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The crystal structures of the title compounds, [Ru(C7H9Si)2(C26H24P2)2] and [Ru(C4H)2(C26H24P2)2], are described. The metal centre in both complexes has an octahedral coordination geometry, with mutually trans buta-1,3-diynyl ligands form­ing pseudo-linear ruthenium-centred polyyne chains.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103007716/sk1628sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270103007716/sk1628Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270103007716/sk1628IIsup3.hkl
Contains datablock II

CCDC references: 214368; 214369

Comment top

There is currently widespread interest in extended, pseudo-one-dimensional molecules that have the potential to act as 'molecular wires' in future nanoscale electronic/photonic devices (Joachim et al., 2000; Tour et al., 2001). Various organotransition metal complexes have received attention in this context (Ward, 1995), but those that arguably show the greatest promise contain linear polyyne chains that bridge metal centres (Bunz, 1996; Paul & Lapinte, 1998; Low & Bruce, 2001). Until very recently, all of the work on such complexes involved end-capped (generally binuclear) species, which have no potential for extension beyond their metallic terminii. However, several systems in which structural extensions may be possible have now been reported (Wong et al., 2000; Fernández et al., 2001; Xu & Ren, 2001).

The connection of multiple trans-{RuII(P—P)2}2+ (P—P is a chelating diphosphine ligand) centres via polyyne chains is an appealing strategy for the stepwise construction of novel wire-like multinuclear complexes. Attractive features of such compounds include visible transparency, reversible redox behaviour and good stability. The complex trans-RuII(C4H)2(dppe)2, (II) [dppe is 1,2- bis(diphenylphosphino)ethane] is an ideal foundation for such syntheses, but was unknown until very recently (Rigaut et al., 2002). We report here the X-ray crystal structure of (II) and of its bis-trimethylsilylated precursor, (I).

The molecular structures of the complexes (I) and (II) are as indicated by 1H NMR spectroscopy, with trans octahedral coordination geometries. The geometric parameters of the trans-{RuII(P—P)2}2+ units are unremarkable, and those of the C4—Ru—C4 chains are very similar to those found previously in the related complexes trans,trans-RuII(C4R)2(CO)2(PEt3)2 (R = H or SiMe3; Sun et al., 1992). The bond distances are consistent with Ru—CC—CC structures, and the CC bonds remote from the Ru(II) centres show a slight lengthening of ca 0.03 Å on replacement of H atoms with SiMe3. Importantly, the Ru(II)-bis(buta-1,3-diynyl) chains are relatively linear. The largest distortion from linearity is the C60—C61—C62 angle of 170.6 (3)° in (I), and the C53—Ru1—C60 angle in this complex is 174.2 (1)°. Complex (II) is hence an attractive starting point for the preparation of linear multinuclear complexes that can be synthesized by the deprotonation and coordination of the C-atom terminii to further trans-{RuII(P—P)2}2+ or other suitable metal centres.

Experimental top

Although the complexes (I) and (II) were unknown when their structures were solved, their syntheses and characterization have recently been reported by other workers (Rigaut et al., 2002). We used essentially identical synthetic and characterization techniques to those now published, and obtained (I) and (II) as pale-yellow air-stable solids. Crystals of (I) and (II) suitable for single-crystal X-ray diffraction measurements were obtained by slow diffusion of acetone vapour into solutions in dichloromethane at 277 K.

Refinement top

The SiMe3 groups in (I) exhibit rotational thermal disorder, which it was not possible to model in separate, fractionally occupied, positions. As a result, the atomic displacement parameters were constrained to approximate isotropic thermal behaviour.

378 reflections are missing from the dataset of (II), as a result of the data collection strategy being calculated for the initially determined smaller cell, rather than for the subsequently found larger cell.

Structure description top

There is currently widespread interest in extended, pseudo-one-dimensional molecules that have the potential to act as 'molecular wires' in future nanoscale electronic/photonic devices (Joachim et al., 2000; Tour et al., 2001). Various organotransition metal complexes have received attention in this context (Ward, 1995), but those that arguably show the greatest promise contain linear polyyne chains that bridge metal centres (Bunz, 1996; Paul & Lapinte, 1998; Low & Bruce, 2001). Until very recently, all of the work on such complexes involved end-capped (generally binuclear) species, which have no potential for extension beyond their metallic terminii. However, several systems in which structural extensions may be possible have now been reported (Wong et al., 2000; Fernández et al., 2001; Xu & Ren, 2001).

The connection of multiple trans-{RuII(P—P)2}2+ (P—P is a chelating diphosphine ligand) centres via polyyne chains is an appealing strategy for the stepwise construction of novel wire-like multinuclear complexes. Attractive features of such compounds include visible transparency, reversible redox behaviour and good stability. The complex trans-RuII(C4H)2(dppe)2, (II) [dppe is 1,2- bis(diphenylphosphino)ethane] is an ideal foundation for such syntheses, but was unknown until very recently (Rigaut et al., 2002). We report here the X-ray crystal structure of (II) and of its bis-trimethylsilylated precursor, (I).

The molecular structures of the complexes (I) and (II) are as indicated by 1H NMR spectroscopy, with trans octahedral coordination geometries. The geometric parameters of the trans-{RuII(P—P)2}2+ units are unremarkable, and those of the C4—Ru—C4 chains are very similar to those found previously in the related complexes trans,trans-RuII(C4R)2(CO)2(PEt3)2 (R = H or SiMe3; Sun et al., 1992). The bond distances are consistent with Ru—CC—CC structures, and the CC bonds remote from the Ru(II) centres show a slight lengthening of ca 0.03 Å on replacement of H atoms with SiMe3. Importantly, the Ru(II)-bis(buta-1,3-diynyl) chains are relatively linear. The largest distortion from linearity is the C60—C61—C62 angle of 170.6 (3)° in (I), and the C53—Ru1—C60 angle in this complex is 174.2 (1)°. Complex (II) is hence an attractive starting point for the preparation of linear multinuclear complexes that can be synthesized by the deprotonation and coordination of the C-atom terminii to further trans-{RuII(P—P)2}2+ or other suitable metal centres.

Computing details top

Data collection: DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998) for (I); COLLECT (Hooft, 1998) for (II). Cell refinement: DENZO, COLLECT for (I); DENZO (Otwinowski and Minor, 1997) for (II). Data reduction: DENZO, COLLECT for (I); DENZO, COLLECT(Otwinowski and Minor, 1997; Hooft, 1998) for (II). For both compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CAMERON (Watkin, et al., 1993). Software used to prepare material for publication: WinGX (Farrugia, 1998) for (II).

Figures top
[Figure 1] Fig. 1. View of the complex (I), with H atoms omitted and displacement ellipsoids shown at the 35% probability level.
[Figure 2] Fig. 2. View of the complex II, with H atoms omittedand displacement ellipsoids shown at the 35% probability level.
(I) top
Crystal data top
[Ru(C7H9Si)2(C26H24P2)2]Z = 2
Mr = 1140.32F(000) = 1188
Triclinic, P1Dx = 1.247 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.677 (3) ÅCell parameters from 42685 reflections
b = 16.058 (3) Åθ = 2.9–27.5°
c = 16.085 (3) ŵ = 0.44 mm1
α = 110.32 (3)°T = 150 K
β = 93.16 (3)°Block, yellow
γ = 96.36 (3)°0.2 × 0.08 × 0.05 mm
V = 3036.3 (13) Å3
Data collection top
Bruker-Nonius KappaCCD area detector
diffractometer
13576 independent reflections
Radiation source: Bruker-Nonius FR591 rotating anode9761 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.096
Detector resolution: 9.091 pixels mm-1θmax = 27.5°, θmin = 2.9°
φ & ω scansh = 1616
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
k = 2020
Tmin = 0.767, Tmax = 0.986l = 2020
42685 measured reflections
Refinement top
Refinement on F218 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.046 w = 1/[σ2(Fo2) + (0.0565P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.122(Δ/σ)max = 0.059
S = 1.03Δρmax = 0.76 e Å3
13576 reflectionsΔρmin = 0.81 e Å3
665 parameters
Crystal data top
[Ru(C7H9Si)2(C26H24P2)2]γ = 96.36 (3)°
Mr = 1140.32V = 3036.3 (13) Å3
Triclinic, P1Z = 2
a = 12.677 (3) ÅMo Kα radiation
b = 16.058 (3) ŵ = 0.44 mm1
c = 16.085 (3) ÅT = 150 K
α = 110.32 (3)°0.2 × 0.08 × 0.05 mm
β = 93.16 (3)°
Data collection top
Bruker-Nonius KappaCCD area detector
diffractometer
13576 independent reflections
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
9761 reflections with I > 2σ(I)
Tmin = 0.767, Tmax = 0.986Rint = 0.096
42685 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.04618 restraints
wR(F2) = 0.122H-atom parameters constrained
S = 1.03Δρmax = 0.76 e Å3
13576 reflectionsΔρmin = 0.81 e Å3
665 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.4535 (9)0.3114 (8)0.4542 (7)0.024 (3)
C20.4027 (10)0.2839 (9)0.5160 (9)0.035 (3)
H20.3270.27670.51290.042*
C30.4605 (12)0.2666 (11)0.5821 (10)0.049 (4)
H30.42440.24810.62430.059*
C40.5707 (11)0.2763 (10)0.5871 (10)0.045 (4)
H40.61040.2650.63290.054*
C50.6227 (10)0.3025 (9)0.5253 (9)0.039 (3)
H50.69840.30860.52820.046*
C60.5647 (10)0.3200 (8)0.4588 (8)0.031 (3)
H60.60090.33790.41620.037*
C70.4742 (9)0.3804 (8)0.3131 (7)0.023 (3)
C80.5091 (9)0.4720 (8)0.3356 (8)0.029 (3)
H80.47980.51460.38240.035*
C90.5863 (10)0.5010 (9)0.2901 (9)0.036 (3)
H90.60890.56330.30540.043*
C100.6304 (11)0.4396 (10)0.2225 (10)0.043 (4)
H100.68330.45970.19160.052*
C110.5976 (10)0.3493 (10)0.2002 (9)0.038 (3)
H110.6280.30720.15370.046*
C120.5203 (9)0.3194 (9)0.2451 (8)0.030 (3)
H120.49860.25690.22950.036*
C130.3184 (9)0.4371 (8)0.4389 (7)0.024 (3)
H13A0.27830.42310.48470.028*
H13B0.37760.48570.46980.028*
C140.2448 (9)0.4679 (8)0.3810 (8)0.024 (3)
H14A0.28830.50110.35020.029*
H14B0.20030.50950.41930.029*
C150.1556 (9)0.4077 (8)0.2000 (7)0.023 (3)
C160.2527 (10)0.4285 (8)0.1698 (8)0.029 (3)
H160.31740.42450.19990.035*
C170.2560 (12)0.4548 (9)0.0966 (9)0.040 (3)
H170.32260.47040.07780.048*
C180.1616 (13)0.4586 (10)0.0507 (9)0.043 (4)
H180.16360.47630.00020.051*
C190.0659 (12)0.4367 (9)0.0782 (9)0.041 (4)
H190.00160.43970.04680.049*
C200.0613 (10)0.4103 (8)0.1519 (8)0.030 (3)
H200.00580.39390.16950.036*
C210.0241 (9)0.3904 (8)0.3329 (7)0.022 (3)
C220.0079 (10)0.4753 (8)0.3568 (8)0.031 (3)
H220.04070.52450.35630.038*
C230.1087 (10)0.4887 (9)0.3811 (9)0.038 (3)
H230.1290.5470.39740.046*
C240.1813 (10)0.4172 (9)0.3818 (9)0.034 (3)
H240.25120.42640.39810.041*
C250.1507 (10)0.3331 (8)0.3588 (8)0.032 (3)
H250.19960.28420.35970.039*
C260.0492 (9)0.3195 (8)0.3343 (7)0.025 (3)
H260.02910.26110.31830.03*
C270.0088 (9)0.1699 (7)0.1036 (7)0.022 (3)
C280.0567 (10)0.1778 (8)0.0306 (7)0.026 (3)
H280.12830.16660.02360.031*
C290.0009 (10)0.2020 (9)0.0320 (8)0.032 (3)
H290.03420.20630.08210.038*
C300.1028 (11)0.2198 (9)0.0220 (8)0.036 (3)
H300.1410.23630.0650.043*
C310.1502 (11)0.2134 (9)0.0511 (8)0.036 (3)
H310.22120.2260.05850.043*
C320.0950 (9)0.1887 (8)0.1138 (8)0.029 (3)
H320.12850.18480.1640.035*
C330.0241 (9)0.0734 (8)0.2217 (7)0.023 (3)
C340.0979 (9)0.0068 (8)0.1588 (8)0.028 (3)
H340.09570.00310.09720.034*
C350.1739 (10)0.0446 (9)0.1854 (9)0.036 (3)
H350.22340.08960.14220.043*
C360.1779 (10)0.0305 (9)0.2744 (10)0.040 (3)
H360.22990.06630.29240.048*
C370.1073 (11)0.0349 (10)0.3374 (9)0.041 (3)
H370.11150.04520.39890.049*
C380.0296 (10)0.0861 (8)0.3111 (8)0.030 (3)
H380.02020.13040.35480.036*
C390.1470 (9)0.0417 (8)0.1171 (7)0.022 (3)
H39A0.09230.00710.07790.027*
H39B0.19580.06140.07950.027*
C400.2091 (9)0.0091 (8)0.1811 (8)0.025 (3)
H40A0.25530.03390.14730.03*
H40B0.15830.0230.20810.03*
C410.2993 (10)0.0541 (8)0.3590 (8)0.028 (3)
C420.2404 (11)0.0818 (9)0.4309 (9)0.038 (3)
H420.1960.12680.43510.045*
C430.2450 (14)0.0451 (11)0.4968 (10)0.052 (4)
H430.20350.0650.54550.062*
C440.3084 (14)0.0192 (11)0.4929 (11)0.057 (4)
H440.31280.04270.53950.068*
C450.3653 (14)0.0495 (12)0.4215 (12)0.061 (5)
H450.40770.09570.41750.073*
C460.3620 (12)0.0135 (10)0.3546 (10)0.047 (4)
H460.40260.03490.30550.057*
C470.4267 (9)0.0957 (8)0.2355 (9)0.029 (3)
C480.5164 (10)0.1174 (9)0.2986 (10)0.039 (3)
H480.5070.13250.360.046*
C490.6183 (11)0.1169 (10)0.2717 (13)0.053 (4)
H490.67820.13060.31470.064*
C500.6330 (12)0.0966 (11)0.1835 (14)0.064 (5)
H500.70320.0970.16580.076*
C510.5468 (12)0.0755 (10)0.1202 (12)0.053 (4)
H510.55760.06170.05910.064*
C520.4442 (10)0.0744 (9)0.1461 (9)0.036 (3)
H520.3850.05910.10220.044*
C530.2855 (9)0.2308 (7)0.1690 (8)0.024 (3)
C540.3222 (9)0.2306 (8)0.1031 (8)0.026 (3)
C550.3709 (10)0.2369 (9)0.0294 (8)0.033 (3)
C560.4157 (11)0.2450 (10)0.0329 (9)0.043 (4)
C570.456 (2)0.1728 (15)0.2238 (13)0.102 (7)
H57A0.46540.11660.21460.153*
H57B0.50350.18070.26750.153*
H57C0.38210.17060.24580.153*
C580.4536 (19)0.3694 (15)0.1335 (15)0.101 (7)
H58A0.37930.3580.15940.152*
H58B0.50030.38560.17380.152*
H58C0.46180.41880.07590.152*
C590.6320 (16)0.287 (3)0.079 (2)0.246 (8)
H59A0.64370.33020.01790.369*
H59B0.67240.31170.11780.369*
H59C0.6560.23070.08140.369*
C600.1578 (9)0.2581 (8)0.4063 (9)0.025 (3)
C610.1216 (9)0.2718 (7)0.4694 (8)0.024 (3)
C620.0695 (10)0.2741 (8)0.5476 (8)0.029 (3)
C630.0268 (11)0.2753 (9)0.6142 (9)0.037 (3)
C640.0672 (14)0.3441 (12)0.8110 (10)0.066 (5)
H64A0.13060.31390.80860.099*
H64B0.03590.35050.86690.099*
H64C0.08730.40350.80780.099*
C650.1565 (12)0.3291 (12)0.7240 (11)0.059 (5)
H65A0.13960.39140.72780.089*
H65B0.18890.32760.77750.089*
H65C0.20650.29580.67120.089*
C660.0641 (14)0.1610 (10)0.7127 (10)0.055 (4)
H66A0.11630.1270.66150.083*
H66B0.0940.16180.76780.083*
H66C0.0010.13250.7070.083*
Si10.4905 (3)0.2673 (4)0.1176 (3)0.0523 (13)
Si20.0319 (3)0.2767 (3)0.7156 (2)0.0324 (9)
P10.3726 (2)0.3370 (2)0.37021 (19)0.0200 (7)
P20.1563 (2)0.3718 (2)0.29627 (19)0.0191 (7)
P30.0827 (2)0.1369 (2)0.18628 (19)0.0191 (7)
P40.2929 (2)0.1027 (2)0.2712 (2)0.0210 (7)
Ru10.22320 (7)0.23761 (6)0.28515 (5)0.0173 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.027 (6)0.019 (6)0.025 (6)0.002 (5)0.001 (5)0.008 (5)
C20.028 (7)0.043 (8)0.039 (7)0.002 (6)0.002 (6)0.024 (7)
C30.045 (9)0.063 (11)0.052 (9)0.004 (8)0.005 (7)0.042 (8)
C40.044 (9)0.050 (9)0.047 (9)0.000 (7)0.013 (7)0.030 (8)
C50.027 (7)0.039 (8)0.049 (8)0.003 (6)0.009 (6)0.017 (7)
C60.030 (7)0.029 (7)0.032 (7)0.000 (6)0.000 (6)0.012 (6)
C70.018 (6)0.029 (7)0.025 (6)0.001 (5)0.001 (5)0.014 (5)
C80.027 (7)0.030 (7)0.029 (7)0.000 (6)0.001 (5)0.012 (6)
C90.035 (7)0.029 (7)0.047 (8)0.005 (6)0.004 (6)0.021 (6)
C100.034 (8)0.051 (9)0.051 (9)0.006 (7)0.015 (7)0.028 (8)
C110.032 (7)0.046 (9)0.037 (8)0.005 (6)0.015 (6)0.014 (7)
C120.025 (6)0.029 (7)0.034 (7)0.002 (5)0.006 (5)0.010 (6)
C130.028 (6)0.021 (6)0.019 (6)0.002 (5)0.004 (5)0.004 (5)
C140.028 (6)0.018 (6)0.027 (6)0.003 (5)0.005 (5)0.006 (5)
C150.034 (7)0.017 (6)0.020 (6)0.005 (5)0.005 (5)0.008 (5)
C160.033 (7)0.029 (7)0.030 (7)0.007 (6)0.009 (6)0.015 (6)
C170.054 (9)0.037 (8)0.037 (8)0.006 (7)0.019 (7)0.020 (6)
C180.071 (11)0.036 (8)0.026 (7)0.007 (8)0.006 (7)0.016 (6)
C190.054 (9)0.038 (8)0.031 (7)0.007 (7)0.006 (7)0.014 (6)
C200.035 (7)0.024 (7)0.029 (7)0.004 (6)0.000 (6)0.009 (5)
C210.024 (6)0.023 (6)0.021 (6)0.007 (5)0.005 (5)0.008 (5)
C220.028 (7)0.026 (7)0.040 (7)0.004 (5)0.010 (6)0.011 (6)
C230.031 (7)0.023 (7)0.057 (9)0.010 (6)0.017 (7)0.007 (6)
C240.026 (7)0.032 (7)0.042 (8)0.007 (6)0.013 (6)0.007 (6)
C250.026 (7)0.026 (7)0.039 (7)0.001 (5)0.010 (6)0.006 (6)
C260.027 (6)0.022 (6)0.026 (6)0.004 (5)0.008 (5)0.007 (5)
C270.027 (6)0.018 (6)0.019 (6)0.002 (5)0.001 (5)0.004 (5)
C280.028 (6)0.025 (6)0.023 (6)0.002 (5)0.003 (5)0.007 (5)
C290.043 (8)0.032 (7)0.023 (6)0.005 (6)0.006 (6)0.012 (6)
C300.041 (8)0.040 (8)0.028 (7)0.009 (6)0.003 (6)0.015 (6)
C310.033 (7)0.041 (8)0.035 (7)0.014 (6)0.001 (6)0.012 (6)
C320.027 (7)0.032 (7)0.026 (6)0.006 (6)0.004 (5)0.009 (6)
C330.022 (6)0.021 (6)0.027 (6)0.004 (5)0.007 (5)0.010 (5)
C340.027 (6)0.026 (7)0.030 (7)0.001 (5)0.004 (5)0.009 (5)
C350.027 (7)0.031 (7)0.046 (8)0.005 (6)0.005 (6)0.011 (6)
C360.032 (7)0.037 (8)0.055 (9)0.004 (6)0.014 (7)0.024 (7)
C370.044 (8)0.046 (9)0.037 (8)0.002 (7)0.014 (7)0.021 (7)
C380.034 (7)0.025 (7)0.030 (7)0.003 (5)0.005 (6)0.010 (5)
C390.022 (6)0.022 (6)0.020 (6)0.002 (5)0.005 (5)0.004 (5)
C400.026 (6)0.019 (6)0.030 (6)0.003 (5)0.005 (5)0.009 (5)
C410.031 (7)0.022 (6)0.032 (7)0.002 (5)0.001 (6)0.012 (5)
C420.048 (8)0.035 (8)0.038 (8)0.013 (7)0.011 (7)0.021 (6)
C430.079 (12)0.046 (9)0.042 (8)0.015 (9)0.018 (8)0.028 (7)
C440.073 (11)0.060 (11)0.058 (10)0.013 (9)0.006 (9)0.046 (9)
C450.070 (12)0.059 (11)0.082 (12)0.031 (9)0.017 (10)0.053 (10)
C460.057 (9)0.046 (9)0.057 (9)0.025 (8)0.022 (8)0.033 (8)
C470.023 (6)0.020 (6)0.045 (8)0.008 (5)0.009 (6)0.011 (6)
C480.028 (7)0.027 (7)0.059 (9)0.006 (6)0.001 (6)0.012 (7)
C490.026 (8)0.034 (8)0.095 (14)0.005 (6)0.001 (8)0.018 (9)
C500.029 (8)0.048 (10)0.115 (16)0.012 (7)0.031 (10)0.024 (10)
C510.044 (9)0.043 (9)0.074 (11)0.011 (7)0.034 (9)0.016 (8)
C520.030 (7)0.030 (7)0.047 (8)0.005 (6)0.017 (6)0.009 (6)
C530.020 (6)0.015 (6)0.034 (7)0.002 (5)0.001 (5)0.007 (5)
C540.021 (6)0.023 (6)0.033 (7)0.003 (5)0.004 (5)0.008 (5)
C550.036 (7)0.038 (8)0.029 (7)0.006 (6)0.012 (6)0.014 (6)
C560.041 (8)0.052 (9)0.037 (8)0.005 (7)0.010 (7)0.019 (7)
C570.148 (8)0.090 (8)0.081 (7)0.016 (4)0.062 (5)0.039 (5)
C580.121 (8)0.093 (8)0.096 (8)0.013 (4)0.015 (4)0.043 (5)
C590.035 (8)0.606 (9)0.243 (9)0.034 (5)0.026 (4)0.335 (5)
C600.016 (6)0.018 (6)0.044 (8)0.002 (5)0.006 (6)0.018 (6)
C610.026 (6)0.012 (6)0.027 (7)0.004 (5)0.009 (6)0.000 (5)
C620.035 (7)0.028 (7)0.025 (6)0.003 (6)0.007 (6)0.009 (5)
C630.047 (8)0.036 (8)0.030 (7)0.007 (7)0.014 (6)0.011 (6)
C640.081 (12)0.072 (13)0.039 (9)0.007 (10)0.005 (9)0.018 (9)
C650.053 (10)0.073 (12)0.063 (11)0.020 (9)0.019 (8)0.034 (9)
C660.080 (12)0.043 (9)0.047 (9)0.001 (8)0.014 (8)0.022 (7)
Si10.040 (2)0.090 (4)0.046 (2)0.010 (2)0.0177 (19)0.046 (3)
Si20.040 (2)0.035 (2)0.0240 (18)0.0033 (17)0.0102 (16)0.0127 (16)
P10.0203 (15)0.0194 (15)0.0200 (15)0.0018 (12)0.0024 (12)0.0070 (12)
P20.0204 (15)0.0183 (15)0.0196 (15)0.0031 (12)0.0047 (12)0.0074 (12)
P30.0202 (15)0.0183 (15)0.0189 (14)0.0020 (12)0.0046 (12)0.0066 (12)
P40.0207 (15)0.0193 (16)0.0246 (16)0.0039 (12)0.0048 (13)0.0091 (13)
Ru10.0184 (5)0.0173 (5)0.0170 (5)0.0025 (4)0.0049 (4)0.0066 (4)
Geometric parameters (Å, º) top
C1—C21.381 (17)C36—C371.372 (19)
C1—C61.398 (16)C36—H360.9500
C1—P11.837 (12)C37—C381.390 (18)
C2—C31.381 (18)C37—H370.9500
C2—H20.9500C38—H380.9500
C3—C41.384 (19)C39—C401.527 (16)
C3—H30.9500C39—P31.852 (11)
C4—C51.38 (2)C39—H39A0.9900
C4—H40.9500C39—H39B0.9900
C5—C61.391 (17)C40—P41.857 (11)
C5—H50.9500C40—H40A0.9900
C6—H60.9500C40—H40B0.9900
C7—C121.396 (16)C41—C421.380 (18)
C7—C81.400 (17)C41—C461.400 (18)
C7—P11.834 (12)C41—P41.837 (13)
C8—C91.387 (17)C42—C431.382 (19)
C8—H80.9500C42—H420.9500
C9—C101.383 (19)C43—C441.37 (2)
C9—H90.9500C43—H430.9500
C10—C111.37 (2)C44—C451.36 (2)
C10—H100.9500C44—H440.9500
C11—C121.389 (18)C45—C461.39 (2)
C11—H110.9500C45—H450.9500
C12—H120.9500C46—H460.9500
C13—C141.521 (16)C47—C521.395 (18)
C13—P11.835 (11)C47—C481.408 (17)
C13—H13A0.9900C47—P41.824 (12)
C13—H13B0.9900C48—C491.384 (19)
C14—P21.866 (11)C48—H480.9500
C14—H14A0.9900C49—C501.37 (2)
C14—H14B0.9900C49—H490.9500
C15—C201.400 (16)C50—C511.38 (2)
C15—C161.397 (17)C50—H500.9500
C15—P21.830 (12)C51—C521.387 (18)
C16—C171.383 (18)C51—H510.9500
C16—H160.9500C52—H520.9500
C17—C181.39 (2)C53—C541.179 (17)
C17—H170.9500C53—Ru12.041 (13)
C18—C191.36 (2)C54—C551.395 (18)
C18—H180.9500C55—C561.217 (19)
C19—C201.392 (18)C56—Si11.814 (15)
C19—H190.9500C57—Si11.84 (2)
C20—H200.9500C57—H57A0.9800
C21—C261.394 (16)C57—H57B0.9800
C21—C221.395 (17)C57—H57C0.9800
C21—P21.828 (11)C58—Si11.85 (2)
C22—C231.375 (17)C58—H58A0.9800
C22—H220.9500C58—H58B0.9800
C23—C241.393 (18)C58—H58C0.9800
C23—H230.9500C59—Si11.82 (2)
C24—C251.376 (18)C59—H59A0.9800
C24—H240.9500C59—H59B0.9800
C25—C261.385 (16)C59—H59C0.9800
C25—H250.9500C60—C611.099 (17)
C26—H260.9500C60—Ru12.095 (14)
C27—C281.388 (16)C61—C621.444 (18)
C27—C321.389 (16)C62—C631.221 (17)
C27—P31.841 (12)C63—Si21.824 (14)
C28—C291.385 (17)C64—Si21.853 (15)
C28—H280.9500C64—H64A0.9800
C29—C301.383 (18)C64—H64B0.9800
C29—H290.9500C64—H64C0.9800
C30—C311.379 (18)C65—Si21.860 (15)
C30—H300.9500C65—H65A0.9800
C31—C321.388 (17)C65—H65B0.9800
C31—H310.9500C65—H65C0.9800
C32—H320.9500C66—Si21.841 (15)
C33—C381.388 (16)C66—H66A0.9800
C33—C341.402 (16)C66—H66B0.9800
C33—P31.838 (12)C66—H66C0.9800
C34—C351.380 (17)P1—Ru12.352 (3)
C34—H340.9500P2—Ru12.356 (3)
C35—C361.373 (19)P3—Ru12.362 (3)
C35—H350.9500P4—Ru12.373 (3)
C2—C1—C6118.8 (11)C42—C41—C46117.5 (12)
C2—C1—P1118.9 (9)C42—C41—P4121.0 (10)
C6—C1—P1122.3 (10)C46—C41—P4121.5 (10)
C1—C2—C3120.9 (12)C41—C42—C43121.0 (13)
C1—C2—H2119.6C41—C42—H42119.5
C3—C2—H2119.5C43—C42—H42119.5
C4—C3—C2120.2 (14)C44—C43—C42120.9 (15)
C4—C3—H3119.9C44—C43—H43119.5
C2—C3—H3119.9C42—C43—H43119.5
C5—C4—C3119.8 (13)C45—C44—C43119.3 (15)
C5—C4—H4120.1C45—C44—H44120.3
C3—C4—H4120.1C43—C44—H44120.3
C4—C5—C6120.2 (12)C44—C45—C46120.7 (15)
C4—C5—H5119.9C44—C45—H45119.7
C6—C5—H5119.9C46—C45—H45119.7
C5—C6—C1120.2 (12)C45—C46—C41120.5 (14)
C5—C6—H6119.9C45—C46—H46119.7
C1—C6—H6119.9C41—C46—H46119.7
C12—C7—C8118.4 (11)C52—C47—C48117.9 (12)
C12—C7—P1118.7 (9)C52—C47—P4121.4 (9)
C8—C7—P1122.9 (9)C48—C47—P4120.6 (10)
C9—C8—C7120.5 (12)C49—C48—C47120.5 (14)
C9—C8—H8119.8C49—C48—H48119.7
C7—C8—H8119.8C47—C48—H48119.8
C10—C9—C8120.3 (13)C50—C49—C48120.3 (15)
C10—C9—H9119.9C50—C49—H49119.9
C8—C9—H9119.8C48—C49—H49119.9
C11—C10—C9119.9 (13)C49—C50—C51120.6 (14)
C11—C10—H10120.0C49—C50—H50119.7
C9—C10—H10120.1C51—C50—H50119.7
C10—C11—C12120.4 (13)C50—C51—C52119.7 (15)
C10—C11—H11119.8C50—C51—H51120.2
C12—C11—H11119.8C52—C51—H51120.2
C11—C12—C7120.6 (12)C51—C52—C47121.0 (13)
C11—C12—H12119.7C51—C52—H52119.5
C7—C12—H12119.7C47—C52—H52119.5
C14—C13—P1110.2 (7)C54—C53—Ru1177.3 (11)
C14—C13—H13A109.6C53—C54—C55175.3 (14)
P1—C13—H13A109.6C56—C55—C54177.8 (15)
C14—C13—H13B109.6C55—C56—Si1174.1 (14)
P1—C13—H13B109.6Si1—C57—H57A109.4
H13A—C13—H13B108.1Si1—C57—H57B109.4
C13—C14—P2112.0 (8)H57A—C57—H57B109.5
C13—C14—H14A109.2Si1—C57—H57C109.6
P2—C14—H14A109.2H57A—C57—H57C109.5
C13—C14—H14B109.2H57B—C57—H57C109.5
P2—C14—H14B109.2Si1—C58—H58A109.4
H14A—C14—H14B107.9Si1—C58—H58B109.5
C20—C15—C16118.2 (11)H58A—C58—H58B109.5
C20—C15—P2122.7 (10)Si1—C58—H58C109.5
C16—C15—P2119.0 (9)H58A—C58—H58C109.5
C17—C16—C15121.0 (12)H58B—C58—H58C109.5
C17—C16—H16119.5Si1—C59—H59A109.5
C15—C16—H16119.5Si1—C59—H59B109.5
C16—C17—C18119.9 (14)H59A—C59—H59B109.5
C16—C17—H17120.1Si1—C59—H59C109.5
C18—C17—H17120.1H59A—C59—H59C109.5
C19—C18—C17119.9 (13)H59B—C59—H59C109.5
C19—C18—H18120.1C61—C60—Ru1177.0 (11)
C17—C18—H18120.0C60—C61—C62170.7 (13)
C18—C19—C20120.9 (13)C63—C62—C61178.9 (15)
C18—C19—H19119.6C62—C63—Si2177.7 (13)
C20—C19—H19119.6Si2—C64—H64A109.5
C19—C20—C15120.1 (13)Si2—C64—H64B109.5
C19—C20—H20120.0H64A—C64—H64B109.5
C15—C20—H20119.9Si2—C64—H64C109.5
C26—C21—C22118.1 (11)H64A—C64—H64C109.5
C26—C21—P2121.0 (9)H64B—C64—H64C109.5
C22—C21—P2120.9 (9)Si2—C65—H65A109.5
C23—C22—C21121.0 (12)Si2—C65—H65B109.5
C23—C22—H22119.5H65A—C65—H65B109.5
C21—C22—H22119.5Si2—C65—H65C109.5
C22—C23—C24120.4 (12)H65A—C65—H65C109.5
C22—C23—H23119.8H65B—C65—H65C109.5
C24—C23—H23119.8Si2—C66—H66A109.5
C25—C24—C23119.3 (12)Si2—C66—H66B109.5
C25—C24—H24120.3H66A—C66—H66B109.5
C23—C24—H24120.3Si2—C66—H66C109.5
C24—C25—C26120.4 (12)H66A—C66—H66C109.5
C24—C25—H25119.8H66B—C66—H66C109.5
C26—C25—H25119.8C56—Si1—C59108.5 (9)
C25—C26—C21120.9 (11)C56—Si1—C58109.6 (9)
C25—C26—H26119.6C59—Si1—C58108.4 (16)
C21—C26—H26119.6C56—Si1—C57109.2 (8)
C28—C27—C32118.9 (11)C59—Si1—C57112.9 (18)
C28—C27—P3120.5 (9)C58—Si1—C57108.2 (10)
C32—C27—P3120.7 (9)C63—Si2—C66109.5 (7)
C29—C28—C27120.5 (12)C63—Si2—C64107.3 (7)
C29—C28—H28119.7C66—Si2—C64111.4 (8)
C27—C28—H28119.8C63—Si2—C65109.9 (7)
C30—C29—C28120.5 (12)C66—Si2—C65109.0 (8)
C30—C29—H29119.8C64—Si2—C65109.8 (8)
C28—C29—H29119.8C13—P1—C1101.9 (5)
C29—C30—C31119.2 (12)C13—P1—C7104.2 (6)
C29—C30—H30120.4C1—P1—C7102.5 (5)
C31—C30—H30120.4C13—P1—Ru1105.0 (4)
C30—C31—C32120.7 (12)C1—P1—Ru1121.6 (4)
C30—C31—H31119.7C7—P1—Ru1119.1 (4)
C32—C31—H31119.7C21—P2—C15102.4 (5)
C31—C32—C27120.2 (12)C21—P2—C14102.5 (5)
C31—C32—H32119.9C15—P2—C14100.9 (5)
C27—C32—H32119.9C21—P2—Ru1120.4 (4)
C38—C33—C34118.2 (11)C15—P2—Ru1118.8 (4)
C38—C33—P3120.8 (9)C14—P2—Ru1109.0 (4)
C34—C33—P3120.9 (9)C33—P3—C27102.0 (5)
C35—C34—C33120.7 (12)C33—P3—C3998.7 (5)
C35—C34—H34119.6C27—P3—C39103.5 (5)
C33—C34—H34119.6C33—P3—Ru1123.6 (4)
C36—C35—C34120.0 (12)C27—P3—Ru1120.3 (4)
C36—C35—H35120.0C39—P3—Ru1104.9 (4)
C34—C35—H35120.0C47—P4—C41101.4 (6)
C35—C36—C37120.5 (13)C47—P4—C40103.4 (5)
C35—C36—H36119.8C41—P4—C40100.2 (5)
C37—C36—H36119.7C47—P4—Ru1116.0 (4)
C36—C37—C38119.9 (13)C41—P4—Ru1124.6 (4)
C36—C37—H37120.1C40—P4—Ru1108.4 (4)
C38—C37—H37120.1C53—Ru1—C60174.2 (4)
C33—C38—C37120.7 (12)C53—Ru1—P191.5 (3)
C33—C38—H38119.6C60—Ru1—P186.3 (3)
C37—C38—H38119.6C53—Ru1—P291.5 (3)
C40—C39—P3107.0 (7)C60—Ru1—P282.9 (3)
C40—C39—H39A110.3P1—Ru1—P282.76 (11)
P3—C39—H39A110.3C53—Ru1—P382.4 (3)
C40—C39—H39B110.3C60—Ru1—P399.8 (3)
P3—C39—H39B110.3P1—Ru1—P3173.93 (10)
H39A—C39—H39B108.6P2—Ru1—P397.77 (11)
C39—C40—P4112.2 (8)C53—Ru1—P487.1 (3)
C39—C40—H40A109.2C60—Ru1—P498.4 (3)
P4—C40—H40A109.2P1—Ru1—P497.05 (11)
C39—C40—H40B109.2P2—Ru1—P4178.66 (11)
P4—C40—H40B109.2P3—Ru1—P482.28 (11)
H40A—C40—H40B107.9
(II) top
Crystal data top
[Ru(C4H)2(C26H24P2)2]Z = 2
Mr = 995.95F(000) = 1028
Triclinic, P1Dx = 1.396 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.9017 (2) ÅCell parameters from 19034 reflections
b = 13.2669 (3) Åθ = 2.9–27.5°
c = 17.1934 (4) ŵ = 0.51 mm1
α = 79.416 (1)°T = 120 K
β = 76.195 (1)°Plate, colourless
γ = 64.499 (2)°0.15 × 0.1 × 0.06 mm
V = 2369.38 (9) Å3
Data collection top
Bruker-Nonius KappaCCD area-detector
diffractometer
4873 reflections with I > 2σ(I)
φ and ω scansRint = 0.073
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
θmax = 25.0°, θmin = 3.1°
Tmin = 0.780, Tmax = 0.872h = 1414
26880 measured reflectionsk = 1515
7995 independent reflectionsl = 2020
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.038 w = 1/[σ2(Fo2) + (0.0417P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.091(Δ/σ)max = 0.018
S = 0.94Δρmax = 0.60 e Å3
7995 reflectionsΔρmin = 0.54 e Å3
589 parameters
Crystal data top
[Ru(C4H)2(C26H24P2)2]γ = 64.499 (2)°
Mr = 995.95V = 2369.38 (9) Å3
Triclinic, P1Z = 2
a = 11.9017 (2) ÅMo Kα radiation
b = 13.2669 (3) ŵ = 0.51 mm1
c = 17.1934 (4) ÅT = 120 K
α = 79.416 (1)°0.15 × 0.1 × 0.06 mm
β = 76.195 (1)°
Data collection top
Bruker-Nonius KappaCCD area-detector
diffractometer
7995 independent reflections
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
4873 reflections with I > 2σ(I)
Tmin = 0.780, Tmax = 0.872Rint = 0.073
26880 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0380 restraints
wR(F2) = 0.091H-atom parameters constrained
S = 0.94Δρmax = 0.60 e Å3
7995 reflectionsΔρmin = 0.54 e Å3
589 parameters
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ru10000.00909 (11)
P10.20305 (9)0.14947 (8)0.02658 (6)0.0106 (2)
P20.11058 (9)0.11048 (8)0.06878 (5)0.0106 (2)
C10.3055 (4)0.2273 (3)0.0481 (2)0.0147 (8)
C20.3006 (4)0.1729 (3)0.1119 (2)0.0194 (9)
H20.24160.09740.11730.023*
C30.3803 (4)0.2270 (3)0.1675 (2)0.0234 (9)
H30.37470.18870.21080.028*
C40.4671 (4)0.3354 (3)0.1601 (2)0.0254 (10)
H40.52070.37250.19870.03*
C50.4769 (4)0.3911 (3)0.0964 (3)0.0320 (11)
H50.53790.46590.09080.038*
C60.3968 (4)0.3367 (3)0.0410 (3)0.0266 (10)
H60.40440.37490.00290.032*
C70.2088 (4)0.2633 (3)0.0756 (2)0.0140 (8)
C80.1878 (4)0.3537 (3)0.0296 (2)0.0161 (9)
H80.17650.35820.02730.019*
C90.1831 (4)0.4373 (3)0.0653 (3)0.0224 (10)
H90.16810.4980.03290.027*
C100.2004 (4)0.4316 (4)0.1482 (3)0.0273 (10)
H100.19740.48850.1730.033*
C110.2219 (4)0.3436 (3)0.1943 (2)0.0256 (10)
H110.23290.33960.25120.031*
C120.2277 (4)0.2601 (3)0.1590 (2)0.0207 (9)
H120.24470.20060.1920.025*
C130.3103 (4)0.0925 (3)0.0979 (2)0.0144 (8)
H13A0.36430.14680.1380.017*
H13B0.36640.08340.0680.017*
C140.2378 (4)0.0207 (3)0.1418 (2)0.0131 (8)
H14A0.29610.05720.16810.016*
H14B0.20140.00920.18380.016*
C150.0366 (4)0.2374 (3)0.1341 (2)0.0134 (8)
C160.0308 (4)0.2338 (3)0.1889 (2)0.0188 (9)
H160.03780.16580.19150.023*
C170.0879 (4)0.3274 (3)0.2397 (2)0.0259 (10)
H170.13290.32310.27680.031*
C180.0791 (4)0.4269 (3)0.2362 (3)0.0279 (10)
H180.11840.49110.27090.034*
C190.0135 (4)0.4329 (3)0.1826 (2)0.0236 (10)
H190.00850.50170.180.028*
C200.0460 (4)0.3384 (3)0.1317 (2)0.0198 (9)
H200.09260.34290.09560.024*
C210.1909 (4)0.1585 (3)0.0147 (2)0.0144 (9)
C220.1240 (4)0.2113 (3)0.0557 (2)0.0146 (9)
H220.04160.21420.07780.018*
C230.1767 (4)0.2593 (3)0.0935 (2)0.0199 (9)
H230.130.29540.14090.024*
C240.2966 (4)0.2551 (3)0.0627 (2)0.0262 (10)
H240.33180.28890.08880.031*
C250.3656 (4)0.2017 (3)0.0059 (2)0.0231 (10)
H250.44850.19840.02690.028*
C260.3137 (4)0.1527 (3)0.0444 (2)0.0185 (9)
H260.36190.11510.0910.022*
C270.0143 (3)0.0217 (3)0.1117 (2)0.0135 (8)
C280.0252 (3)0.0320 (3)0.1770 (2)0.0123 (8)
C290.0563 (4)0.0334 (3)0.2500 (2)0.0220 (9)
C300.0895 (4)0.0287 (4)0.3112 (3)0.0314 (11)
H300.1160.0250.360.038*
Ru1'0.500.50.00848 (11)
P1'0.60825 (9)0.11348 (8)0.43363 (5)0.0098 (2)
P2'0.70135 (9)0.14628 (8)0.46261 (6)0.0107 (2)
C1'0.6964 (4)0.1497 (3)0.4897 (2)0.0118 (8)
C2'0.8209 (4)0.1380 (3)0.4596 (2)0.0199 (9)
H2'0.8640.10530.41040.024*
C3'0.8818 (4)0.1736 (4)0.5007 (2)0.0265 (10)
H3'0.96660.16490.47980.032*
C4'0.8203 (4)0.2217 (4)0.5719 (2)0.0282 (10)
H4'0.86230.24590.60010.034*
C5'0.6969 (4)0.2343 (3)0.6018 (2)0.0203 (9)
H5'0.65350.26930.65010.024*
C6'0.6361 (4)0.1966 (3)0.5622 (2)0.0152 (9)
H6'0.55250.20290.58470.018*
C7'0.5309 (4)0.2484 (3)0.3758 (2)0.0146 (8)
C8'0.5304 (4)0.3476 (3)0.3906 (2)0.0219 (9)
H8'0.57530.34690.42970.026*
C9'0.4650 (4)0.4483 (3)0.3487 (3)0.0307 (11)
H9'0.4630.51630.36060.037*
C10'0.4028 (4)0.4500 (4)0.2899 (3)0.0376 (12)
H10'0.35880.51880.26080.045*
C11'0.4049 (4)0.3513 (4)0.2736 (3)0.0359 (12)
H11'0.3630.35220.23270.043*
C12'0.4678 (4)0.2506 (3)0.3163 (2)0.0243 (10)
H12'0.46780.18310.30510.029*
C13'0.7291 (4)0.0315 (3)0.3537 (2)0.0139 (8)
H13C0.68780.0270.31160.017*
H13D0.78690.0690.32850.017*
C14'0.8037 (4)0.0852 (3)0.3893 (2)0.0159 (8)
H14C0.86650.08250.41670.019*
H14D0.85050.13480.34530.019*
C15'0.7016 (3)0.2552 (3)0.4102 (2)0.0137 (8)
C16'0.7037 (4)0.2407 (3)0.3270 (2)0.0181 (9)
H16'0.71370.17710.29590.022*
C17'0.6912 (4)0.3190 (3)0.2900 (2)0.0216 (9)
H17'0.69150.30830.23380.026*
C18'0.6782 (4)0.4126 (3)0.3350 (2)0.0240 (10)
H18'0.66930.4660.30960.029*
C19'0.6782 (4)0.4284 (3)0.4168 (3)0.0213 (9)
H19'0.67080.49330.44750.026*
C20'0.6888 (4)0.3496 (3)0.4541 (2)0.0169 (9)
H20'0.68740.36040.51040.02*
C21'0.8142 (4)0.2341 (3)0.5294 (2)0.0151 (9)
C22'0.9212 (4)0.3278 (3)0.5001 (3)0.0254 (10)
H22'0.93150.34730.44760.03*
C23'1.0118 (4)0.3918 (3)0.5476 (3)0.0315 (11)
H23'1.0840.45470.52740.038*
C24'0.9974 (4)0.3643 (4)0.6241 (3)0.0314 (11)
H24'1.05880.40880.65680.038*
C25'0.8935 (4)0.2720 (4)0.6526 (2)0.0321 (11)
H25'0.88360.25260.70510.039*
C26'0.8036 (4)0.2074 (3)0.6053 (2)0.0246 (10)
H26'0.73310.14340.62560.03*
C27'0.5257 (3)0.0084 (3)0.6126 (2)0.0137 (8)
C28'0.5382 (4)0.0099 (3)0.6789 (2)0.0138 (8)
C29'0.5645 (4)0.0005 (3)0.7551 (2)0.0169 (9)
C30'0.5895 (4)0.0120 (4)0.8207 (2)0.0285 (10)
H30'0.60940.02190.87270.034*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0089 (2)0.0092 (2)0.0090 (2)0.00416 (18)0.00036 (17)0.00097 (17)
P10.0094 (5)0.0093 (5)0.0121 (5)0.0037 (4)0.0003 (4)0.0009 (4)
P20.0110 (5)0.0109 (5)0.0104 (5)0.0059 (4)0.0003 (4)0.0009 (4)
C10.0084 (19)0.014 (2)0.022 (2)0.0054 (16)0.0038 (16)0.0003 (16)
C20.014 (2)0.024 (2)0.018 (2)0.0058 (18)0.0012 (16)0.0057 (17)
C30.023 (2)0.035 (3)0.013 (2)0.013 (2)0.0046 (17)0.0013 (17)
C40.026 (2)0.025 (2)0.029 (2)0.016 (2)0.0112 (19)0.0117 (19)
C50.025 (2)0.012 (2)0.059 (3)0.0002 (19)0.023 (2)0.001 (2)
C60.023 (2)0.020 (2)0.041 (3)0.0068 (19)0.013 (2)0.0084 (19)
C70.0079 (19)0.016 (2)0.017 (2)0.0039 (16)0.0006 (15)0.0039 (16)
C80.011 (2)0.015 (2)0.021 (2)0.0054 (17)0.0017 (16)0.0041 (16)
C90.013 (2)0.017 (2)0.039 (3)0.0079 (18)0.0010 (18)0.0071 (18)
C100.024 (2)0.026 (2)0.036 (3)0.010 (2)0.001 (2)0.017 (2)
C110.027 (2)0.029 (2)0.020 (2)0.007 (2)0.0013 (18)0.0142 (19)
C120.020 (2)0.021 (2)0.020 (2)0.0083 (18)0.0007 (17)0.0038 (17)
C130.010 (2)0.011 (2)0.019 (2)0.0015 (16)0.0004 (16)0.0019 (16)
C140.015 (2)0.017 (2)0.0087 (19)0.0082 (17)0.0010 (15)0.0028 (15)
C150.014 (2)0.011 (2)0.0122 (19)0.0042 (16)0.0023 (16)0.0000 (15)
C160.024 (2)0.014 (2)0.017 (2)0.0074 (18)0.0045 (17)0.0012 (16)
C170.026 (2)0.024 (2)0.029 (2)0.0091 (19)0.0137 (19)0.0032 (18)
C180.028 (2)0.021 (2)0.034 (2)0.0104 (19)0.014 (2)0.0128 (19)
C190.022 (2)0.011 (2)0.036 (2)0.0074 (18)0.0037 (19)0.0031 (18)
C200.015 (2)0.017 (2)0.028 (2)0.0093 (17)0.0030 (17)0.0027 (17)
C210.017 (2)0.013 (2)0.012 (2)0.0062 (18)0.0013 (16)0.0022 (16)
C220.018 (2)0.011 (2)0.016 (2)0.0066 (17)0.0044 (17)0.0023 (16)
C230.025 (2)0.018 (2)0.019 (2)0.0093 (18)0.0028 (17)0.0058 (16)
C240.032 (3)0.031 (3)0.027 (2)0.022 (2)0.012 (2)0.0034 (19)
C250.024 (2)0.033 (2)0.019 (2)0.019 (2)0.0034 (18)0.0018 (18)
C260.018 (2)0.023 (2)0.017 (2)0.0114 (18)0.0016 (17)0.0005 (17)
C270.007 (2)0.008 (2)0.022 (2)0.0029 (16)0.0011 (16)0.0031 (16)
C280.0069 (19)0.0085 (19)0.021 (2)0.0030 (15)0.0018 (16)0.0059 (15)
C290.017 (2)0.025 (2)0.021 (2)0.0063 (18)0.0006 (17)0.0056 (17)
C300.030 (3)0.041 (3)0.024 (2)0.010 (2)0.006 (2)0.013 (2)
Ru1'0.0086 (2)0.0069 (2)0.0095 (2)0.00309 (18)0.00079 (17)0.00111 (17)
P1'0.0103 (5)0.0077 (5)0.0117 (5)0.0052 (4)0.0009 (4)0.0006 (4)
P2'0.0072 (5)0.0082 (5)0.0142 (5)0.0007 (4)0.0008 (4)0.0031 (4)
C1'0.013 (2)0.0061 (19)0.016 (2)0.0025 (16)0.0045 (16)0.0004 (15)
C2'0.019 (2)0.027 (2)0.015 (2)0.0104 (19)0.0017 (17)0.0073 (17)
C3'0.019 (2)0.038 (3)0.031 (2)0.020 (2)0.0007 (19)0.005 (2)
C4'0.032 (3)0.042 (3)0.024 (2)0.026 (2)0.0075 (19)0.008 (2)
C5'0.030 (2)0.019 (2)0.015 (2)0.0135 (19)0.0022 (17)0.0039 (16)
C6'0.015 (2)0.011 (2)0.016 (2)0.0049 (17)0.0016 (16)0.0038 (16)
C7'0.0089 (19)0.016 (2)0.017 (2)0.0065 (17)0.0001 (16)0.0034 (16)
C8'0.022 (2)0.015 (2)0.027 (2)0.0079 (18)0.0019 (18)0.0006 (17)
C9'0.019 (2)0.011 (2)0.055 (3)0.0036 (18)0.007 (2)0.007 (2)
C10'0.023 (2)0.023 (3)0.062 (3)0.011 (2)0.017 (2)0.025 (2)
C11'0.035 (3)0.035 (3)0.043 (3)0.019 (2)0.024 (2)0.020 (2)
C12'0.023 (2)0.021 (2)0.034 (2)0.0139 (19)0.0123 (19)0.0071 (19)
C13'0.015 (2)0.018 (2)0.013 (2)0.0106 (18)0.0033 (16)0.0012 (16)
C14'0.012 (2)0.018 (2)0.018 (2)0.0083 (17)0.0032 (16)0.0045 (16)
C15'0.0075 (19)0.010 (2)0.019 (2)0.0000 (16)0.0022 (16)0.0047 (16)
C16'0.016 (2)0.019 (2)0.016 (2)0.0044 (17)0.0017 (16)0.0065 (16)
C17'0.020 (2)0.028 (2)0.019 (2)0.0092 (19)0.0014 (17)0.0111 (18)
C18'0.013 (2)0.027 (2)0.037 (3)0.0064 (18)0.0003 (18)0.022 (2)
C19'0.014 (2)0.012 (2)0.037 (3)0.0032 (17)0.0051 (18)0.0026 (18)
C20'0.014 (2)0.013 (2)0.023 (2)0.0040 (17)0.0054 (16)0.0017 (16)
C21'0.014 (2)0.0051 (19)0.025 (2)0.0050 (16)0.0032 (16)0.0037 (16)
C22'0.016 (2)0.017 (2)0.045 (3)0.0026 (18)0.0114 (19)0.0100 (19)
C23'0.017 (2)0.013 (2)0.065 (3)0.0011 (17)0.018 (2)0.008 (2)
C24'0.023 (2)0.026 (3)0.039 (3)0.005 (2)0.018 (2)0.014 (2)
C25'0.026 (2)0.042 (3)0.018 (2)0.007 (2)0.0049 (18)0.005 (2)
C26'0.015 (2)0.027 (2)0.023 (2)0.0022 (19)0.0023 (18)0.0000 (18)
C27'0.0056 (19)0.0045 (19)0.027 (2)0.0030 (16)0.0030 (16)0.0027 (16)
C28'0.013 (2)0.008 (2)0.015 (2)0.0012 (16)0.0029 (16)0.0037 (15)
C29'0.013 (2)0.018 (2)0.017 (2)0.0044 (17)0.0029 (16)0.0016 (16)
C30'0.030 (2)0.032 (3)0.021 (2)0.009 (2)0.0073 (19)0.0013 (19)
Geometric parameters (Å, º) top
Ru1—C272.050 (4)Ru1'—C27'2.060 (4)
Ru1—C27i2.050 (4)Ru1'—C27'ii2.060 (4)
Ru1—P22.3581 (9)Ru1'—P1'2.3592 (9)
Ru1—P2i2.3581 (9)Ru1'—P1'ii2.3592 (9)
Ru1—P1i2.3793 (9)Ru1'—P2'2.3751 (9)
Ru1—P12.3793 (9)Ru1'—P2'ii2.3751 (9)
P1—C71.829 (4)P1'—C1'1.830 (4)
P1—C11.837 (4)P1'—C13'1.844 (4)
P1—C131.857 (4)P1'—C7'1.845 (4)
P2—C211.830 (4)P2'—C15'1.836 (4)
P2—C151.837 (4)P2'—C21'1.837 (4)
P2—C141.837 (4)P2'—C14'1.862 (4)
C1—C61.394 (5)C1'—C6'1.390 (5)
C1—C21.398 (5)C1'—C2'1.397 (6)
C2—C31.386 (5)C2'—C3'1.383 (6)
C2—H20.95C2'—H2'0.95
C3—C41.370 (6)C3'—C4'1.377 (6)
C3—H30.95C3'—H3'0.95
C4—C51.385 (6)C4'—C5'1.381 (6)
C4—H40.95C4'—H4'0.95
C5—C61.389 (6)C5'—C6'1.382 (6)
C5—H50.95C5'—H5'0.95
C6—H60.95C6'—H6'0.95
C7—C121.394 (5)C7'—C8'1.383 (6)
C7—C81.394 (5)C7'—C12'1.396 (6)
C8—C91.389 (5)C8'—C9'1.389 (5)
C8—H80.95C8'—H8'0.95
C9—C101.383 (6)C9'—C10'1.381 (7)
C9—H90.95C9'—H9'0.95
C10—C111.370 (6)C10'—C11'1.376 (7)
C10—H100.95C10'—H10'0.95
C11—C121.391 (6)C11'—C12'1.388 (6)
C11—H110.95C11'—H11'0.95
C12—H120.95C12'—H12'0.95
C13—C141.532 (5)C13'—C14'1.513 (5)
C13—H13A0.99C13'—H13C0.99
C13—H13B0.99C13'—H13D0.99
C14—H14A0.99C14'—H14C0.99
C14—H14B0.99C14'—H14D0.99
C15—C161.394 (5)C15'—C20'1.387 (5)
C15—C201.400 (5)C15'—C16'1.403 (5)
C16—C171.388 (5)C16'—C17'1.388 (5)
C16—H160.95C16'—H16'0.95
C17—C181.380 (6)C17'—C18'1.386 (6)
C17—H170.95C17'—H17'0.95
C18—C191.375 (6)C18'—C19'1.385 (6)
C18—H180.95C18'—H18'0.95
C19—C201.403 (5)C19'—C20'1.385 (5)
C19—H190.95C19'—H19'0.95
C20—H200.95C20'—H20'0.95
C21—C221.401 (5)C21'—C26'1.378 (6)
C21—C261.402 (6)C21'—C22'1.408 (5)
C22—C231.382 (5)C22'—C23'1.388 (6)
C22—H220.95C22'—H22'0.95
C23—C241.378 (6)C23'—C24'1.381 (6)
C23—H230.95C23'—H23'0.95
C24—C251.384 (6)C24'—C25'1.377 (6)
C24—H240.95C24'—H24'0.95
C25—C261.392 (6)C25'—C26'1.382 (6)
C25—H250.95C25'—H25'0.95
C26—H260.95C26'—H26'0.95
C27—C281.198 (5)C27'—C28'1.189 (5)
C28—C291.396 (6)C28'—C29'1.391 (6)
C29—C301.193 (6)C29'—C30'1.198 (6)
C30—H300.95C30'—H30'0.95
C27—Ru1—C27i180.0 (2)C27'—Ru1'—C27'ii180.0000 (10)
C27—Ru1—P294.07 (10)C27'—Ru1'—P1'94.28 (10)
C27i—Ru1—P285.93 (10)C27'ii—Ru1'—P1'85.72 (10)
C27—Ru1—P2i85.93 (10)C27'—Ru1'—P1'ii85.72 (10)
C27i—Ru1—P2i94.07 (10)C27'ii—Ru1'—P1'ii94.28 (10)
P2—Ru1—P2i180.00 (4)P1'—Ru1'—P1'ii180.00 (4)
C27—Ru1—P1i83.91 (10)C27'—Ru1'—P2'95.99 (10)
C27i—Ru1—P1i96.09 (10)C27'ii—Ru1'—P2'84.01 (10)
P2—Ru1—P1i97.15 (3)P1'—Ru1'—P2'82.26 (3)
P2i—Ru1—P1i82.85 (3)P1'ii—Ru1'—P2'97.74 (3)
C27—Ru1—P196.09 (10)C27'—Ru1'—P2'ii84.01 (10)
C27i—Ru1—P183.91 (10)C27'ii—Ru1'—P2'ii95.99 (10)
P2—Ru1—P182.85 (3)P1'—Ru1'—P2'ii97.74 (3)
P2i—Ru1—P197.15 (3)P1'ii—Ru1'—P2'ii82.26 (3)
P1i—Ru1—P1180.00 (9)P2'—Ru1'—P2'ii180
C7—P1—C1101.70 (17)C1'—P1'—C13'104.74 (17)
C7—P1—C13105.05 (17)C1'—P1'—C7'101.59 (17)
C1—P1—C1398.85 (17)C13'—P1'—C7'101.13 (17)
C7—P1—Ru1115.25 (13)C1'—P1'—Ru1'119.06 (12)
C1—P1—Ru1125.18 (13)C13'—P1'—Ru1'105.31 (12)
C13—P1—Ru1108.19 (11)C7'—P1'—Ru1'122.44 (13)
C21—P2—C15101.27 (17)C15'—P2'—C21'99.98 (17)
C21—P2—C14104.72 (17)C15'—P2'—C14'104.38 (17)
C15—P2—C14101.36 (16)C21'—P2'—C14'98.85 (18)
C21—P2—Ru1120.50 (12)C15'—P2'—Ru1'115.43 (12)
C15—P2—Ru1121.52 (13)C21'—P2'—Ru1'126.50 (13)
C14—P2—Ru1104.85 (12)C14'—P2'—Ru1'108.74 (12)
C6—C1—C2117.3 (3)C6'—C1'—C2'118.5 (3)
C6—C1—P1123.1 (3)C6'—C1'—P1'119.4 (3)
C2—C1—P1119.4 (3)C2'—C1'—P1'122.0 (3)
C3—C2—C1121.3 (4)C3'—C2'—C1'120.6 (4)
C3—C2—H2119.4C3'—C2'—H2'119.7
C1—C2—H2119.4C1'—C2'—H2'119.7
C4—C3—C2120.1 (4)C4'—C3'—C2'120.4 (4)
C4—C3—H3119.9C4'—C3'—H3'119.8
C2—C3—H3119.9C2'—C3'—H3'119.8
C3—C4—C5120.2 (4)C3'—C4'—C5'119.5 (4)
C3—C4—H4119.9C3'—C4'—H4'120.3
C5—C4—H4119.9C5'—C4'—H4'120.3
C4—C5—C6119.4 (4)C4'—C5'—C6'120.7 (4)
C4—C5—H5120.3C4'—C5'—H5'119.7
C6—C5—H5120.3C6'—C5'—H5'119.7
C5—C6—C1121.6 (4)C5'—C6'—C1'120.4 (4)
C5—C6—H6119.2C5'—C6'—H6'119.8
C1—C6—H6119.2C1'—C6'—H6'119.8
C12—C7—C8118.0 (4)C8'—C7'—C12'118.9 (3)
C12—C7—P1121.7 (3)C8'—C7'—P1'122.5 (3)
C8—C7—P1120.2 (3)C12'—C7'—P1'118.5 (3)
C9—C8—C7121.4 (4)C7'—C8'—C9'120.6 (4)
C9—C8—H8119.3C7'—C8'—H8'119.7
C7—C8—H8119.3C9'—C8'—H8'119.7
C10—C9—C8119.7 (4)C10'—C9'—C8'120.2 (4)
C10—C9—H9120.2C10'—C9'—H9'119.9
C8—C9—H9120.2C8'—C9'—H9'119.9
C11—C10—C9119.7 (4)C11'—C10'—C9'119.6 (4)
C11—C10—H10120.2C11'—C10'—H10'120.2
C9—C10—H10120.2C9'—C10'—H10'120.2
C10—C11—C12121.0 (4)C10'—C11'—C12'120.6 (4)
C10—C11—H11119.5C10'—C11'—H11'119.7
C12—C11—H11119.5C12'—C11'—H11'119.7
C11—C12—C7120.3 (4)C11'—C12'—C7'120.0 (4)
C11—C12—H12119.9C11'—C12'—H12'120
C7—C12—H12119.9C7'—C12'—H12'120
C14—C13—P1112.4 (3)C14'—C13'—P1'109.5 (2)
C14—C13—H13A109.1C14'—C13'—H13C109.8
P1—C13—H13A109.1P1'—C13'—H13C109.8
C14—C13—H13B109.1C14'—C13'—H13D109.8
P1—C13—H13B109.1P1'—C13'—H13D109.8
H13A—C13—H13B107.9H13C—C13'—H13D108.2
C13—C14—P2109.1 (2)C13'—C14'—P2'112.7 (3)
C13—C14—H14A109.9C13'—C14'—H14C109
P2—C14—H14A109.9P2'—C14'—H14C109
C13—C14—H14B109.9C13'—C14'—H14D109
P2—C14—H14B109.9P2'—C14'—H14D109
H14A—C14—H14B108.3H14C—C14'—H14D107.8
C16—C15—C20118.3 (3)C20'—C15'—C16'118.8 (4)
C16—C15—P2119.2 (3)C20'—C15'—P2'119.7 (3)
C20—C15—P2122.5 (3)C16'—C15'—P2'121.3 (3)
C17—C16—C15121.3 (4)C17'—C16'—C15'120.3 (4)
C17—C16—H16119.4C17'—C16'—H16'119.9
C15—C16—H16119.4C15'—C16'—H16'119.9
C18—C17—C16120.0 (4)C18'—C17'—C16'120.0 (4)
C18—C17—H17120C18'—C17'—H17'120
C16—C17—H17120C16'—C17'—H17'120
C19—C18—C17119.9 (4)C19'—C18'—C17'120.0 (4)
C19—C18—H18120C19'—C18'—H18'120
C17—C18—H18120C17'—C18'—H18'120
C18—C19—C20120.6 (4)C18'—C19'—C20'120.0 (4)
C18—C19—H19119.7C18'—C19'—H19'120
C20—C19—H19119.7C20'—C19'—H19'120
C15—C20—C19119.9 (4)C19'—C20'—C15'120.9 (4)
C15—C20—H20120.1C19'—C20'—H20'119.6
C19—C20—H20120.1C15'—C20'—H20'119.6
C22—C21—C26118.3 (3)C26'—C21'—C22'118.1 (4)
C22—C21—P2119.0 (3)C26'—C21'—P2'122.6 (3)
C26—C21—P2122.5 (3)C22'—C21'—P2'119.1 (3)
C23—C22—C21120.6 (4)C23'—C22'—C21'120.3 (4)
C23—C22—H22119.7C23'—C22'—H22'119.9
C21—C22—H22119.7C21'—C22'—H22'119.9
C24—C23—C22120.5 (4)C24'—C23'—C22'120.2 (4)
C24—C23—H23119.8C24'—C23'—H23'119.9
C22—C23—H23119.8C22'—C23'—H23'119.9
C23—C24—C25120.1 (4)C25'—C24'—C23'119.6 (4)
C23—C24—H24120C25'—C24'—H24'120.2
C25—C24—H24120C23'—C24'—H24'120.2
C24—C25—C26120.0 (4)C24'—C25'—C26'120.4 (4)
C24—C25—H25120C24'—C25'—H25'119.8
C26—C25—H25120C26'—C25'—H25'119.8
C25—C26—C21120.5 (4)C21'—C26'—C25'121.3 (4)
C25—C26—H26119.8C21'—C26'—H26'119.3
C21—C26—H26119.8C25'—C26'—H26'119.3
C28—C27—Ru1178.4 (3)C28'—C27'—Ru1'177.1 (3)
C27—C28—C29171.6 (4)C27'—C28'—C29'173.6 (4)
C30—C29—C28175.9 (5)C30'—C29'—C28'177.5 (4)
C29—C30—H30180C29'—C30'—H30'180
Symmetry codes: (i) x, y, z; (ii) x+1, y, z+1.

Experimental details

(I)(II)
Crystal data
Chemical formula[Ru(C7H9Si)2(C26H24P2)2][Ru(C4H)2(C26H24P2)2]
Mr1140.32995.95
Crystal system, space groupTriclinic, P1Triclinic, P1
Temperature (K)150120
a, b, c (Å)12.677 (3), 16.058 (3), 16.085 (3)11.9017 (2), 13.2669 (3), 17.1934 (4)
α, β, γ (°)110.32 (3), 93.16 (3), 96.36 (3)79.416 (1), 76.195 (1), 64.499 (2)
V3)3036.3 (13)2369.38 (9)
Z22
Radiation typeMo KαMo Kα
µ (mm1)0.440.51
Crystal size (mm)0.2 × 0.08 × 0.050.15 × 0.1 × 0.06
Data collection
DiffractometerBruker-Nonius KappaCCD area detectorBruker-Nonius KappaCCD area-detector
Absorption correctionMulti-scan
(SORTAV; Blessing, 1995)
Multi-scan
(SORTAV; Blessing, 1995)
Tmin, Tmax0.767, 0.9860.780, 0.872
No. of measured, independent and
observed [I > 2σ(I)] reflections
42685, 13576, 9761 26880, 7995, 4873
Rint0.0960.073
(sin θ/λ)max1)0.6490.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.122, 1.03 0.038, 0.091, 0.94
No. of reflections135767995
No. of parameters665589
No. of restraints180
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.76, 0.810.60, 0.54

Computer programs: DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998), COLLECT (Hooft, 1998), DENZO (Otwinowski and Minor, 1997), DENZO, COLLECT(Otwinowski and Minor, 1997; Hooft, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), CAMERON (Watkin, et al., 1993), WinGX (Farrugia, 1998).

Selected geometric parameters (Å, º) for (I) top
C53—C541.179 (17)C61—C621.444 (18)
C53—Ru12.041 (13)C62—C631.221 (17)
C54—C551.395 (18)P1—Ru12.352 (3)
C55—C561.217 (19)P2—Ru12.356 (3)
C60—C611.099 (17)P3—Ru12.362 (3)
C60—Ru12.095 (14)P4—Ru12.373 (3)
C54—C53—Ru1177.3 (11)C60—C61—C62170.7 (13)
C53—C54—C55175.3 (14)C63—C62—C61178.9 (15)
C56—C55—C54177.8 (15)C53—Ru1—C60174.2 (4)
C61—C60—Ru1177.0 (11)
Selected geometric parameters (Å, º) for (II) top
Ru1—C272.050 (4)C27—C281.198 (5)
Ru1—P22.3581 (9)C28—C291.396 (6)
Ru1—P12.3793 (9)C29—C301.193 (6)
C27—Ru1—C27i180.0 (2)C27—C28—C29171.6 (4)
C28—C27—Ru1178.4 (3)C30—C29—C28175.9 (5)
Symmetry code: (i) x, y, z.
 

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