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The title syn isomer of [Ru2(μ-SPh)2(PPh3)2(CO)4] or [Ru2(μ-C6H5S)2(C18H15P)2(CO)4], which was previously expected to be present in solution, is now confirmed by the determination of its crystal structure. The compound contains two six-coordinated RuI atoms, joined by an Ru—Ru single bond with a length of 2.6809 (6) Å. A mirror plane passes through the mid-point of the Ru—Ru bond and the two bridging thiolate ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803026874/br6125sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803026874/br6125Isup2.hkl
Contains datablock I

CCDC reference: 227773

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • R factor = 0.049
  • wR factor = 0.069
  • Data-to-parameter ratio = 20.2

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 0.00 Deg. PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.00 PLAT037_ALERT_1_A _diffrn_reflns_theta_full .......... Not Given . ? PLAT038_ALERT_1_A _diffrn_measured_fraction_theta_max Not Given . ? PLAT039_ALERT_1_A _diffrn_measured_fraction_theta_full Not Given . ?
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.106 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.11 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ru1 - C2 = 5.42 su PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C52 H40 O4 P2 Ru2 S2
5 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Ru2(C6H5S)2(C18H15P)2(CO)4]F(000) = 2136
Mr = 1057.04Dx = 1.473 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 3928 reflections
a = 17.2502 (9) Åθ = 2.5–25°
b = 24.4253 (13) ŵ = 0.83 mm1
c = 11.3154 (6) ÅT = 294 K
V = 4767.6 (4) Å3Columnar, yellow
Z = 40.30 × 0.11 × 0.10 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer
5947 independent reflections
Radiation source: fine-focus sealed tube3016 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.106
φ and ω scansθmax = 28.3°, θmin = 1.7°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1995)
h = 2222
Tmin = 0.818, Tmax = 0.922k = 1832
29562 measured reflectionsl = 1514
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: difference Fourier map
wR(F2) = 0.069H-atom parameters not refined
S = 0.88 w = 1/[σ2(Fo2) + (0.0208P)2]
where P = (Fo2 + 2Fc2)/3
5947 reflections(Δ/σ)max = 0.002
295 parametersΔρmax = 0.81 e Å3
0 restraintsΔρmin = 0.49 e Å3
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
Ru10.316846 (15)0.695121 (12)0.04656 (2)0.03455 (9)
S10.35959 (8)0.75000.12174 (12)0.0419 (4)
S20.42677 (7)0.75000.10965 (12)0.0377 (4)
P10.38476 (5)0.61117 (4)0.02761 (8)0.0384 (3)
O10.24155 (17)0.67167 (14)0.2810 (3)0.0820 (11)
O20.16459 (14)0.66757 (13)0.0676 (3)0.0739 (10)
C10.2727 (2)0.68002 (16)0.1935 (3)0.0475 (11)
C20.2230 (2)0.67722 (15)0.0243 (3)0.0450 (11)
C30.2954 (3)0.75000.2451 (4)0.0430 (15)
C40.2732 (2)0.70168 (18)0.2973 (3)0.0612 (12)
C50.2290 (3)0.7021 (2)0.3992 (4)0.0801 (15)
C60.2065 (4)0.75000.4504 (6)0.080 (2)
C70.4544 (3)0.75000.2619 (5)0.0403 (14)
C80.4027 (3)0.75000.3561 (5)0.0498 (16)
C90.4320 (4)0.75000.4695 (5)0.0659 (18)
C100.5098 (4)0.75000.4894 (5)0.076 (2)
C110.5604 (4)0.75000.3974 (6)0.074 (2)
C120.5334 (3)0.75000.2829 (5)0.0571 (17)
C130.4585 (2)0.60147 (15)0.1424 (3)0.0430 (10)
C140.4376 (3)0.60887 (18)0.2608 (4)0.0656 (13)
C150.4929 (3)0.6045 (2)0.3487 (4)0.0858 (17)
C160.5681 (3)0.5930 (2)0.3210 (5)0.0874 (19)
C170.5897 (3)0.5850 (2)0.2069 (5)0.0775 (16)
C180.5354 (3)0.58923 (17)0.1169 (4)0.0595 (12)
C190.3264 (2)0.54890 (14)0.0354 (3)0.0419 (9)
C200.3438 (2)0.50575 (19)0.1090 (4)0.0654 (13)
C210.2969 (3)0.4599 (2)0.1132 (4)0.0880 (17)
C220.2318 (3)0.4565 (2)0.0453 (6)0.0896 (17)
C230.2146 (3)0.4978 (2)0.0309 (5)0.0876 (17)
C240.2606 (2)0.54396 (17)0.0347 (4)0.0664 (12)
C250.4398 (2)0.60354 (16)0.1095 (3)0.0393 (10)
C260.4323 (2)0.56001 (17)0.1848 (4)0.0553 (12)
C270.4758 (3)0.5573 (2)0.2881 (4)0.0734 (15)
C280.5274 (3)0.5979 (2)0.3135 (4)0.0708 (15)
C290.5352 (2)0.64217 (19)0.2398 (4)0.0604 (13)
C300.4921 (2)0.64511 (16)0.1380 (4)0.0513 (11)
H4A0.28930.66810.26550.080*
H5A0.21290.67140.43150.080*
H6A0.17810.75000.52270.080*
H8A0.34740.75000.34360.080*
H9A0.39640.75000.52880.080*
H10A0.52770.75000.55940.080*
H11A0.61740.75000.41660.080*
H12A0.57380.75000.22010.080*
H14A0.38810.61740.27730.080*
H15A0.47300.60420.42590.080*
H16A0.60720.58830.37940.080*
H17A0.64090.58090.18240.080*
H18A0.55330.58490.04130.080*
H20A0.38680.50870.15980.080*
H21A0.31080.43320.16700.080*
H22A0.20670.42590.05320.080*
H23A0.17130.49630.07560.080*
H24A0.25040.57150.08700.080*
H26A0.39840.53320.17120.080*
H27A0.46880.52720.33750.080*
H28A0.55450.59270.38020.080*
H29A0.57170.67040.25850.080*
H30A0.49650.67420.08020.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.03451 (14)0.03508 (16)0.03406 (15)0.00207 (18)0.00108 (16)0.00056 (18)
S10.0477 (8)0.0426 (9)0.0355 (8)0.0000.0027 (7)0.000
S20.0325 (7)0.0413 (9)0.0394 (8)0.0000.0023 (6)0.000
P10.0410 (5)0.0355 (6)0.0388 (6)0.0024 (5)0.0003 (5)0.0022 (5)
O10.075 (2)0.117 (3)0.054 (2)0.032 (2)0.0196 (17)0.000 (2)
O20.0415 (17)0.104 (3)0.076 (2)0.0071 (17)0.0150 (15)0.0112 (19)
C10.043 (2)0.053 (3)0.046 (3)0.009 (2)0.001 (2)0.006 (2)
C20.042 (2)0.051 (3)0.042 (3)0.001 (2)0.007 (2)0.001 (2)
C30.060 (4)0.036 (4)0.034 (3)0.0000.001 (3)0.000
C40.092 (3)0.048 (3)0.044 (3)0.006 (3)0.007 (2)0.002 (2)
C50.123 (4)0.070 (4)0.047 (3)0.028 (4)0.020 (3)0.006 (3)
C60.102 (6)0.088 (6)0.050 (4)0.0000.025 (4)0.000
C70.042 (3)0.033 (3)0.046 (4)0.0000.008 (3)0.000
C80.039 (3)0.056 (4)0.054 (4)0.0000.012 (3)0.000
C90.066 (4)0.083 (5)0.049 (4)0.0000.001 (4)0.000
C100.089 (5)0.092 (6)0.047 (4)0.0000.028 (4)0.000
C110.064 (4)0.086 (6)0.072 (5)0.0000.037 (4)0.000
C120.038 (3)0.072 (5)0.062 (4)0.0000.008 (3)0.000
C130.048 (3)0.033 (3)0.048 (3)0.003 (2)0.009 (2)0.001 (2)
C140.080 (3)0.063 (3)0.054 (3)0.017 (3)0.014 (3)0.005 (3)
C150.130 (5)0.074 (4)0.053 (3)0.028 (4)0.034 (4)0.000 (3)
C160.100 (4)0.060 (4)0.102 (5)0.003 (4)0.066 (4)0.003 (3)
C170.058 (3)0.079 (4)0.095 (4)0.004 (3)0.026 (3)0.008 (3)
C180.059 (3)0.059 (3)0.061 (3)0.007 (3)0.015 (2)0.008 (2)
C190.043 (2)0.037 (2)0.046 (2)0.003 (2)0.004 (2)0.002 (2)
C200.075 (3)0.050 (3)0.071 (3)0.018 (3)0.010 (2)0.010 (3)
C210.111 (5)0.062 (4)0.091 (4)0.026 (4)0.005 (3)0.024 (3)
C220.079 (4)0.055 (4)0.135 (5)0.031 (3)0.015 (4)0.011 (4)
C230.062 (3)0.058 (3)0.143 (5)0.013 (3)0.023 (3)0.006 (4)
C240.061 (3)0.047 (3)0.091 (3)0.008 (3)0.014 (3)0.007 (3)
C250.039 (2)0.038 (3)0.042 (2)0.004 (2)0.0001 (19)0.004 (2)
C260.061 (3)0.053 (3)0.052 (3)0.012 (3)0.010 (2)0.006 (2)
C270.081 (3)0.079 (4)0.060 (3)0.006 (3)0.013 (3)0.026 (3)
C280.066 (3)0.098 (4)0.048 (3)0.002 (3)0.020 (3)0.005 (3)
C290.057 (3)0.060 (3)0.065 (3)0.002 (3)0.022 (3)0.007 (3)
C300.053 (3)0.047 (3)0.054 (3)0.003 (2)0.011 (2)0.001 (2)
Geometric parameters (Å, º) top
Ru1—C21.858 (4)C13—C181.389 (5)
Ru1—C11.866 (4)C13—C141.399 (5)
Ru1—P12.3713 (10)C14—C151.382 (5)
Ru1—S22.4294 (11)C14—H14A0.9000
Ru1—S12.4428 (11)C15—C161.364 (6)
Ru1—Ru1i2.6809 (6)C15—H15A0.9393
S1—C31.782 (5)C16—C171.358 (6)
S1—Ru1i2.4428 (11)C16—H16A0.9501
S2—C71.788 (5)C17—C181.387 (5)
S2—Ru1i2.4294 (11)C17—H17A0.9310
P1—C191.826 (4)C18—H18A0.9158
P1—C251.829 (4)C19—C201.376 (5)
P1—C131.834 (4)C19—C241.390 (5)
O1—C11.145 (4)C20—C211.383 (6)
O2—C21.145 (4)C20—H20A0.9414
C3—C41.374 (4)C21—C221.364 (6)
C3—C4i1.374 (4)C21—H21A0.9238
C4—C51.383 (5)C22—C231.360 (6)
C4—H4A0.9374C22—H22A0.8666
C5—C61.363 (5)C23—C241.380 (6)
C5—H5A0.8782C23—H23A0.9033
C6—C5i1.363 (5)C24—H24A0.9133
C6—H6A0.9531C25—C261.368 (5)
C7—C121.382 (6)C25—C301.396 (5)
C7—C81.390 (6)C26—C271.390 (5)
C8—C91.380 (7)C26—H26A0.8911
C8—H8A0.9639C27—C281.364 (6)
C9—C101.360 (8)C27—H27A0.9324
C9—H9A0.9095C28—C291.371 (6)
C10—C111.360 (8)C28—H28A0.8977
C10—H10A0.8505C29—C301.373 (5)
C11—C121.376 (7)C29—H29A0.9584
C11—H11A1.0067C30—H30A0.9678
C12—H12A0.9957
C2—Ru1—C188.99 (16)C11—C12—H12A115.8
C2—Ru1—P1100.83 (12)C7—C12—H12A124.5
C1—Ru1—P196.40 (12)C18—C13—C14118.2 (4)
C2—Ru1—S2159.45 (12)C18—C13—P1122.9 (3)
C1—Ru1—S299.55 (12)C14—C13—P1118.9 (3)
P1—Ru1—S296.78 (3)C15—C14—C13120.1 (4)
C2—Ru1—S193.20 (12)C15—C14—H14A121.6
C1—Ru1—S1157.89 (12)C13—C14—H14A118.3
P1—Ru1—S1104.76 (3)C16—C15—C14120.5 (5)
S2—Ru1—S171.98 (4)C16—C15—H15A124.1
C2—Ru1—Ru1i103.60 (12)C14—C15—H15A114.7
C1—Ru1—Ru1i101.40 (12)C17—C16—C15120.5 (5)
P1—Ru1—Ru1i149.85 (2)C17—C16—H16A116.8
S2—Ru1—Ru1i56.513 (17)C15—C16—H16A122.6
S1—Ru1—Ru1i56.720 (18)C16—C17—C18120.2 (5)
C3—S1—Ru1i115.02 (14)C16—C17—H17A123.9
C3—S1—Ru1115.02 (14)C18—C17—H17A115.5
Ru1i—S1—Ru166.56 (4)C17—C18—C13120.5 (4)
C7—S2—Ru1i119.44 (14)C17—C18—H18A116.7
C7—S2—Ru1119.44 (14)C13—C18—H18A122.8
Ru1i—S2—Ru166.97 (3)C20—C19—C24117.2 (4)
C19—P1—C25104.01 (17)C20—C19—P1123.2 (3)
C19—P1—C13103.92 (17)C24—C19—P1119.7 (3)
C25—P1—C13103.17 (18)C19—C20—C21121.0 (4)
C19—P1—Ru1116.33 (12)C19—C20—H20A118.8
C25—P1—Ru1114.92 (12)C21—C20—H20A120.2
C13—P1—Ru1112.99 (13)C22—C21—C20120.8 (5)
O1—C1—Ru1176.0 (4)C22—C21—H21A122.9
O2—C2—Ru1178.2 (4)C20—C21—H21A116.3
C4—C3—C4i118.4 (5)C23—C22—C21119.4 (5)
C4—C3—S1120.6 (3)C23—C22—H22A126.6
C4i—C3—S1120.6 (3)C21—C22—H22A113.9
C3—C4—C5120.4 (4)C22—C23—C24120.1 (5)
C3—C4—H4A120.3C22—C23—H23A120.4
C5—C4—H4A119.3C24—C23—H23A119.4
C6—C5—C4121.2 (5)C23—C24—C19121.5 (4)
C6—C5—H5A117.7C23—C24—H24A120.7
C4—C5—H5A121.1C19—C24—H24A117.7
C5—C6—C5i118.4 (6)C26—C25—C30118.9 (4)
C5—C6—H6A120.8C26—C25—P1123.9 (3)
C5i—C6—H6A120.8C30—C25—P1117.2 (3)
C12—C7—C8120.1 (5)C25—C26—C27120.6 (4)
C12—C7—S2115.4 (4)C25—C26—H26A121.6
C8—C7—S2124.6 (4)C27—C26—H26A117.7
C9—C8—C7118.5 (5)C28—C27—C26119.6 (4)
C9—C8—H8A119.9C28—C27—H27A122.2
C7—C8—H8A121.5C26—C27—H27A118.2
C10—C9—C8121.0 (6)C27—C28—C29120.6 (4)
C10—C9—H9A122.9C27—C28—H28A114.4
C8—C9—H9A116.0C29—C28—H28A125.0
C11—C10—C9120.5 (6)C28—C29—C30119.9 (4)
C11—C10—H10A118.6C28—C29—H29A119.8
C9—C10—H10A120.9C30—C29—H29A120.2
C10—C11—C12120.2 (5)C29—C30—C25120.3 (4)
C10—C11—H11A117.5C29—C30—H30A124.2
C12—C11—H11A122.3C25—C30—H30A115.4
C11—C12—C7119.7 (6)
Symmetry code: (i) x, y+3/2, z.
 

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