrodona, X. & Llobet, A. (2007). Inorg. Chem. 46, 10707-10716.]).

[Scheme 1]

Experimental

Crystal data
  • [RuCl2(C30H43N3OSi)(C2H6OS)]·2CH2Cl2

  • Mr = 909.71

  • Triclinic, [P \overline 1]

  • a = 10.913 (2) Å

  • b = 18.435 (4) Å

  • c = 22.413 (5) Å

  • α = 82.039 (3)°

  • β = 76.212 (3)°

  • γ = 89.148 (3)°

  • V = 4336.4 (15) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 0.84 mm−1

  • T = 126 K

  • 0.33 × 0.31 × 0.02 mm

Data collection
  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.769, Tmax = 0.988

  • 52307 measured reflections

  • 15775 independent reflections

  • 8958 reflections with I > 2σ(I)

  • Rint = 0.085

Refinement
  • R[F2 > 2σ(F2)] = 0.049

  • wR(F2) = 0.124

  • S = 0.98

  • 15775 reflections

  • 861 parameters

  • 24 restraints

  • H-atom parameters constrained

  • Δρmax = 0.70 e Å−3

  • Δρmin = −0.57 e Å−3

Data collection: SMART (Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]).

Supporting information


Comment top

Desilylation of 1 to eliminate the trimethylsilyl substituent with concomitant Ru—O bond formation (and a tetradentate BPPA ligand) has been unsuccessful to date. The utility of BPPA-TMS as a BPPA transfer agent remains an open question.

The distorted octahedral structures at the low spin d6 Ru(II) centers of 1 and cis,fac-[RuCl2(BPEA)(DMSO)] (3, BPEA = N,N-bis(2-pyridylmethyl)ethylamine)) (Mola et al., 2007) are very similar. The sulfur-bound DMSO ligand is cis to the aliphatic nitrogen in both 1 and 3, and the facial binding of the pyridyl and tertiary amine N atoms is seemingly independent tertiary nitrogen steric bulk (i.e., ethyl (3) versus 2-trimethylsiloxo-3,5-tert- butylbenzyl (1)). The average Ru-pyridyl nitrogen lengths (1, 2.077 (3) Å; 3, 2.07 (4) Å) and the average Ru—Cl distances (1, 2.430 (6) Å; 3, 2.435 (9) Å) are statistically indistinguishable. The angles that define the edges of the distorted octahedra range from 79.61 (5) to 99.79 (4)° in 3 to 77.42 (14) to 99.43 (11) in 1. In both structures, the tertiary amine nitrogen-Ru—S angle (defined by N(3 A)—Ru(1 A)—S(1 A) in 1) is most obtuse while angles that define edges occupied by the facially bound ligands are most acute.

The 1H NMR spectra of 1 has similar features to that of 3, and is fully consistent with the solid-state structure. It is noteworthy that the six N—CH2-py and N—CH2—Ph ligand backbone H atoms are diastereotopic; each exhibits a doublet due to geminal coupling.

Related literature top

The application of tetradentate monoanionic (TDMA) ligands for stabilizing reactive metal complexes motivates ligand design efforts (Chomitz et al., 2009). The TDMA precursor N,N- bis-(2-pyridylmethyl)(2-hydroxy-3,5-di-tert-butylbenzyl)amine (HBPPA) has been employed to prepare main group, transition metal and actinide BPPA complexes (Chomitz et al., 2007; Marinescu et al., 2007) but Ru(BPPA) complexes have not been reported. Coordination complexes of ruthenium that contain chloro, DMSO, and pyridylic ligands demonstrate promising applications as chemotherapeutic agents (Velders et al., 2004; Bratsos et al., 2007). Substitution mechanisms for related complexes have been studied, see: Mola et al. (2007).

Experimental top

The following procedures were conducted under nitrogen using standard techniques for handling air and moisture sensitive substances. Ethanol (40 ml) was added to BPPA-TMS (1.50 g, 3.06 mmol) and RuCl2(DMSO)4 (1.48 g, 3.06 mmol). The mixture was heated to reflux (15 hr); the solids dissolved affording a red-orange solution. Solvent removal in vacuo provided a red oily residue that was washed with pentane (10 ml). Treatment with Et2O (45 ml) resulted in a yellow solid containing 1 and 2. The suspension was vigorously stirred (20 min) to generate a fine powder. The Et2O was decanted, and the solid was dried in vacuo. Kinetic product 2 was extracted with toluene (30 ml); the remaining solid was washed with toluene (10 ml) to remove traces of 2. The residue was dried in vacuo, and 1 was extracted with CH2Cl2 (30 ml). The CH2Cl2 extract was filtered, and the solvent removed in vacuo revealing yellow-orange 1. Pentane diffusion into a dichloromethane solution of 1 yielded crystals of 1 with 2 CH2Cl2 molecules per formula unit (1.13 g, 40%). Mp: 162–163 °C (dec).

Refinement top

All hydrogen atoms were placed in ideal positions with C-H ranging from 0.95Å to 0.99Å and U(H) set to 1.2Ueq(C) or 1.5Ueq(Cmethyl) and refined as riding atoms. Two dichloromethane molecules were multipositioned. These could not be modeled as anisotropic, partial molecules and their contribution to the scattering power was suppressed using the SQUEEZE option in PLATON (Spek, 2003). One of the two remaining dichloromethane solvents refined well while the other was split into two fragments refining to a 0.693 (16):0.307 (16) ratio. The final refinement employed 24 bond distance (SAME) and anisotropic (DELU) restraints.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Figures top
[Figure 1] Fig. 1. Molecular structure of one of the two molecules in the asymmetric unit of 1 (50% displacement ellipsoids). The solvent molecules are not shown.
cis,fac-Dichlorido{N-[3,5-di-tert-butyl-2- (trimethylsilyloxy)benzyl]-N,N-bis(2- pyridylmethyl)amine}(dimethyl sulfoxide)ruthenium(II) dichloromethane disolvate top
Crystal data top
[RuCl2(C30H43N3OSi)(C2H6OS)]·2CH2Cl2Z = 4
Mr = 909.71F(000) = 1880
Triclinic, P1Dx = 1.393 Mg m3
Hall symbol: -P 1Melting point: 162 K
a = 10.913 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 18.435 (4) ÅCell parameters from 7479 reflections
c = 22.413 (5) Åθ = 2.5–23.0°
α = 82.039 (3)°µ = 0.84 mm1
β = 76.212 (3)°T = 126 K
γ = 89.148 (3)°Plate, yellow
V = 4336.4 (15) Å30.33 × 0.31 × 0.02 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
15775 independent reflections
Radiation source: sealed tube8958 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.085
ϕ and ω scansθmax = 25.4°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 1213
Tmin = 0.769, Tmax = 0.988k = 2122
52307 measured reflectionsl = 026
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.124H-atom parameters constrained
S = 0.98 w = 1/[σ2(Fo2) + (0.0583P)2]
where P = (Fo2 + 2Fc2)/3
15775 reflections(Δ/σ)max = 0.001
861 parametersΔρmax = 0.70 e Å3
24 restraintsΔρmin = 0.57 e Å3
Crystal data top
[RuCl2(C30H43N3OSi)(C2H6OS)]·2CH2Cl2γ = 89.148 (3)°
Mr = 909.71V = 4336.4 (15) Å3
Triclinic, P1Z = 4
a = 10.913 (2) ÅMo Kα radiation
b = 18.435 (4) ŵ = 0.84 mm1
c = 22.413 (5) ÅT = 126 K
α = 82.039 (3)°0.33 × 0.31 × 0.02 mm
β = 76.212 (3)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
15775 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
8958 reflections with I > 2σ(I)
Tmin = 0.769, Tmax = 0.988Rint = 0.085
52307 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04924 restraints
wR(F2) = 0.124H-atom parameters constrained
S = 0.98Δρmax = 0.70 e Å3
15775 reflectionsΔρmin = 0.57 e Å3
861 parameters
Special details top

Experimental. Anal Calcd. For C34H53Cl6N3O2SSiRu C, 44.89; H, 5.87; N, 4.62. Found C, 45.13; H, 5.86; N, 4.96.

NMR (CD3CN, 400 MHz) 1H δ 9.73 (d, J = 5.2 Hz 1H, α-pyridyl), 9.27 (d, J = 5.2, 1H, α-pyridyl), 7.57 (app t, J = 7.6 Hz, 1H, para-pyridyl), 7.44 (app t, J = 7.6 Hz, 1H, para-pyridyl), 7.37 (d, J = 2.4, 1H, aromatic phenol), 7.24 (app t, J = 6.0 Hz, 1H, B-pyridyl), 7.18 (d, J = 2.4 Hz, 1H, aromatic phenol), 7.01 (app t, J = 6.4 Hz, 1H, B-pyridyl), 6.94 (m, 2H, pyridyl), 5.27 (s, 4H, CH2Cl2), 5.05 (d, J = 14 Hz, 1H, NCH2py), 4.95 (d, J = 15 Hz, 1H, NCH2py), 4.69 (d, J = 14 Hz, 1H, NCH2py), 4.56 (d, J = 16 Hz, 1H, NCH2py), 3.62 (s, 3H, DMSO), 3.28 (d, J = 15 Hz, 1H, NCH2Ph), 3.11 (d, J = 17 Hz, NCH2Ph), 2.87 (s, 3H, DMSO), 1.41 (sm, 9H, tert-Bu), 1.29 (s, 9H, tert-Bu), 0.156 (s, 9H, SiMe3).

NMR (CD3CN, 400 MHz) 13C{1H} δ 164.3, 160.9, 154.5, 153.2, 151.6, 143.0, 140.6, 136.5, 135.0, 129.3, 125.5, 123.7, 123.6, 123.5, 120.6, 119.6, 68.7, 65.1, 63.8, 53.6, 44.8, 44.0, 35.4, 34.2, 31.6, 31.4, 2.1. The expected sixteen aromatic carbon environments are present, along with eleven other environments (including one for for dichloromethane solvate), consistent with the solid-state structure of 1.

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. A crystal (approximate dimensions 1/4x 0.12 x 0.04 mm3) was placed onto the tip of a 0.1 mm diameter glass capillary and mounted on a CCD area detector diffractometer for a data collection at 173 (2) K (SMART V5.054, Bruker Analytical X-ray Systems, Madison, WI (2001).). A preliminary set of cell constants was calculated from reflections harvested from three sets of 20 frames. These initial sets of frames were oriented such that orthogonal wedges of reciprocal space were surveyed. This produced initial orientation matrices determined from 48 reflections. The data collection was carried out using Mo Kα radiation (graphite monochromator) with a frame time of 8 s and a detector distance of 4.8 cm. A randomly oriented region of reciprocal space was surveyed to the extent of one sphere and to a resolution of 0.77 Å. Four major sections of frames were collected with 0.30° steps in ω at four different ϕ settings and a detector position of -28° in 2θ. The intensity data were corrected for absorption and decay (SADABS).

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.

The structure is P-1 with two complexes and four dichloromethane molecules per asymmetric unit. The two indpendent ruthenium complexes are enantiomeric. The structure is best described as having Z=4 and Z'=2. The two ruthenium complexes are related by a pseudo-b-glide perpendicular to the a axis. The fit is quite good for the atoms bound to the Ru atom, but the atoms on the benzyl portion are not as good. However, this is just pseudosymmetry.

The four dichlormethane molecules are related similarly. Two dichloromethane molecules were multipositioned. These could not be modeled as anisotropic, partial molecules. These two were commented out of the res file and PLATON/Squeeze was run to remove diffuse scattering effects from the diffraction data.

PLATON / Squeeze results (Spek, 2009):

Total Potential Solvent Area Vol: 608.2 Å

per Unit Cell Vol: 4336.4 Å [14.0%]

Total Potential Solvent Accessible Void Vol: 608.2 Å

Electron Count / Cell = 67 - To be included in D(calc), F000 & Mol.Wght.

Correction - Since two DCM with electron count = 84 were removed, then 84 electron will be added into F000. The empirical formula is correct.

One of the two remaining dichloromethane solvents refined well while the other was split into two fragments refining to a 0.695:0.305 ratio. The final refinement employed 24 bond distance (SAME) and anisotropic (DELU) restraints.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ru1A0.29376 (4)0.13565 (2)0.115631 (17)0.01704 (11)
Cl1A0.30575 (12)0.24252 (6)0.16712 (5)0.0241 (3)
Cl2A0.34173 (12)0.21477 (7)0.01658 (5)0.0265 (3)
S1A0.08900 (11)0.15552 (7)0.12116 (6)0.0208 (3)
Si1A0.49345 (14)0.11139 (8)0.33698 (7)0.0304 (4)
O1A0.4449 (3)0.03571 (17)0.31556 (14)0.0276 (9)
O2A0.0055 (3)0.12446 (18)0.17877 (14)0.0271 (9)
N1A0.2767 (4)0.04179 (19)0.07772 (17)0.0190 (9)
N2A0.4846 (3)0.1227 (2)0.11801 (16)0.0182 (9)
N3A0.2778 (4)0.0513 (2)0.19379 (17)0.0179 (9)
C1A0.3088 (5)0.0334 (3)0.0179 (2)0.0254 (12)
H1AA0.35520.07160.01120.031*
C2A0.2771 (5)0.0283 (3)0.0033 (2)0.0342 (14)
H2AB0.30190.03210.04630.041*
C3A0.2101 (5)0.0843 (3)0.0369 (3)0.0353 (14)
H3AA0.18530.12630.02220.042*
C4A0.1794 (5)0.0784 (3)0.0994 (2)0.0302 (13)
H4AA0.13570.11740.12860.036*
C5A0.2133 (4)0.0146 (3)0.1192 (2)0.0227 (12)
C6A0.1828 (5)0.0024 (3)0.1866 (2)0.0236 (12)
H6AA0.09670.01690.19860.028*
H6AB0.18690.04930.21360.028*
C7A0.4031 (4)0.0129 (2)0.1856 (2)0.0188 (11)
H7AA0.41220.01260.22620.023*
H7AB0.40650.02410.15730.023*
C8A0.5079 (5)0.0677 (2)0.1596 (2)0.0198 (11)
C9A0.6227 (5)0.0616 (3)0.1757 (2)0.0240 (12)
H9AA0.63720.02190.20490.029*
C10A0.7160 (5)0.1139 (3)0.1486 (2)0.0292 (13)
H10A0.79570.11060.15890.035*
C11A0.6914 (4)0.1714 (3)0.1061 (2)0.0252 (13)
H11B0.75380.20830.08720.030*
C12A0.5754 (4)0.1742 (3)0.0919 (2)0.0238 (12)
H12B0.55870.21340.06290.029*
C13A0.2423 (4)0.0793 (2)0.2559 (2)0.0198 (11)
H13A0.16170.10560.25890.024*
H13B0.30770.11530.25720.024*
C14A0.2280 (5)0.0210 (3)0.3121 (2)0.0235 (12)
C15A0.3303 (4)0.0031 (3)0.3377 (2)0.0198 (11)
C16A0.3174 (5)0.0649 (3)0.3827 (2)0.0223 (12)
C17A0.1948 (5)0.0944 (3)0.4064 (2)0.0277 (13)
H17A0.18370.13580.43770.033*
C18A0.0890 (5)0.0676 (3)0.3876 (2)0.0265 (13)
C19A0.1088 (5)0.0115 (3)0.3380 (2)0.0233 (12)
H19A0.03970.00530.32130.028*
C20A0.0437 (5)0.0989 (3)0.4162 (3)0.0395 (15)
C21A0.1305 (6)0.0365 (4)0.4392 (3)0.073 (2)
H21A0.21740.05530.45470.109*
H21B0.12680.00310.40480.109*
H21C0.10220.01770.47260.109*
C22A0.0947 (6)0.1316 (4)0.3685 (3)0.079 (3)
H22A0.03550.16760.35040.119*
H22B0.10530.09270.33570.119*
H22C0.17650.15570.38850.119*
C23A0.0488 (5)0.1573 (3)0.4723 (3)0.0505 (18)
H23A0.00140.20010.45880.076*
H23B0.13680.17190.49170.076*
H23C0.01140.13740.50240.076*
C24A0.4293 (5)0.1028 (3)0.4046 (2)0.0287 (13)
C25A0.3952 (6)0.1816 (3)0.4386 (3)0.0517 (18)
H25A0.36090.21000.41230.078*
H25B0.33210.17950.47760.078*
H25C0.47120.20510.44760.078*
C26A0.5413 (5)0.1092 (3)0.3498 (3)0.0465 (16)
H26A0.57480.06020.33090.070*
H26B0.51380.13370.31900.070*
H26C0.60740.13790.36450.070*
C27A0.4694 (5)0.0597 (3)0.4507 (2)0.0417 (15)
H27A0.49610.01000.43040.063*
H27B0.53970.08430.46480.063*
H27C0.39810.05710.48640.063*
C28A0.3788 (6)0.1316 (3)0.4077 (2)0.0467 (17)
H28A0.29990.14810.39720.070*
H28B0.41360.17010.42530.070*
H28C0.36220.08720.43830.070*
C29A0.6577 (5)0.0943 (3)0.3460 (3)0.0551 (19)
H29A0.71000.08030.30750.083*
H29B0.65630.05470.38020.083*
H29C0.69290.13900.35500.083*
C30A0.5066 (5)0.1913 (3)0.2768 (2)0.0393 (15)
H30A0.42210.20670.27320.059*
H30B0.55460.17830.23700.059*
H30C0.55030.23150.28800.059*
C31A0.0407 (5)0.1256 (3)0.0575 (2)0.0300 (13)
H31A0.04390.14350.05680.045*
H31B0.03960.07190.06230.045*
H31C0.10020.14490.01850.045*
C32A0.0529 (5)0.2500 (2)0.1080 (2)0.0284 (13)
H32A0.03750.25500.10990.043*
H32B0.10150.27170.06690.043*
H32C0.07470.27540.13980.043*
Ru1B0.09676 (4)0.63569 (2)0.115900 (18)0.01900 (12)
Cl1B0.04663 (12)0.74054 (6)0.17174 (6)0.0278 (3)
Cl2B0.11675 (13)0.71495 (7)0.01828 (6)0.0323 (3)
S1B0.30095 (12)0.65563 (7)0.10974 (6)0.0247 (3)
Si1B0.21556 (15)0.61342 (9)0.37330 (7)0.0355 (4)
O1B0.1606 (3)0.53386 (18)0.34994 (15)0.0296 (9)
O2B0.3538 (3)0.62659 (19)0.16344 (16)0.0341 (9)
N1B0.1388 (4)0.5427 (2)0.07480 (18)0.0227 (10)
N2B0.0989 (4)0.6230 (2)0.13090 (18)0.0219 (10)
N3B0.0615 (3)0.5517 (2)0.19497 (17)0.0185 (9)
C1B0.1459 (5)0.5359 (3)0.0146 (2)0.0268 (13)
H1BA0.11970.57550.01120.032*
C2B0.1902 (5)0.4731 (3)0.0107 (2)0.0334 (14)
H2BB0.19560.47010.05320.040*
C3B0.2263 (5)0.4147 (3)0.0269 (2)0.0348 (14)
H3BA0.25820.37160.01040.042*
C4B0.2153 (5)0.4203 (3)0.0897 (2)0.0277 (13)
H4BA0.23760.38050.11660.033*
C5B0.1715 (4)0.4846 (3)0.1120 (2)0.0220 (12)
C6B0.1608 (4)0.4966 (2)0.1781 (2)0.0205 (11)
H6BA0.13820.44990.20610.025*
H6BB0.24270.51450.18270.025*
C7B0.0641 (4)0.5167 (2)0.1998 (2)0.0212 (12)
H7BA0.05190.47520.17550.025*
H7BB0.10130.49680.24370.025*
C8B0.1535 (5)0.5687 (3)0.1771 (2)0.0209 (12)
C9B0.2821 (5)0.5614 (3)0.1982 (2)0.0313 (13)
H9BA0.31810.52340.23060.038*
C10B0.3592 (5)0.6103 (3)0.1717 (3)0.0367 (15)
H10B0.44850.60550.18520.044*
C11B0.3037 (5)0.6664 (3)0.1252 (3)0.0359 (14)
H11A0.35410.70110.10690.043*
C12B0.1740 (5)0.6704 (3)0.1064 (2)0.0275 (13)
H12A0.13600.70850.07450.033*
C13B0.0659 (5)0.5802 (3)0.25443 (19)0.0225 (12)
H13C0.14430.60990.24700.027*
H13D0.00620.61310.26500.027*
C14B0.0617 (5)0.5227 (3)0.3090 (2)0.0230 (12)
C15B0.0486 (5)0.4984 (3)0.3533 (2)0.0250 (12)
C16B0.0451 (5)0.4371 (3)0.3990 (2)0.0276 (13)
C17B0.0722 (5)0.4081 (3)0.4004 (2)0.0311 (14)
H17B0.07570.36760.43110.037*
C18B0.1847 (5)0.4341 (3)0.3601 (2)0.0294 (13)
C19B0.1757 (5)0.4917 (3)0.3149 (2)0.0287 (13)
H19B0.25100.51100.28660.034*
C20B0.3134 (5)0.3992 (3)0.3607 (3)0.0381 (15)
C21B0.3074 (7)0.3400 (4)0.4148 (3)0.089 (3)
H21D0.39190.32040.41330.134*
H21E0.25010.30050.41260.134*
H21F0.27640.36040.45360.134*
C22B0.3627 (8)0.3685 (5)0.3007 (3)0.102 (3)
H22D0.44850.35080.29880.153*
H22E0.36400.40700.26560.153*
H22F0.30780.32780.29860.153*
C23B0.4075 (6)0.4569 (4)0.3655 (3)0.074 (2)
H23D0.49140.43550.36090.111*
H23E0.38150.47400.40610.111*
H23F0.41010.49830.33260.111*
C24B0.1653 (5)0.4035 (3)0.4473 (2)0.0344 (14)
C25B0.1391 (6)0.3274 (3)0.4791 (3)0.0499 (18)
H25D0.21660.30710.50820.075*
H25E0.07360.33180.50170.075*
H25F0.11050.29490.44770.075*
C26B0.2744 (6)0.3947 (3)0.4168 (3)0.0524 (18)
H26D0.34900.37490.44850.079*
H26E0.25040.36090.38600.079*
H26F0.29390.44250.39640.079*
C27B0.2033 (6)0.4525 (3)0.4985 (2)0.0491 (18)
H27D0.27910.43190.52890.074*
H27E0.22080.50180.48020.074*
H27F0.13430.45520.51930.074*
C28B0.1051 (6)0.6473 (3)0.4147 (3)0.0505 (17)
H28D0.02150.65570.38640.076*
H28E0.09940.61090.45010.076*
H28F0.13590.69340.42950.076*
C29B0.3792 (6)0.5965 (3)0.4213 (3)0.0556 (18)
H29D0.37710.56700.46100.083*
H29E0.42790.57010.39930.083*
H29F0.41900.64340.42900.083*
C30B0.2306 (6)0.6826 (3)0.3077 (3)0.0477 (16)
H30D0.14710.69410.27990.072*
H30E0.26670.72720.32340.072*
H30F0.28600.66330.28480.072*
C31B0.4028 (5)0.6244 (3)0.0436 (2)0.0397 (15)
H31D0.48930.64170.03950.059*
H31E0.37450.64360.00620.059*
H31F0.40050.57070.04890.059*
C32B0.3455 (5)0.7505 (3)0.0915 (2)0.0321 (14)
H32D0.43630.75590.08790.048*
H32E0.29880.77710.12450.048*
H32F0.32590.77050.05200.048*
Cl1C0.47593 (17)0.55631 (10)0.87226 (9)0.0723 (6)
C1C0.4109 (5)0.6421 (2)0.8598 (3)0.068 (2)
H1C10.38670.66200.89970.082*
H1C20.47590.67550.83120.082*
Cl2C0.27935 (18)0.64103 (10)0.82890 (11)0.0853 (7)
Cl1D0.0460 (8)0.3220 (2)0.2756 (2)0.075 (2)0.693 (16)
C1D0.0112 (11)0.2334 (4)0.2809 (3)0.050 (3)0.693 (16)
H1D10.03740.20300.26110.060*0.693 (16)
H1D20.10020.23470.25710.060*0.693 (16)
Cl2D0.0030 (13)0.1918 (5)0.3562 (4)0.093 (2)0.693 (16)
Cl1E0.0996 (13)0.2932 (12)0.2747 (6)0.096 (4)0.307 (16)
C1E0.0426 (14)0.2746 (15)0.2952 (10)0.075 (8)0.307 (16)
H1E10.10670.26470.25800.090*0.307 (16)
H1E20.07110.31870.30920.090*0.307 (16)
Cl2E0.035 (4)0.2007 (13)0.3534 (9)0.109 (9)0.307 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru1A0.0150 (2)0.0158 (2)0.0193 (2)0.00084 (17)0.00409 (18)0.00129 (17)
Cl1A0.0263 (7)0.0180 (7)0.0291 (7)0.0011 (5)0.0106 (6)0.0010 (5)
Cl2A0.0276 (8)0.0246 (7)0.0232 (7)0.0017 (6)0.0035 (6)0.0065 (5)
S1A0.0161 (7)0.0228 (7)0.0237 (7)0.0007 (5)0.0067 (6)0.0000 (6)
Si1A0.0315 (9)0.0294 (9)0.0326 (9)0.0023 (7)0.0132 (7)0.0018 (7)
O1A0.022 (2)0.030 (2)0.030 (2)0.0017 (16)0.0065 (16)0.0006 (16)
O2A0.0152 (19)0.035 (2)0.0273 (19)0.0032 (16)0.0022 (16)0.0034 (16)
N1A0.020 (2)0.013 (2)0.025 (2)0.0036 (17)0.0107 (19)0.0009 (18)
N2A0.018 (2)0.019 (2)0.017 (2)0.0043 (18)0.0025 (18)0.0018 (18)
N3A0.018 (2)0.014 (2)0.021 (2)0.0021 (17)0.0058 (18)0.0002 (17)
C1A0.027 (3)0.028 (3)0.019 (3)0.006 (2)0.005 (2)0.002 (2)
C2A0.047 (4)0.033 (4)0.025 (3)0.009 (3)0.010 (3)0.012 (3)
C3A0.043 (4)0.022 (3)0.046 (4)0.003 (3)0.020 (3)0.010 (3)
C4A0.030 (3)0.016 (3)0.045 (4)0.004 (2)0.014 (3)0.004 (2)
C5A0.017 (3)0.020 (3)0.032 (3)0.000 (2)0.012 (2)0.003 (2)
C6A0.023 (3)0.017 (3)0.026 (3)0.000 (2)0.001 (2)0.001 (2)
C7A0.017 (3)0.014 (3)0.027 (3)0.005 (2)0.010 (2)0.000 (2)
C8A0.023 (3)0.014 (3)0.021 (3)0.003 (2)0.002 (2)0.004 (2)
C9A0.021 (3)0.027 (3)0.023 (3)0.008 (2)0.007 (2)0.001 (2)
C10A0.012 (3)0.045 (4)0.031 (3)0.000 (2)0.004 (2)0.004 (3)
C11A0.015 (3)0.028 (3)0.029 (3)0.003 (2)0.001 (2)0.002 (2)
C12A0.021 (3)0.021 (3)0.026 (3)0.004 (2)0.000 (2)0.000 (2)
C13A0.017 (3)0.020 (3)0.022 (3)0.003 (2)0.002 (2)0.004 (2)
C14A0.027 (3)0.018 (3)0.024 (3)0.000 (2)0.006 (2)0.001 (2)
C15A0.016 (3)0.021 (3)0.022 (3)0.002 (2)0.004 (2)0.000 (2)
C16A0.026 (3)0.017 (3)0.024 (3)0.001 (2)0.011 (2)0.002 (2)
C17A0.032 (3)0.027 (3)0.022 (3)0.004 (3)0.006 (3)0.002 (2)
C18A0.025 (3)0.028 (3)0.025 (3)0.001 (2)0.006 (2)0.001 (2)
C19A0.023 (3)0.023 (3)0.021 (3)0.000 (2)0.003 (2)0.003 (2)
C20A0.022 (3)0.047 (4)0.041 (4)0.008 (3)0.006 (3)0.018 (3)
C21A0.029 (4)0.065 (5)0.097 (6)0.009 (3)0.016 (4)0.029 (4)
C22A0.058 (5)0.106 (6)0.072 (5)0.058 (5)0.024 (4)0.021 (5)
C23A0.032 (4)0.054 (4)0.052 (4)0.012 (3)0.002 (3)0.027 (3)
C24A0.024 (3)0.030 (3)0.035 (3)0.003 (2)0.016 (3)0.006 (2)
C25A0.048 (4)0.036 (4)0.076 (5)0.002 (3)0.034 (4)0.011 (3)
C26A0.034 (4)0.050 (4)0.060 (4)0.011 (3)0.020 (3)0.009 (3)
C27A0.045 (4)0.048 (4)0.039 (3)0.001 (3)0.025 (3)0.002 (3)
C28A0.061 (5)0.043 (4)0.035 (3)0.006 (3)0.009 (3)0.007 (3)
C29A0.041 (4)0.045 (4)0.085 (5)0.008 (3)0.032 (4)0.003 (4)
C30A0.049 (4)0.026 (3)0.040 (3)0.009 (3)0.006 (3)0.003 (3)
C31A0.022 (3)0.039 (3)0.034 (3)0.005 (2)0.014 (3)0.009 (3)
C32A0.019 (3)0.025 (3)0.043 (3)0.006 (2)0.014 (3)0.000 (3)
Ru1B0.0183 (2)0.0168 (2)0.0210 (2)0.00028 (17)0.00551 (18)0.00220 (17)
Cl1B0.0285 (8)0.0185 (7)0.0332 (7)0.0010 (5)0.0036 (6)0.0000 (6)
Cl2B0.0388 (9)0.0288 (8)0.0268 (7)0.0020 (6)0.0106 (6)0.0105 (6)
S1B0.0189 (7)0.0261 (8)0.0276 (7)0.0002 (6)0.0048 (6)0.0004 (6)
Si1B0.0317 (10)0.0375 (10)0.0354 (9)0.0037 (7)0.0036 (8)0.0065 (8)
O1B0.031 (2)0.028 (2)0.029 (2)0.0044 (17)0.0087 (17)0.0026 (16)
O2B0.022 (2)0.038 (2)0.042 (2)0.0010 (17)0.0139 (18)0.0059 (18)
N1B0.018 (2)0.023 (2)0.027 (2)0.0021 (18)0.0056 (19)0.001 (2)
N2B0.019 (2)0.022 (3)0.026 (2)0.0008 (19)0.008 (2)0.005 (2)
N3B0.013 (2)0.020 (2)0.023 (2)0.0010 (17)0.0072 (18)0.0022 (18)
C1B0.021 (3)0.030 (3)0.025 (3)0.005 (2)0.004 (2)0.005 (2)
C2B0.041 (4)0.030 (3)0.031 (3)0.003 (3)0.008 (3)0.009 (3)
C3B0.031 (3)0.029 (3)0.042 (4)0.001 (3)0.001 (3)0.013 (3)
C4B0.024 (3)0.020 (3)0.036 (3)0.001 (2)0.005 (3)0.002 (2)
C5B0.018 (3)0.018 (3)0.027 (3)0.002 (2)0.003 (2)0.003 (2)
C6B0.023 (3)0.017 (3)0.021 (3)0.007 (2)0.008 (2)0.004 (2)
C7B0.018 (3)0.019 (3)0.024 (3)0.005 (2)0.005 (2)0.004 (2)
C8B0.021 (3)0.020 (3)0.025 (3)0.003 (2)0.010 (2)0.005 (2)
C9B0.026 (3)0.029 (3)0.040 (3)0.002 (3)0.012 (3)0.001 (3)
C10B0.016 (3)0.043 (4)0.054 (4)0.001 (3)0.013 (3)0.010 (3)
C11B0.032 (4)0.033 (3)0.048 (4)0.006 (3)0.019 (3)0.007 (3)
C12B0.028 (3)0.021 (3)0.034 (3)0.006 (2)0.014 (3)0.005 (2)
C13B0.029 (3)0.024 (3)0.015 (3)0.004 (2)0.007 (2)0.001 (2)
C14B0.026 (3)0.023 (3)0.020 (3)0.001 (2)0.007 (2)0.002 (2)
C15B0.021 (3)0.024 (3)0.031 (3)0.002 (2)0.008 (2)0.001 (2)
C16B0.037 (4)0.025 (3)0.021 (3)0.002 (3)0.008 (3)0.002 (2)
C17B0.042 (4)0.024 (3)0.026 (3)0.002 (3)0.008 (3)0.002 (2)
C18B0.033 (3)0.027 (3)0.028 (3)0.005 (3)0.005 (3)0.004 (3)
C19B0.031 (3)0.035 (3)0.021 (3)0.006 (3)0.007 (2)0.002 (2)
C20B0.034 (4)0.045 (4)0.038 (4)0.017 (3)0.015 (3)0.005 (3)
C21B0.067 (6)0.097 (7)0.088 (6)0.035 (5)0.018 (5)0.040 (5)
C22B0.102 (7)0.138 (8)0.089 (6)0.079 (6)0.041 (5)0.072 (6)
C23B0.044 (5)0.076 (6)0.108 (6)0.022 (4)0.028 (4)0.015 (5)
C24B0.033 (3)0.033 (3)0.030 (3)0.003 (3)0.002 (3)0.004 (3)
C25B0.054 (4)0.033 (4)0.054 (4)0.011 (3)0.007 (3)0.014 (3)
C26B0.046 (4)0.055 (4)0.049 (4)0.019 (3)0.005 (3)0.008 (3)
C27B0.059 (5)0.049 (4)0.030 (3)0.004 (3)0.008 (3)0.004 (3)
C28B0.055 (4)0.046 (4)0.056 (4)0.001 (3)0.017 (3)0.018 (3)
C29B0.044 (4)0.056 (5)0.059 (4)0.008 (3)0.005 (3)0.015 (3)
C30B0.048 (4)0.045 (4)0.049 (4)0.020 (3)0.010 (3)0.006 (3)
C31B0.024 (3)0.041 (4)0.050 (4)0.004 (3)0.005 (3)0.013 (3)
C32B0.025 (3)0.030 (3)0.037 (3)0.005 (2)0.003 (3)0.001 (3)
Cl1C0.0637 (13)0.0573 (12)0.0960 (14)0.0096 (9)0.0320 (11)0.0135 (10)
C1C0.089 (6)0.042 (4)0.079 (5)0.016 (4)0.037 (5)0.001 (4)
Cl2C0.0590 (13)0.0635 (13)0.1423 (19)0.0031 (10)0.0388 (13)0.0191 (13)
Cl1D0.100 (5)0.048 (2)0.075 (2)0.026 (2)0.015 (2)0.0104 (17)
C1D0.065 (8)0.042 (5)0.044 (4)0.013 (5)0.007 (5)0.017 (4)
Cl2D0.137 (5)0.073 (3)0.054 (3)0.031 (3)0.006 (3)0.004 (3)
Cl1E0.085 (8)0.107 (12)0.109 (7)0.030 (7)0.040 (6)0.031 (7)
C1E0.077 (14)0.11 (2)0.047 (15)0.013 (18)0.022 (13)0.028 (11)
Cl2E0.17 (2)0.115 (13)0.045 (8)0.076 (13)0.028 (9)0.038 (7)
Geometric parameters (Å, º) top
Ru1A—N1A2.060 (4)S1B—O2B1.487 (4)
Ru1A—N2A2.105 (4)S1B—C32B1.787 (5)
Ru1A—N3A2.151 (4)S1B—C31B1.788 (5)
Ru1A—S1A2.2359 (14)Si1B—O1B1.680 (4)
Ru1A—Cl2A2.4293 (13)Si1B—C30B1.846 (6)
Ru1A—Cl1A2.4371 (12)Si1B—C28B1.850 (6)
S1A—O2A1.496 (3)Si1B—C29B1.858 (6)
S1A—C32A1.780 (5)O1B—C15B1.391 (6)
S1A—C31A1.790 (5)N1B—C1B1.356 (6)
Si1A—O1A1.670 (3)N1B—C5B1.361 (6)
Si1A—C30A1.837 (5)N2B—C12B1.341 (6)
Si1A—C28A1.850 (5)N2B—C8B1.366 (6)
Si1A—C29A1.868 (6)N3B—C6B1.492 (6)
O1A—C15A1.397 (5)N3B—C7B1.498 (5)
N1A—C1A1.333 (6)N3B—C13B1.510 (5)
N1A—C5A1.368 (5)C1B—C2B1.391 (7)
N2A—C8A1.344 (6)C1B—H1BA0.9500
N2A—C12A1.349 (5)C2B—C3B1.385 (7)
N3A—C6A1.495 (5)C2B—H2BB0.9500
N3A—C13A1.514 (5)C3B—C4B1.402 (7)
N3A—C7A1.514 (6)C3B—H3BA0.9500
C1A—C2A1.370 (6)C4B—C5B1.384 (6)
C1A—H1AA0.9500C4B—H4BA0.9500
C2A—C3A1.365 (7)C5B—C6B1.506 (6)
C2A—H2AB0.9500C6B—H6BA0.9900
C3A—C4A1.378 (7)C6B—H6BB0.9900
C3A—H3AA0.9500C7B—C8B1.485 (7)
C4A—C5A1.399 (6)C7B—H7BA0.9900
C4A—H4AA0.9500C7B—H7BB0.9900
C5A—C6A1.515 (6)C8B—C9B1.372 (7)
C6A—H6AA0.9900C9B—C10B1.395 (7)
C6A—H6AB0.9900C9B—H9BA0.9500
C7A—C8A1.492 (6)C10B—C11B1.394 (7)
C7A—H7AA0.9900C10B—H10B0.9500
C7A—H7AB0.9900C11B—C12B1.377 (7)
C8A—C9A1.383 (7)C11B—H11A0.9500
C9A—C10A1.380 (6)C12B—H12A0.9500
C9A—H9AA0.9500C13B—C14B1.495 (6)
C10A—C11A1.393 (7)C13B—H13C0.9900
C10A—H10A0.9500C13B—H13D0.9900
C11A—C12A1.376 (6)C14B—C19B1.389 (7)
C11A—H11B0.9500C14B—C15B1.400 (6)
C12A—H12B0.9500C15B—C16B1.422 (7)
C13A—C14A1.519 (6)C16B—C17B1.385 (7)
C13A—H13A0.9900C16B—C24B1.561 (7)
C13A—H13B0.9900C17B—C18B1.386 (7)
C14A—C19A1.397 (6)C17B—H17B0.9500
C14A—C15A1.411 (7)C18B—C19B1.383 (7)
C15A—C16A1.399 (6)C18B—C20B1.538 (7)
C16A—C17A1.404 (6)C19B—H19B0.9500
C16A—C24A1.544 (7)C20B—C21B1.504 (8)
C17A—C18A1.383 (7)C20B—C22B1.508 (8)
C17A—H17A0.9500C20B—C23B1.521 (8)
C18A—C19A1.387 (6)C21B—H21D0.9800
C18A—C20A1.523 (7)C21B—H21E0.9800
C19A—H19A0.9500C21B—H21F0.9800
C20A—C22A1.513 (8)C22B—H22D0.9800
C20A—C23A1.529 (7)C22B—H22E0.9800
C20A—C21A1.545 (8)C22B—H22F0.9800
C21A—H21A0.9800C23B—H23D0.9800
C21A—H21B0.9800C23B—H23E0.9800
C21A—H21C0.9800C23B—H23F0.9800
C22A—H22A0.9800C24B—C26B1.529 (8)
C22A—H22B0.9800C24B—C27B1.535 (7)
C22A—H22C0.9800C24B—C25B1.537 (7)
C23A—H23A0.9800C25B—H25D0.9800
C23A—H23B0.9800C25B—H25E0.9800
C23A—H23C0.9800C25B—H25F0.9800
C24A—C26A1.528 (7)C26B—H26D0.9800
C24A—C27A1.532 (7)C26B—H26E0.9800
C24A—C25A1.551 (7)C26B—H26F0.9800
C25A—H25A0.9800C27B—H27D0.9800
C25A—H25B0.9800C27B—H27E0.9800
C25A—H25C0.9800C27B—H27F0.9800
C26A—H26A0.9800C28B—H28D0.9800
C26A—H26B0.9800C28B—H28E0.9800
C26A—H26C0.9800C28B—H28F0.9800
C27A—H27A0.9800C29B—H29D0.9800
C27A—H27B0.9800C29B—H29E0.9800
C27A—H27C0.9800C29B—H29F0.9800
C28A—H28A0.9800C30B—H30D0.9800
C28A—H28B0.9800C30B—H30E0.9800
C28A—H28C0.9800C30B—H30F0.9800
C29A—H29A0.9800C31B—H31D0.9800
C29A—H29B0.9800C31B—H31E0.9800
C29A—H29C0.9800C31B—H31F0.9800
C30A—H30A0.9800C32B—H32D0.9800
C30A—H30B0.9800C32B—H32E0.9800
C30A—H30C0.9800C32B—H32F0.9800
C31A—H31A0.9800Cl1C—C1C1.738 (3)
C31A—H31B0.9800C1C—Cl2C1.738 (3)
C31A—H31C0.9800C1C—H1C10.9900
C32A—H32A0.9800C1C—H1C20.9900
C32A—H32B0.9800Cl1D—C1D1.739 (3)
C32A—H32C0.9800C1D—Cl2D1.737 (4)
Ru1B—N1B2.052 (4)C1D—H1D10.9900
Ru1B—N2B2.092 (4)C1D—H1D20.9900
Ru1B—N3B2.149 (4)Cl1E—C1E1.738 (4)
Ru1B—S1B2.2324 (14)C1E—Cl2E1.738 (4)
Ru1B—Cl2B2.4220 (13)C1E—H1E10.9900
Ru1B—Cl1B2.4320 (13)C1E—H1E20.9900
N1A—Ru1A—N2A96.38 (15)S1B—Ru1B—Cl2B89.29 (5)
N1A—Ru1A—N3A77.42 (14)N1B—Ru1B—Cl1B175.87 (12)
N2A—Ru1A—N3A79.17 (14)N2B—Ru1B—Cl1B84.96 (11)
N1A—Ru1A—S1A88.67 (11)N3B—Ru1B—Cl1B97.72 (11)
N2A—Ru1A—S1A174.29 (10)S1B—Ru1B—Cl1B89.06 (5)
N3A—Ru1A—S1A99.43 (11)Cl2B—Ru1B—Cl1B90.20 (5)
N1A—Ru1A—Cl2A94.58 (11)O2B—S1B—C32B106.0 (2)
N2A—Ru1A—Cl2A93.85 (10)O2B—S1B—C31B105.7 (2)
N3A—Ru1A—Cl2A168.59 (11)C32B—S1B—C31B97.9 (2)
S1A—Ru1A—Cl2A88.38 (5)O2B—S1B—Ru1B118.80 (14)
N1A—Ru1A—Cl1A176.16 (11)C32B—S1B—Ru1B112.96 (18)
N2A—Ru1A—Cl1A84.67 (10)C31B—S1B—Ru1B113.15 (18)
N3A—Ru1A—Cl1A99.19 (10)O1B—Si1B—C30B112.1 (2)
S1A—Ru1A—Cl1A90.12 (4)O1B—Si1B—C28B107.8 (2)
Cl2A—Ru1A—Cl1A89.03 (4)C30B—Si1B—C28B110.0 (3)
O2A—S1A—C32A105.4 (2)O1B—Si1B—C29B107.9 (2)
O2A—S1A—C31A106.6 (2)C30B—Si1B—C29B104.9 (3)
C32A—S1A—C31A98.9 (2)C28B—Si1B—C29B114.1 (3)
O2A—S1A—Ru1A118.72 (15)C15B—O1B—Si1B130.3 (3)
C32A—S1A—Ru1A113.44 (16)C1B—N1B—C5B118.4 (4)
C31A—S1A—Ru1A111.64 (17)C1B—N1B—Ru1B126.7 (3)
O1A—Si1A—C30A112.6 (2)C5B—N1B—Ru1B114.7 (3)
O1A—Si1A—C28A108.5 (2)C12B—N2B—C8B118.5 (4)
C30A—Si1A—C28A108.7 (3)C12B—N2B—Ru1B125.0 (3)
O1A—Si1A—C29A106.6 (2)C8B—N2B—Ru1B115.6 (3)
C30A—Si1A—C29A105.4 (3)C6B—N3B—C7B108.0 (3)
C28A—Si1A—C29A115.1 (3)C6B—N3B—C13B112.2 (4)
C15A—O1A—Si1A129.6 (3)C7B—N3B—C13B111.2 (3)
C1A—N1A—C5A118.2 (4)C6B—N3B—Ru1B104.3 (3)
C1A—N1A—Ru1A127.2 (3)C7B—N3B—Ru1B107.8 (3)
C5A—N1A—Ru1A114.2 (3)C13B—N3B—Ru1B113.0 (3)
C8A—N2A—C12A118.9 (4)N1B—C1B—C2B122.2 (5)
C8A—N2A—Ru1A115.5 (3)N1B—C1B—H1BA118.9
C12A—N2A—Ru1A123.8 (3)C2B—C1B—H1BA118.9
C6A—N3A—C13A112.6 (3)C3B—C2B—C1B119.1 (5)
C6A—N3A—C7A107.0 (3)C3B—C2B—H2BB120.4
C13A—N3A—C7A110.8 (4)C1B—C2B—H2BB120.4
C6A—N3A—Ru1A105.0 (3)C2B—C3B—C4B119.1 (5)
C13A—N3A—Ru1A113.8 (3)C2B—C3B—H3BA120.5
C7A—N3A—Ru1A107.1 (3)C4B—C3B—H3BA120.5
N1A—C1A—C2A122.3 (5)C5B—C4B—C3B119.0 (5)
N1A—C1A—H1AA118.8C5B—C4B—H4BA120.5
C2A—C1A—H1AA118.8C3B—C4B—H4BA120.5
C3A—C2A—C1A120.6 (5)N1B—C5B—C4B122.2 (5)
C3A—C2A—H2AB119.7N1B—C5B—C6B115.0 (4)
C1A—C2A—H2AB119.7C4B—C5B—C6B122.8 (5)
C2A—C3A—C4A118.5 (5)N3B—C6B—C5B109.1 (4)
C2A—C3A—H3AA120.8N3B—C6B—H6BA109.9
C4A—C3A—H3AA120.8C5B—C6B—H6BA109.9
C3A—C4A—C5A119.2 (5)N3B—C6B—H6BB109.9
C3A—C4A—H4AA120.4C5B—C6B—H6BB109.9
C5A—C4A—H4AA120.4H6BA—C6B—H6BB108.3
N1A—C5A—C4A121.1 (4)C8B—C7B—N3B112.6 (4)
N1A—C5A—C6A115.5 (4)C8B—C7B—H7BA109.1
C4A—C5A—C6A123.4 (4)N3B—C7B—H7BA109.1
N3A—C6A—C5A107.8 (3)C8B—C7B—H7BB109.1
N3A—C6A—H6AA110.1N3B—C7B—H7BB109.1
C5A—C6A—H6AA110.1H7BA—C7B—H7BB107.8
N3A—C6A—H6AB110.1N2B—C8B—C9B121.7 (5)
C5A—C6A—H6AB110.1N2B—C8B—C7B115.1 (4)
H6AA—C6A—H6AB108.5C9B—C8B—C7B123.1 (4)
C8A—C7A—N3A109.6 (4)C8B—C9B—C10B119.2 (5)
C8A—C7A—H7AA109.8C8B—C9B—H9BA120.4
N3A—C7A—H7AA109.8C10B—C9B—H9BA120.4
C8A—C7A—H7AB109.8C11B—C10B—C9B119.1 (5)
N3A—C7A—H7AB109.8C11B—C10B—H10B120.4
H7AA—C7A—H7AB108.2C9B—C10B—H10B120.4
N2A—C8A—C9A122.1 (4)C12B—C11B—C10B118.4 (5)
N2A—C8A—C7A115.4 (4)C12B—C11B—H11A120.8
C9A—C8A—C7A122.5 (4)C10B—C11B—H11A120.8
C10A—C9A—C8A119.1 (5)N2B—C12B—C11B123.0 (5)
C10A—C9A—H9AA120.5N2B—C12B—H12A118.5
C8A—C9A—H9AA120.5C11B—C12B—H12A118.5
C9A—C10A—C11A118.9 (5)C14B—C13B—N3B115.2 (4)
C9A—C10A—H10A120.5C14B—C13B—H13C108.5
C11A—C10A—H10A120.5N3B—C13B—H13C108.5
C12A—C11A—C10A119.0 (4)C14B—C13B—H13D108.5
C12A—C11A—H11B120.5N3B—C13B—H13D108.5
C10A—C11A—H11B120.5H13C—C13B—H13D107.5
N2A—C12A—C11A122.0 (5)C19B—C14B—C15B118.8 (5)
N2A—C12A—H12B119.0C19B—C14B—C13B116.8 (4)
C11A—C12A—H12B119.0C15B—C14B—C13B124.4 (5)
N3A—C13A—C14A115.2 (4)O1B—C15B—C14B118.4 (4)
N3A—C13A—H13A108.5O1B—C15B—C16B121.6 (4)
C14A—C13A—H13A108.5C14B—C15B—C16B120.0 (5)
N3A—C13A—H13B108.5C17B—C16B—C15B116.9 (5)
C14A—C13A—H13B108.5C17B—C16B—C24B119.9 (5)
H13A—C13A—H13B107.5C15B—C16B—C24B123.1 (5)
C19A—C14A—C15A119.2 (4)C16B—C17B—C18B124.7 (5)
C19A—C14A—C13A118.1 (4)C16B—C17B—H17B117.7
C15A—C14A—C13A122.7 (4)C18B—C17B—H17B117.7
O1A—C15A—C16A121.4 (4)C19B—C18B—C17B116.1 (5)
O1A—C15A—C14A118.0 (4)C19B—C18B—C20B119.9 (5)
C16A—C15A—C14A120.6 (4)C17B—C18B—C20B123.8 (5)
C15A—C16A—C17A116.3 (5)C18B—C19B—C14B123.1 (5)
C15A—C16A—C24A123.8 (4)C18B—C19B—H19B118.4
C17A—C16A—C24A119.8 (4)C14B—C19B—H19B118.4
C18A—C17A—C16A124.7 (5)C21B—C20B—C22B109.9 (6)
C18A—C17A—H17A117.6C21B—C20B—C23B106.7 (5)
C16A—C17A—H17A117.6C22B—C20B—C23B108.2 (6)
C17A—C18A—C19A116.7 (5)C21B—C20B—C18B112.9 (5)
C17A—C18A—C20A123.5 (5)C22B—C20B—C18B109.0 (5)
C19A—C18A—C20A119.8 (5)C23B—C20B—C18B110.1 (5)
C18A—C19A—C14A121.6 (5)C20B—C21B—H21D109.5
C18A—C19A—H19A119.2C20B—C21B—H21E109.5
C14A—C19A—H19A119.2H21D—C21B—H21E109.5
C22A—C20A—C18A110.3 (5)C20B—C21B—H21F109.5
C22A—C20A—C23A109.0 (5)H21D—C21B—H21F109.5
C18A—C20A—C23A112.6 (5)H21E—C21B—H21F109.5
C22A—C20A—C21A108.9 (6)C20B—C22B—H22D109.5
C18A—C20A—C21A108.9 (5)C20B—C22B—H22E109.5
C23A—C20A—C21A107.0 (5)H22D—C22B—H22E109.5
C20A—C21A—H21A109.5C20B—C22B—H22F109.5
C20A—C21A—H21B109.5H22D—C22B—H22F109.5
H21A—C21A—H21B109.5H22E—C22B—H22F109.5
C20A—C21A—H21C109.5C20B—C23B—H23D109.5
H21A—C21A—H21C109.5C20B—C23B—H23E109.5
H21B—C21A—H21C109.5H23D—C23B—H23E109.5
C20A—C22A—H22A109.5C20B—C23B—H23F109.5
C20A—C22A—H22B109.5H23D—C23B—H23F109.5
H22A—C22A—H22B109.5H23E—C23B—H23F109.5
C20A—C22A—H22C109.5C26B—C24B—C27B110.5 (5)
H22A—C22A—H22C109.5C26B—C24B—C25B107.5 (4)
H22B—C22A—H22C109.5C27B—C24B—C25B106.8 (5)
C20A—C23A—H23A109.5C26B—C24B—C16B111.5 (4)
C20A—C23A—H23B109.5C27B—C24B—C16B109.1 (4)
H23A—C23A—H23B109.5C25B—C24B—C16B111.3 (5)
C20A—C23A—H23C109.5C24B—C25B—H25D109.5
H23A—C23A—H23C109.5C24B—C25B—H25E109.5
H23B—C23A—H23C109.5H25D—C25B—H25E109.5
C26A—C24A—C27A109.8 (4)C24B—C25B—H25F109.5
C26A—C24A—C16A111.3 (4)H25D—C25B—H25F109.5
C27A—C24A—C16A109.8 (4)H25E—C25B—H25F109.5
C26A—C24A—C25A106.6 (5)C24B—C26B—H26D109.5
C27A—C24A—C25A106.6 (4)C24B—C26B—H26E109.5
C16A—C24A—C25A112.6 (4)H26D—C26B—H26E109.5
C24A—C25A—H25A109.5C24B—C26B—H26F109.5
C24A—C25A—H25B109.5H26D—C26B—H26F109.5
H25A—C25A—H25B109.5H26E—C26B—H26F109.5
C24A—C25A—H25C109.5C24B—C27B—H27D109.5
H25A—C25A—H25C109.5C24B—C27B—H27E109.5
H25B—C25A—H25C109.5H27D—C27B—H27E109.5
C24A—C26A—H26A109.5C24B—C27B—H27F109.5
C24A—C26A—H26B109.5H27D—C27B—H27F109.5
H26A—C26A—H26B109.5H27E—C27B—H27F109.5
C24A—C26A—H26C109.5Si1B—C28B—H28D109.5
H26A—C26A—H26C109.5Si1B—C28B—H28E109.5
H26B—C26A—H26C109.5H28D—C28B—H28E109.5
C24A—C27A—H27A109.5Si1B—C28B—H28F109.5
C24A—C27A—H27B109.5H28D—C28B—H28F109.5
H27A—C27A—H27B109.5H28E—C28B—H28F109.5
C24A—C27A—H27C109.5Si1B—C29B—H29D109.5
H27A—C27A—H27C109.5Si1B—C29B—H29E109.5
H27B—C27A—H27C109.5H29D—C29B—H29E109.5
Si1A—C28A—H28A109.5Si1B—C29B—H29F109.5
Si1A—C28A—H28B109.5H29D—C29B—H29F109.5
H28A—C28A—H28B109.5H29E—C29B—H29F109.5
Si1A—C28A—H28C109.5Si1B—C30B—H30D109.5
H28A—C28A—H28C109.5Si1B—C30B—H30E109.5
H28B—C28A—H28C109.5H30D—C30B—H30E109.5
Si1A—C29A—H29A109.5Si1B—C30B—H30F109.5
Si1A—C29A—H29B109.5H30D—C30B—H30F109.5
H29A—C29A—H29B109.5H30E—C30B—H30F109.5
Si1A—C29A—H29C109.5S1B—C31B—H31D109.5
H29A—C29A—H29C109.5S1B—C31B—H31E109.5
H29B—C29A—H29C109.5H31D—C31B—H31E109.5
Si1A—C30A—H30A109.5S1B—C31B—H31F109.5
Si1A—C30A—H30B109.5H31D—C31B—H31F109.5
H30A—C30A—H30B109.5H31E—C31B—H31F109.5
Si1A—C30A—H30C109.5S1B—C32B—H32D109.5
H30A—C30A—H30C109.5S1B—C32B—H32E109.5
H30B—C30A—H30C109.5H32D—C32B—H32E109.5
S1A—C31A—H31A109.5S1B—C32B—H32F109.5
S1A—C31A—H31B109.5H32D—C32B—H32F109.5
H31A—C31A—H31B109.5H32E—C32B—H32F109.5
S1A—C31A—H31C109.5Cl2C—C1C—Cl1C113.6 (3)
H31A—C31A—H31C109.5Cl2C—C1C—H1C1108.9
H31B—C31A—H31C109.5Cl1C—C1C—H1C1108.9
S1A—C32A—H32A109.5Cl2C—C1C—H1C2108.9
S1A—C32A—H32B109.5Cl1C—C1C—H1C2108.9
H32A—C32A—H32B109.5H1C1—C1C—H1C2107.7
S1A—C32A—H32C109.5Cl2D—C1D—Cl1D114.3 (4)
H32A—C32A—H32C109.5Cl2D—C1D—H1D1108.7
H32B—C32A—H32C109.5Cl1D—C1D—H1D1108.7
N1B—Ru1B—N2B95.09 (15)Cl2D—C1D—H1D2108.7
N1B—Ru1B—N3B78.23 (15)Cl1D—C1D—H1D2108.7
N2B—Ru1B—N3B80.17 (15)H1D1—C1D—H1D2107.6
N1B—Ru1B—S1B90.67 (11)Cl2E—C1E—Cl1E114.2 (5)
N2B—Ru1B—S1B173.35 (11)Cl2E—C1E—H1E1108.7
N3B—Ru1B—S1B97.80 (10)Cl1E—C1E—H1E1108.7
N1B—Ru1B—Cl2B93.91 (12)Cl2E—C1E—H1E2108.7
N2B—Ru1B—Cl2B93.62 (12)Cl1E—C1E—H1E2108.7
N3B—Ru1B—Cl2B169.41 (10)H1E1—C1E—H1E2107.6
N1A—Ru1A—S1A—O2A90.25 (19)N1B—Ru1B—S1B—O2B93.0 (2)
N2A—Ru1A—S1A—O2A62.1 (11)N2B—Ru1B—S1B—O2B57.0 (10)
N3A—Ru1A—S1A—O2A13.23 (18)N3B—Ru1B—S1B—O2B14.8 (2)
Cl2A—Ru1A—S1A—O2A175.14 (16)Cl2B—Ru1B—S1B—O2B173.09 (17)
Cl1A—Ru1A—S1A—O2A86.11 (16)Cl1B—Ru1B—S1B—O2B82.88 (17)
N1A—Ru1A—S1A—C32A145.1 (2)N1B—Ru1B—S1B—C32B141.9 (2)
N2A—Ru1A—S1A—C32A62.6 (11)N2B—Ru1B—S1B—C32B68.0 (10)
N3A—Ru1A—S1A—C32A137.9 (2)N3B—Ru1B—S1B—C32B139.8 (2)
Cl2A—Ru1A—S1A—C32A50.49 (19)Cl2B—Ru1B—S1B—C32B48.03 (19)
Cl1A—Ru1A—S1A—C32A38.54 (19)Cl1B—Ru1B—S1B—C32B42.18 (19)
N1A—Ru1A—S1A—C31A34.4 (2)N1B—Ru1B—S1B—C31B31.8 (2)
N2A—Ru1A—S1A—C31A173.2 (11)N2B—Ru1B—S1B—C31B178.2 (10)
N3A—Ru1A—S1A—C31A111.4 (2)N3B—Ru1B—S1B—C31B110.0 (2)
Cl2A—Ru1A—S1A—C31A60.20 (19)Cl2B—Ru1B—S1B—C31B62.1 (2)
Cl1A—Ru1A—S1A—C31A149.22 (19)Cl1B—Ru1B—S1B—C31B152.3 (2)
C30A—Si1A—O1A—C15A110.8 (4)C30B—Si1B—O1B—C15B115.5 (4)
C28A—Si1A—O1A—C15A9.6 (5)C28B—Si1B—O1B—C15B5.7 (5)
C29A—Si1A—O1A—C15A134.1 (4)C29B—Si1B—O1B—C15B129.4 (4)
N2A—Ru1A—N1A—C1A83.3 (4)N2B—Ru1B—N1B—C1B82.5 (4)
N3A—Ru1A—N1A—C1A160.7 (4)N3B—Ru1B—N1B—C1B161.4 (4)
S1A—Ru1A—N1A—C1A99.3 (4)S1B—Ru1B—N1B—C1B100.8 (4)
Cl2A—Ru1A—N1A—C1A11.1 (4)Cl2B—Ru1B—N1B—C1B11.5 (4)
Cl1A—Ru1A—N1A—C1A170.9 (14)Cl1B—Ru1B—N1B—C1B172.9 (13)
N2A—Ru1A—N1A—C5A104.0 (3)N2B—Ru1B—N1B—C5B102.7 (3)
N3A—Ru1A—N1A—C5A26.6 (3)N3B—Ru1B—N1B—C5B23.8 (3)
S1A—Ru1A—N1A—C5A73.4 (3)S1B—Ru1B—N1B—C5B74.0 (3)
Cl2A—Ru1A—N1A—C5A161.6 (3)Cl2B—Ru1B—N1B—C5B163.3 (3)
Cl1A—Ru1A—N1A—C5A1.8 (19)Cl1B—Ru1B—N1B—C5B12.3 (17)
N1A—Ru1A—N2A—C8A70.1 (3)N1B—Ru1B—N2B—C12B118.2 (4)
N3A—Ru1A—N2A—C8A5.8 (3)N3B—Ru1B—N2B—C12B164.7 (4)
S1A—Ru1A—N2A—C8A82.1 (12)S1B—Ru1B—N2B—C12B91.9 (11)
Cl2A—Ru1A—N2A—C8A165.1 (3)Cl2B—Ru1B—N2B—C12B23.9 (4)
Cl1A—Ru1A—N2A—C8A106.2 (3)Cl1B—Ru1B—N2B—C12B65.9 (4)
N1A—Ru1A—N2A—C12A125.4 (4)N1B—Ru1B—N2B—C8B73.1 (3)
N3A—Ru1A—N2A—C12A158.7 (4)N3B—Ru1B—N2B—C8B4.0 (3)
S1A—Ru1A—N2A—C12A82.4 (12)S1B—Ru1B—N2B—C8B76.8 (11)
Cl2A—Ru1A—N2A—C12A30.4 (3)Cl2B—Ru1B—N2B—C8B167.4 (3)
Cl1A—Ru1A—N2A—C12A58.3 (3)Cl1B—Ru1B—N2B—C8B102.7 (3)
N1A—Ru1A—N3A—C6A38.5 (3)N1B—Ru1B—N3B—C6B36.4 (3)
N2A—Ru1A—N3A—C6A137.6 (3)N2B—Ru1B—N3B—C6B133.8 (3)
S1A—Ru1A—N3A—C6A48.0 (3)S1B—Ru1B—N3B—C6B52.6 (3)
Cl2A—Ru1A—N3A—C6A84.7 (6)Cl2B—Ru1B—N3B—C6B79.1 (7)
Cl1A—Ru1A—N3A—C6A139.7 (3)Cl1B—Ru1B—N3B—C6B142.7 (2)
N1A—Ru1A—N3A—C13A162.1 (3)N1B—Ru1B—N3B—C7B78.2 (3)
N2A—Ru1A—N3A—C13A98.7 (3)N2B—Ru1B—N3B—C7B19.1 (3)
S1A—Ru1A—N3A—C13A75.6 (3)S1B—Ru1B—N3B—C7B167.3 (3)
Cl2A—Ru1A—N3A—C13A151.7 (4)Cl2B—Ru1B—N3B—C7B35.5 (8)
Cl1A—Ru1A—N3A—C13A16.0 (3)Cl1B—Ru1B—N3B—C7B102.6 (3)
N1A—Ru1A—N3A—C7A75.0 (3)N1B—Ru1B—N3B—C13B158.6 (3)
N2A—Ru1A—N3A—C7A24.1 (3)N2B—Ru1B—N3B—C13B104.1 (3)
S1A—Ru1A—N3A—C7A161.5 (2)S1B—Ru1B—N3B—C13B69.5 (3)
Cl2A—Ru1A—N3A—C7A28.9 (7)Cl2B—Ru1B—N3B—C13B158.8 (5)
Cl1A—Ru1A—N3A—C7A106.8 (2)Cl1B—Ru1B—N3B—C13B20.6 (3)
C5A—N1A—C1A—C2A2.0 (8)C5B—N1B—C1B—C2B2.7 (7)
Ru1A—N1A—C1A—C2A170.5 (4)Ru1B—N1B—C1B—C2B171.9 (3)
N1A—C1A—C2A—C3A0.2 (9)N1B—C1B—C2B—C3B1.2 (7)
C1A—C2A—C3A—C4A2.4 (9)C1B—C2B—C3B—C4B1.0 (7)
C2A—C3A—C4A—C5A2.5 (8)C2B—C3B—C4B—C5B1.5 (7)
C1A—N1A—C5A—C4A1.9 (7)C1B—N1B—C5B—C4B2.2 (6)
Ru1A—N1A—C5A—C4A171.5 (4)Ru1B—N1B—C5B—C4B173.1 (3)
C1A—N1A—C5A—C6A178.4 (4)C1B—N1B—C5B—C6B179.9 (4)
Ru1A—N1A—C5A—C6A8.2 (5)Ru1B—N1B—C5B—C6B4.8 (5)
C3A—C4A—C5A—N1A0.3 (8)C3B—C4B—C5B—N1B0.1 (7)
C3A—C4A—C5A—C6A179.4 (5)C3B—C4B—C5B—C6B177.8 (4)
C13A—N3A—C6A—C5A168.6 (4)C7B—N3B—C6B—C5B70.7 (4)
C7A—N3A—C6A—C5A69.5 (5)C13B—N3B—C6B—C5B166.4 (3)
Ru1A—N3A—C6A—C5A44.1 (4)Ru1B—N3B—C6B—C5B43.8 (4)
N1A—C5A—C6A—N3A25.5 (6)N1B—C5B—C6B—N3B27.7 (5)
C4A—C5A—C6A—N3A154.8 (5)C4B—C5B—C6B—N3B154.4 (4)
C6A—N3A—C7A—C8A150.5 (4)C6B—N3B—C7B—C8B143.7 (4)
C13A—N3A—C7A—C8A86.4 (4)C13B—N3B—C7B—C8B92.8 (5)
Ru1A—N3A—C7A—C8A38.3 (4)Ru1B—N3B—C7B—C8B31.5 (4)
C12A—N2A—C8A—C9A1.1 (7)C12B—N2B—C8B—C9B0.6 (7)
Ru1A—N2A—C8A—C9A166.4 (3)Ru1B—N2B—C8B—C9B170.0 (4)
C12A—N2A—C8A—C7A179.4 (4)C12B—N2B—C8B—C7B177.4 (4)
Ru1A—N2A—C8A—C7A15.3 (5)Ru1B—N2B—C8B—C7B13.1 (5)
N3A—C7A—C8A—N2A36.5 (5)N3B—C7B—C8B—N2B30.5 (6)
N3A—C7A—C8A—C9A145.2 (4)N3B—C7B—C8B—C9B152.7 (4)
N2A—C8A—C9A—C10A0.6 (7)N2B—C8B—C9B—C10B0.3 (7)
C7A—C8A—C9A—C10A178.8 (4)C7B—C8B—C9B—C10B176.3 (5)
C8A—C9A—C10A—C11A0.3 (7)C8B—C9B—C10B—C11B1.2 (8)
C9A—C10A—C11A—C12A0.6 (7)C9B—C10B—C11B—C12B1.2 (8)
C8A—N2A—C12A—C11A0.8 (7)C8B—N2B—C12B—C11B0.6 (7)
Ru1A—N2A—C12A—C11A164.8 (3)Ru1B—N2B—C12B—C11B169.0 (4)
C10A—C11A—C12A—N2A0.0 (7)C10B—C11B—C12B—N2B0.3 (8)
C6A—N3A—C13A—C14A59.5 (5)C6B—N3B—C13B—C14B53.5 (5)
C7A—N3A—C13A—C14A60.2 (5)C7B—N3B—C13B—C14B67.6 (5)
Ru1A—N3A—C13A—C14A179.0 (3)Ru1B—N3B—C13B—C14B171.1 (3)
N3A—C13A—C14A—C19A90.4 (5)N3B—C13B—C14B—C19B84.7 (5)
N3A—C13A—C14A—C15A87.5 (5)N3B—C13B—C14B—C15B94.8 (6)
Si1A—O1A—C15A—C16A97.0 (5)Si1B—O1B—C15B—C14B79.7 (6)
Si1A—O1A—C15A—C14A84.5 (5)Si1B—O1B—C15B—C16B102.6 (5)
C19A—C14A—C15A—O1A172.9 (4)C19B—C14B—C15B—O1B174.8 (4)
C13A—C14A—C15A—O1A9.2 (7)C13B—C14B—C15B—O1B5.7 (7)
C19A—C14A—C15A—C16A8.5 (7)C19B—C14B—C15B—C16B7.4 (7)
C13A—C14A—C15A—C16A169.4 (4)C13B—C14B—C15B—C16B172.0 (4)
O1A—C15A—C16A—C17A173.0 (4)O1B—C15B—C16B—C17B176.8 (4)
C14A—C15A—C16A—C17A8.5 (7)C14B—C15B—C16B—C17B5.6 (7)
O1A—C15A—C16A—C24A9.7 (7)O1B—C15B—C16B—C24B1.7 (7)
C14A—C15A—C16A—C24A168.8 (4)C14B—C15B—C16B—C24B176.0 (4)
C15A—C16A—C17A—C18A1.3 (7)C15B—C16B—C17B—C18B0.9 (8)
C24A—C16A—C17A—C18A176.1 (5)C24B—C16B—C17B—C18B179.4 (5)
C16A—C17A—C18A—C19A5.7 (8)C16B—C17B—C18B—C19B1.8 (8)
C16A—C17A—C18A—C20A177.3 (5)C16B—C17B—C18B—C20B177.4 (5)
C17A—C18A—C19A—C14A5.7 (7)C17B—C18B—C19B—C14B0.2 (8)
C20A—C18A—C19A—C14A177.1 (5)C20B—C18B—C19B—C14B175.6 (5)
C15A—C14A—C19A—C18A1.1 (7)C15B—C14B—C19B—C18B4.8 (8)
C13A—C14A—C19A—C18A176.9 (4)C13B—C14B—C19B—C18B174.7 (4)
C17A—C18A—C20A—C22A115.9 (6)C19B—C18B—C20B—C21B177.0 (5)
C19A—C18A—C20A—C22A61.1 (7)C17B—C18B—C20B—C21B7.5 (8)
C17A—C18A—C20A—C23A6.1 (8)C19B—C18B—C20B—C22B60.6 (7)
C19A—C18A—C20A—C23A176.9 (5)C17B—C18B—C20B—C22B114.9 (6)
C17A—C18A—C20A—C21A124.6 (6)C19B—C18B—C20B—C23B57.9 (7)
C19A—C18A—C20A—C21A58.4 (7)C17B—C18B—C20B—C23B126.6 (6)
C15A—C16A—C24A—C26A42.8 (6)C17B—C16B—C24B—C26B136.2 (5)
C17A—C16A—C24A—C26A134.5 (5)C15B—C16B—C24B—C26B45.4 (7)
C15A—C16A—C24A—C27A79.0 (6)C17B—C16B—C24B—C27B101.4 (6)
C17A—C16A—C24A—C27A103.8 (5)C15B—C16B—C24B—C27B77.0 (6)
C15A—C16A—C24A—C25A162.4 (5)C17B—C16B—C24B—C25B16.1 (7)
C17A—C16A—C24A—C25A14.8 (7)C15B—C16B—C24B—C25B165.4 (5)

Experimental details

Crystal data
Chemical formula[RuCl2(C30H43N3OSi)(C2H6OS)]·2CH2Cl2
Mr909.71
Crystal system, space groupTriclinic, P1
Temperature (K)126
a, b, c (Å)10.913 (2), 18.435 (4), 22.413 (5)
α, β, γ (°)82.039 (3), 76.212 (3), 89.148 (3)
V3)4336.4 (15)
Z4
Radiation typeMo Kα
µ (mm1)0.84
Crystal size (mm)0.33 × 0.31 × 0.02
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.769, 0.988
No. of measured, independent and
observed [I > 2σ(I)] reflections
52307, 15775, 8958
Rint0.085
(sin θ/λ)max1)0.604
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.049, 0.124, 0.98
No. of reflections15775
No. of parameters861
No. of restraints24
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.70, 0.57

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

 

Acknowledgements

The donors of the Petroleum Research Fund, administered by the American Chemical Society (ACS-PRF 48003-UFS), supported this research. PJF is grateful to Henry S. LaPierre and Victor G. Young, Jr for their expertise, and to the John Arnold research group for their hospitality.

References

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Volume 65| Part 11| November 2009| Pages m1371-m1372
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