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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 1| January 2011| Page m14
https://doi.org/10.1107/S1600536810049706

cis-Di­chlorido­tetra­kis­(tri­methyl­phosphane-κP)ruthenium(II) benzene disolvate

Chen Fua and Ting Bin Wena*

aDepartment of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, Fujian, People's Republic of China
*Correspondence e-mail: chwtb@xmu.edu.cn

(Received 19 November 2010; accepted 28 November 2010; online 4 December 2010)

The title compound, cis-[RuCl2(C3H9P)4]·2C6H6, contains a complex mol­ecule with a crystallographic mirror plane passing through the RuII atom, the two cis-disposed Cl ligands and two P atoms of the two cis-disposed P(CH3)3 ligands. The RuII atom adopts a distorted octa­hedral RuCl2P4 coordination geometry with the two trans-disposed P atoms occupying the axial positions. The packing of the structure is accomplished through non-classical C—H⋯Cl hydrogen bonds between the benzene solvent mol­ecule and one of the Cl ligands.

Related literature

For general background to trans-[RuCl2(P(CH3)3)4], see: Csok et al. (2007[Csok, Z., Gandum, C., Rissanen, K., Tuzi, A. & Rodrigues, J. (2007). J. Organomet. Chem. 692, 5263-5271.]); Gotzig et al. (1985[Gotzig, J., Werner, R. & Werner, H. (1985). J. Organomet. Chem. 290, 99-114.]); Hartwig et al. (1991[Hartwig, J. F., Bergman, R. G. & Andersen, R. A. (1991). Organometallics, 10, 3344-3362.]); Hirano et al. (2010[Hirano, M., Togashi, S., Ito, M., Sakaguchi, Y., Komine, N. & Komiya, S. (2010). Organometallics, 29, 3146-3159.]); Kohlmann & Werner (1993[Kohlmann, W. & Werner, H. (1993). Z. Naturforsch. Teil B, 48, 1499-1511.]). For a related structure, see: Joo et al. (1994[Joo, F., Kannisto, M., Katho, A., Reibenspies, J., Daigle, D. & Darensbourg, D. (1994). Inorg. Chem. 33, 200-208.]).

[Scheme 1]

Experimental

Crystal data

  • [RuCl2(C3H9P)4]·2C6H6

  • Mr = 632.47

  • Orthorhombic, P n m a

  • a = 17.6243 (15) Å

  • b = 18.1889 (19) Å

  • c = 9.4610 (11) Å

  • V = 3032.9 (5) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 0.92 mm−1

  • T = 173 K

  • 0.18 × 0.12 × 0.06 mm
Data collection

  • Oxford Diffraction Gemini S Ultra diffractometer

  • Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]) Tmin = 0.949, Tmax = 1.000

  • 14352 measured reflections

  • 3550 independent reflections

  • 1653 reflections with I > 2σ(I)

  • Rint = 0.148
Refinement

  • R[F2 > 2σ(F2)] = 0.058

  • wR(F2) = 0.081

  • S = 0.82

  • 3550 reflections

  • 139 parameters

  • H-atom parameters constrained

  • Δρmax = 0.97 e Å−3

  • Δρmin = −0.57 e Å−3

Table 1
Selected bond lengths (Å)

Ru1—P1 2.2690 (19)
Ru1—P2 2.297 (2)
Ru1—P3 2.3819 (14)
Ru1—Cl1 2.479 (2)
Ru1—Cl2 2.5038 (19)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
C4S—H4SA⋯Cl2 0.93 2.83 3.710 (5) 159

Data collection: CrysAlis CCD (Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]); cell refinement: CrysAlis RED (Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810049706/wm2431sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810049706/wm2431Isup2.hkl

checkCIF report


Comment top

The ruthenium(II) complex trans-[RuCl2(PMe3)4], which can be readily prepared from the reaction of RuCl2(PPh3)3 with PMe3 in hexane at room temperature (Gotzig et al., 1985), has proved to be a useful precursor for a wide variety of ruthenium compounds (Hartwig et al., 1991; Kohlmann & Werner, 1993; Csok et al., 2007; Hirano et al., 2010). However, its geometrical isomer, cis-[RuCl2(PMe3)4], has not been reported yet. During our preparation of ruthenium compounds with phosphine ligands using trans-[RuCl2(PMe3)4] as the starting material, we found that the trans-isomer slowly isomerizes to the cis-isomer, the structure of which we report here as the benzene disolvate.

As shown in Fig.1, the structure of the title complex possesses a crystallographic mirror plane passing through the RuII atom, the two cis-disposed Cl ligands and the two P atoms as well as two C atoms of the two cis-disposed PMe3 ligands. Thus the asymmetric unit of the structure contains half of a molecule. The RuII atom adopts a distorted octahedral geometry with the two trans-disposed P atoms occupying the axial positions. The bond lengths of the two axial Ru—P bonds (2.3819 (14) Å), which are actually image-related, are slightly longer than those of the two equatorial Ru—P bonds which are trans to the Cl ligands (2.2690 (19) and 2.297 (2) Å, respectively). The two Ru—Cl bond lengths are 2.479 (2) and 2.5038 (19) Å, respectively, while the Cl(1)—Ru(1)—Cl(2) bond angle is 86.20 (7)°. These geometric values are similar to those reported for the only example of a sructurally characterized monodentate tetrakis(phosphine)-cis-dichlorido-ruthenium(II) complex, viz. [cis-RuCl2(PTA)4] (PTA = 1,3,5-triaza-7-phospha-adamantane-κP); 2.488 (2) and 2.503 (2) Å, 84.2 (1) °; Joo et al., 1994).

The packing of the structure (Fig. 2) is accomplished through non-classical C—H···Cl hydrogen bonds between the benzene solvent molecule and one of the Cl ligands (Table 2).

Related literature top

For general background to trans-[RuCl2(P(CH3)3)4], see: Csok et al. (2007); Gotzig et al. (1985); Hartwig et al. (1991); Hirano et al. (2010); Kohlmann & Werner (1993). For a related structure, see: Joo et al. (1994).

Experimental top

Route A: To a solution of RuCl2(PPh3)3 (0.25 g, 0.24 mmol) in toluene (8 ml) under nitrogen atmosphere was added PMe3 (0.27 ml, 2.5 mmol) and the resulting yellow solution was refluxed for 20 h. The solvent was removed under vacuum, and the solid residue was washed with n-hexane, and dried under vacuum to afford a white solid. Yield: 90 mg, 80%. Route B: A solution of trans-[RuCl2(PMe3)4] (100 mg, 0.21 mmol) in benzene (5 ml) was refluxed for 12 h under nitrogen atmosphere. After the solution was cooled to ambient temperature, a white solid was precipitated, which was collected by filtration, washed with n-hexane, and dried under vacuum. Yield: 72 mg, 72%. Crystals suitable for X-ray analysis were obtained from standing a solution of trans-[RuCl2(PMe3)4] in benzene at room temperature for 2 weeks.

Refinement top

The benzene solvent molecule was treated as a rigid body. All non-hydrogen atoms were refined anisotropically. The hydrogen atoms were positioned geometrically (C—H = 0.96 or 0.93 Å for methyl or phenyl H atoms, respectively) and were included in the refinement in the riding model approximation. The displacement parameters of methyl H atoms were set to 1.5Ueq(C), while those of the phenyl H atoms were set to 1.2Ueq(C). In the final Fourier map the highest peak is 0.04 Å from atom Ru1 and the deepest hole is 0.71 Å from atom Ru1.

Structure description top

The ruthenium(II) complex trans-[RuCl2(PMe3)4], which can be readily prepared from the reaction of RuCl2(PPh3)3 with PMe3 in hexane at room temperature (Gotzig et al., 1985), has proved to be a useful precursor for a wide variety of ruthenium compounds (Hartwig et al., 1991; Kohlmann & Werner, 1993; Csok et al., 2007; Hirano et al., 2010). However, its geometrical isomer, cis-[RuCl2(PMe3)4], has not been reported yet. During our preparation of ruthenium compounds with phosphine ligands using trans-[RuCl2(PMe3)4] as the starting material, we found that the trans-isomer slowly isomerizes to the cis-isomer, the structure of which we report here as the benzene disolvate.

As shown in Fig.1, the structure of the title complex possesses a crystallographic mirror plane passing through the RuII atom, the two cis-disposed Cl ligands and the two P atoms as well as two C atoms of the two cis-disposed PMe3 ligands. Thus the asymmetric unit of the structure contains half of a molecule. The RuII atom adopts a distorted octahedral geometry with the two trans-disposed P atoms occupying the axial positions. The bond lengths of the two axial Ru—P bonds (2.3819 (14) Å), which are actually image-related, are slightly longer than those of the two equatorial Ru—P bonds which are trans to the Cl ligands (2.2690 (19) and 2.297 (2) Å, respectively). The two Ru—Cl bond lengths are 2.479 (2) and 2.5038 (19) Å, respectively, while the Cl(1)—Ru(1)—Cl(2) bond angle is 86.20 (7)°. These geometric values are similar to those reported for the only example of a sructurally characterized monodentate tetrakis(phosphine)-cis-dichlorido-ruthenium(II) complex, viz. [cis-RuCl2(PTA)4] (PTA = 1,3,5-triaza-7-phospha-adamantane-κP); 2.488 (2) and 2.503 (2) Å, 84.2 (1) °; Joo et al., 1994).

The packing of the structure (Fig. 2) is accomplished through non-classical C—H···Cl hydrogen bonds between the benzene solvent molecule and one of the Cl ligands (Table 2).

For general background to trans-[RuCl2(P(CH3)3)4], see: Csok et al. (2007); Gotzig et al. (1985); Hartwig et al. (1991); Hirano et al. (2010); Kohlmann & Werner (1993). For a related structure, see: Joo et al. (1994).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2008); cell refinement: CrysAlis RED (Oxford Diffraction, 2008); data reduction: CrysAlis RED (Oxford Diffraction, 2008); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The coordination of the RuII atom in the structure of cis-[RuCl2(P(CH3)3)4] with the atom labelling and displacement ellipsoids drawn at the 30% probability level. H atoms have been omitted for clarity. [Symmetry code: (A) x, -y+1/2, z.]
[Figure 2] Fig. 2. The packing diagram of the structure viewed down the c axis, showing the non-classical C—H···Cl hydrogen bonds between the benzene solvent molecule and one of the Cl ligands of the complex molecule.
cis-Dichloridotetrakis(trimethylphosphane-κP)ruthenium(II) benzene disolvate top
Crystal data top
[RuCl2(C3H9P)4]·2C6H6F(000) = 1320
Mr = 632.47Dx = 1.385 Mg m−3
Orthorhombic, PnmaMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ac 2nCell parameters from 1376 reflections
a = 17.6243 (15) Åθ = 2.3–28.9°
b = 18.1889 (19) ŵ = 0.92 mm−1
c = 9.4610 (11) ÅT = 173 K
V = 3032.9 (5) Å3Block, colorless
Z = 40.18 × 0.12 × 0.06 mm
Data collection top
Oxford Diffraction Gemini S Ultra
diffractometer		3550 independent reflections
Radiation source: Enhance (Mo) X-ray Source1653 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.148
Detector resolution: 16.1930 pixels mm-1θmax = 27.5°, θmin = 2.3°
ω scansh = −22→21
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2008)		k = −23→22
Tmin = 0.949, Tmax = 1.000l = −10→12
14352 measured reflections
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)] = 0.058Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H-atom parameters constrained
S = 0.82 w = 1/[σ2(Fo2) + (0.0104P)2]
where P = (Fo2 + 2Fc2)/3
3550 reflections(Δ/σ)max = 0.003
139 parametersΔρmax = 0.97 e Å−3
0 restraintsΔρmin = −0.57 e Å−3
Crystal data top
[RuCl2(C3H9P)4]·2C6H6V = 3032.9 (5) Å3
Mr = 632.47Z = 4
Orthorhombic, PnmaMo Kα radiation
a = 17.6243 (15) ŵ = 0.92 mm−1
b = 18.1889 (19) ÅT = 173 K
c = 9.4610 (11) Å0.18 × 0.12 × 0.06 mm
Data collection top
Oxford Diffraction Gemini S Ultra
diffractometer		3550 independent reflections
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2008)		1653 reflections with I > 2σ(I)
Tmin = 0.949, Tmax = 1.000Rint = 0.148
14352 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0580 restraints
wR(F2) = 0.081H-atom parameters constrained
S = 0.82Δρmax = 0.97 e Å−3
3550 reflectionsΔρmin = −0.57 e Å−3
139 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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ru10.54358 (3)0.25000.30360 (7)0.01803 (17)
Cl10.47805 (10)0.25000.0718 (2)0.0308 (6)
Cl20.41377 (9)0.25000.4111 (2)0.0347 (6)
P10.66211 (10)0.25000.2100 (2)0.0221 (5)
P20.57932 (10)0.25000.5371 (2)0.0233 (6)
P30.53321 (8)0.37973 (7)0.27518 (17)0.0273 (4)
C110.6660 (4)0.25000.0209 (8)0.032 (2)
H11A0.71780.2500−0.01040.049*
H11B0.64080.2069−0.01420.049*
C120.7266 (2)0.3256 (2)0.2488 (6)0.0303 (17)
H12A0.77400.31750.20150.045*
H12B0.73500.32820.34890.045*
H12C0.70470.37090.21650.045*
C210.6769 (3)0.25000.5976 (8)0.036 (2)
H21A0.67850.25000.69900.055*
H21B0.70200.20690.56230.055*
C220.5445 (3)0.3255 (3)0.6447 (6)0.057 (2)
H22A0.56270.32000.73970.086*
H22B0.49000.32520.64470.086*
H22C0.56240.37130.60650.086*
C310.5557 (3)0.4150 (3)0.1015 (6)0.0368 (16)
H31A0.54990.46750.10100.055*
H31B0.52210.39360.03310.055*
H31C0.60720.40270.07810.055*
C320.4370 (2)0.4140 (3)0.2916 (7)0.0447 (18)
H32A0.43690.46640.27890.067*
H32B0.41770.40230.38370.067*
H32C0.40560.39160.22080.067*
C330.5837 (3)0.4488 (3)0.3798 (6)0.046 (2)
H33A0.57000.49710.34760.069*
H33B0.63740.44200.36900.069*
H33C0.57030.44360.47760.069*
C1S0.2535 (3)0.4577 (2)0.8727 (8)0.069 (3)
H1SA0.22730.49190.92730.082*
C2S0.3127 (4)0.4177 (4)0.9316 (4)0.073 (3)
H2SA0.32630.42511.02550.088*
C3S0.3518 (2)0.3667 (3)0.8500 (8)0.068 (3)
H3SA0.39150.33990.88940.081*
C4S0.3316 (3)0.3557 (2)0.7096 (8)0.059 (2)
H4SA0.35780.32150.65500.071*
C5S0.2724 (3)0.3957 (3)0.6507 (4)0.059 (2)
H5SA0.25890.38830.55670.071*
C6S0.23327 (19)0.4467 (3)0.7323 (8)0.064 (3)
H6SA0.19360.47350.69290.076*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0145 (3)0.0200 (3)0.0196 (4)0.000−0.0017 (4)0.000
Cl10.0333 (12)0.0318 (13)0.0275 (14)0.000−0.0146 (10)0.000
Cl20.0154 (11)0.0489 (14)0.0398 (15)0.000−0.0001 (10)0.000
P10.0212 (10)0.0254 (12)0.0197 (14)0.0000.0015 (11)0.000
P20.0181 (11)0.0330 (14)0.0187 (14)0.0000.0012 (10)0.000
P30.0230 (8)0.0249 (8)0.0339 (11)0.0015 (7)−0.0029 (8)−0.0031 (8)
C110.029 (5)0.036 (6)0.032 (6)0.0000.012 (4)0.000
C120.026 (3)0.029 (3)0.036 (5)0.002 (3)0.003 (3)0.000 (3)
C210.023 (5)0.073 (7)0.013 (5)0.000−0.004 (4)0.000
C220.059 (4)0.081 (5)0.032 (4)0.027 (4)−0.006 (4)−0.018 (4)
C310.048 (4)0.027 (3)0.035 (4)−0.003 (3)−0.002 (3)0.008 (3)
C320.039 (4)0.031 (3)0.064 (5)0.009 (3)−0.008 (4)−0.001 (4)
C330.039 (4)0.033 (4)0.066 (6)−0.007 (3)0.003 (3)−0.013 (4)
C1S0.085 (6)0.053 (6)0.067 (7)−0.029 (5)0.050 (5)−0.019 (6)
C2S0.099 (7)0.091 (8)0.029 (5)−0.066 (5)−0.019 (5)0.026 (6)
C3S0.039 (4)0.063 (6)0.101 (9)−0.009 (4)−0.006 (5)0.041 (6)
C4S0.056 (5)0.026 (4)0.097 (8)−0.004 (3)0.049 (5)−0.009 (5)
C5S0.087 (6)0.059 (6)0.033 (5)−0.050 (4)−0.003 (5)0.007 (5)
C6S0.035 (4)0.037 (5)0.119 (10)−0.007 (3)0.010 (5)0.029 (6)
Geometric parameters (Å, º) top
Ru1—P12.2690 (19)C22—H22B0.9600
Ru1—P22.297 (2)C22—H22C0.9600
Ru1—P3i2.3819 (14)C31—H31A0.9600
Ru1—P32.3819 (14)C31—H31B0.9600
Ru1—Cl12.479 (2)C31—H31C0.9600
Ru1—Cl22.5038 (19)C32—H32A0.9600
P1—C111.790 (8)C32—H32B0.9600
P1—C121.821 (4)C32—H32C0.9600
P1—C12i1.821 (4)C33—H33A0.9600
P2—C211.812 (6)C33—H33B0.9600
P2—C221.816 (5)C33—H33C0.9600
P2—C22i1.816 (5)C1S—C2S1.3900
P3—C311.808 (5)C1S—C6S1.3900
P3—C321.813 (4)C1S—H1SA0.9300
P3—C331.831 (5)C2S—C3S1.3900
C11—H11A0.9600C2S—H2SA0.9300
C11—H11B0.9598C3S—C4S1.3900
C12—H12A0.9600C3S—H3SA0.9300
C12—H12B0.9600C4S—C5S1.3900
C12—H12C0.9600C4S—H4SA0.9300
C21—H21A0.9600C5S—C6S1.3900
C21—H21B0.9599C5S—H5SA0.9300
C22—H22A0.9600C6S—H6SA0.9300
P1—Ru1—P297.07 (8)H21A—C21—H21B109.5
P1—Ru1—P3i91.52 (4)P2—C22—H22A109.5
P2—Ru1—P3i97.45 (4)P2—C22—H22B109.5
P1—Ru1—P391.52 (4)H22A—C22—H22B109.5
P2—Ru1—P397.45 (4)P2—C22—H22C109.5
P3i—Ru1—P3164.31 (8)H22A—C22—H22C109.5
P1—Ru1—Cl194.79 (8)H22B—C22—H22C109.5
P2—Ru1—Cl1168.14 (7)P3—C31—H31A109.5
P3i—Ru1—Cl182.20 (4)P3—C31—H31B109.5
P3—Ru1—Cl182.20 (4)H31A—C31—H31B109.5
P1—Ru1—Cl2179.01 (9)P3—C31—H31C109.5
P2—Ru1—Cl281.94 (7)H31A—C31—H31C109.5
P3i—Ru1—Cl288.61 (4)H31B—C31—H31C109.5
P3—Ru1—Cl288.61 (4)P3—C32—H32A109.5
Cl1—Ru1—Cl286.20 (7)P3—C32—H32B109.5
C11—P1—C12100.2 (2)H32A—C32—H32B109.5
C11—P1—C12i100.2 (2)P3—C32—H32C109.5
C12—P1—C12i98.0 (3)H32A—C32—H32C109.5
C11—P1—Ru1115.2 (2)H32B—C32—H32C109.5
C12—P1—Ru1119.71 (17)P3—C33—H33A109.5
C12i—P1—Ru1119.71 (17)P3—C33—H33B109.5
C21—P2—C2298.3 (2)H33A—C33—H33B109.5
C21—P2—C22i98.3 (2)P3—C33—H33C109.5
C22—P2—C22i98.3 (4)H33A—C33—H33C109.5
C21—P2—Ru1124.3 (3)H33B—C33—H33C109.5
C22—P2—Ru1116.5 (2)C2S—C1S—C6S120.0
C22i—P2—Ru1116.5 (2)C2S—C1S—H1SA120.0
C31—P3—C3299.3 (3)C6S—C1S—H1SA120.0
C31—P3—C3398.1 (3)C3S—C2S—C1S120.0
C32—P3—C3399.9 (2)C3S—C2S—H2SA120.0
C31—P3—Ru1115.93 (18)C1S—C2S—H2SA120.0
C32—P3—Ru1113.76 (17)C2S—C3S—C4S120.0
C33—P3—Ru1125.57 (19)C2S—C3S—H3SA120.0
P1—C11—H11A110.1C4S—C3S—H3SA120.0
P1—C11—H11B109.1C3S—C4S—C5S120.0
H11A—C11—H11B109.5C3S—C4S—H4SA120.0
P1—C12—H12A109.5C5S—C4S—H4SA120.0
P1—C12—H12B109.5C6S—C5S—C4S120.0
H12A—C12—H12B109.5C6S—C5S—H5SA120.0
P1—C12—H12C109.5C4S—C5S—H5SA120.0
H12A—C12—H12C109.5C5S—C6S—C1S120.0
H12B—C12—H12C109.5C5S—C6S—H6SA120.0
P2—C21—H21A110.1C1S—C6S—H6SA120.0
P2—C21—H21B109.1
Symmetry code: (i) x, −y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C4S—H4SA···Cl20.932.833.710 (5)159

Experimental details

Crystal data
Chemical formula[RuCl2(C3H9P)4]·2C6H6
Mr632.47
Crystal system, space groupOrthorhombic, Pnma
Temperature (K)173
a, b, c (Å)17.6243 (15), 18.1889 (19), 9.4610 (11)
V (Å3)3032.9 (5)
Z4
Radiation typeMo Kα
µ (mm−1)0.92
Crystal size (mm)0.18 × 0.12 × 0.06
Data collection
DiffractometerOxford Diffraction Gemini S Ultra
Absorption correctionMulti-scan
(CrysAlis RED; Oxford Diffraction, 2008)
Tmin, Tmax0.949, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections		14352, 3550, 1653
Rint0.148
(sin θ/λ)max (Å−1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.058, 0.081, 0.82
No. of reflections3550
No. of parameters139
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.97, −0.57

Computer programs: CrysAlis CCD (Oxford Diffraction, 2008), CrysAlis RED (Oxford Diffraction, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Ru1—P12.2690 (19)Ru1—Cl12.479 (2)
Ru1—P22.297 (2)Ru1—Cl22.5038 (19)
Ru1—P32.3819 (14)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C4S—H4SA···Cl20.932.833.710 (5)159.0
 

Acknowledgements

The authors acknowledge financial support from the Young Talent Project of Department of Science & Technology of Fujian Province (grant No. 2007 F3095).

References

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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

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ISSN: 2056-9890
Volume 67| Part 1| January 2011| Page m14
https://doi.org/10.1107/S1600536810049706
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