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

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ISSN: 2056-9890

μ-Propane-1,3-di­thiol­ato-κ4S,S′:S,S′-bis­­[dicarbon­yl(tri­phenyl­phosphane-κP)iron(II)](FeFe)

aCollege of Chemistry and Chemical Engineering, Hunan Normal University, Hunan 410081, People's Republic of China
*Correspondence e-mail: yinbangshao@yahoo.cn

(Received 30 September 2011; accepted 3 October 2011; online 8 October 2011)

The title compound, [Fe2(C3H6S2)(C18H15P)2(CO)4], which might serve as an active-site model of [FeFe]-hydrogenase, contains two fused Fe/S/C/C/C/S six-membered rings, one of which has a chair conformation and the other a boat conformation. Each Fe atom is coordinated by two carbonyl ligands, a triphenyl­phosphane ligand and a bis-bidentate dithiol­ate ligand, and also forms an Fe—Fe bond [2.5167 (16) Å]. Together, the six bonded atoms form a very distorted octa­hedral arrangement.

Related literature

For details of the synthesis, see: Li et al. (2005[Li, P., Wang, M., He, C., Li, G., Liu, X., Chen, C., Akermark, B. & Sun, L. (2005). Eur. J. Inorg. Chem. pp. 2506-2513.]). For more details about [FeFe]-hydrogenase model complexes, see: Song et al. (2005[Song, L. C., Yang, Z. Y., Bian, H. Z., Liu, Y., Wang, H. T., Liu, X. F. & Hu, Q. M. (2005). Organometallics, 24, 6126-6135.]); Liu & Xiao (2011[Liu, X. F. & Xiao, X. W. (2011). J. Organomet. Chem. 696, 2767-2771.]); Liu & Yin (2010[Liu, X. F. & Yin, B. S. (2010). J. Coord. Chem. 63, 4061-4067.], 2011[Liu, X. F. & Yin, B. S. (2011). Z. Anorg. Allg. Chem. 637, 377-379.]); Liu et al. (2011[Liu, X. F., Xiao, X. W. & Shen, L. J. (2011). J. Coord. Chem. 64, 1023-1031.]).

[Scheme 1]

Experimental

Crystal data
  • [Fe2(C3H6S2)(C18H15P)2(CO)4]

  • Mr = 854.48

  • Triclinic, [P \overline 1]

  • a = 9.139 (5) Å

  • b = 13.480 (5) Å

  • c = 16.786 (10) Å

  • α = 77.773 (19)°

  • β = 89.50 (2)°

  • γ = 71.187 (18)°

  • V = 1909.1 (17) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 1.00 mm−1

  • T = 113 K

  • 0.06 × 0.04 × 0.04 mm

Data collection
  • Rigaku Saturn724 CCD diffractometer

  • Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2005[Rigaku/MSC (2005). CrystalClear and CrystalStructure. Rigaku/MSC Inc., The Woodlands, Texas, USA.]) Tmin = 0.943, Tmax = 0.961

  • 15996 measured reflections

  • 6709 independent reflections

  • 2718 reflections with I > 2σ(I)

  • Rint = 0.124

Refinement
  • R[F2 > 2σ(F2)] = 0.075

  • wR(F2) = 0.146

  • S = 0.97

  • 6709 reflections

  • 478 parameters

  • H-atom parameters constrained

  • Δρmax = 1.35 e Å−3

  • Δρmin = −0.66 e Å−3

Table 1
Selected bond lengths (Å)

Fe1—C2 1.719 (8)
Fe1—C1 1.773 (8)
Fe1—P1 2.237 (2)
Fe1—S2 2.254 (2)
Fe1—S1 2.285 (2)
Fe2—C4 1.720 (8)
Fe2—C3 1.750 (8)
Fe2—P2 2.230 (2)
Fe2—S1 2.276 (2)
Fe2—S2 2.287 (2)

Data collection: CrystalClear (Rigaku/MSC, 2005[Rigaku/MSC (2005). CrystalClear and CrystalStructure. Rigaku/MSC Inc., The Woodlands, Texas, USA.]); cell refinement: CrystalClear; data reduction: CrystalClear; 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: XP in SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: CrystalStructure (Rigaku/MSC, 2005[Rigaku/MSC (2005). CrystalClear and CrystalStructure. Rigaku/MSC Inc., The Woodlands, Texas, USA.]).

Supporting information


Comment top

[FeFe]-hydrogenases are a class of natural enzymes that can catalyze the production and consumption of hydrogen gas in several microorganisms (Song et al., 2005); Liu & Yin, 2010, 2011); Liu & Xiao, 2011; Liu et al., 2011). In continuated our work, a [FeFe]-hydrogenases model complex had been synthesized. The strucuture was confirmed by X-ray crstallography.

Single-crystal X-ray diffraction analysis reveals that the title complex crystallizes in the triclinic space group P-1. As shown in Fig. 1, the title complex contains four carbonyls and two PPh3 ligands. The diiron propanedithiolate consists of two fused six-membered rings, in which one ring has a chair conformation and the other ring has a boat conformation. The PPh3 ligands reside in an axial position of the square-pyramidal geometry of the Fe atoms. As shown in Fig. 2, the crystal structure is stabilized by van der Waals interactions.

Related literature top

For details of the synthesis, see: Li et al. (2005). For more details about [FeFe]-hydrogenase model complexes, see: Song et al. (2005); Liu & Xiao (2011); Liu & Yin (2010, 2011); Liu et al. (2011).

Experimental top

The title complex was prepared according to the literature procedures (Li et al , 2005)). Crystals were grown from slow evaporation of dichloromethane and hexane solution at room temperature.

Refinement top

All the H atoms were positioned geometrically (C—H = 0.93–0.97 Å) and refined as riding with Uiso(H) = 1.2Ueq(C) or 1.5Ueq(methyl C).

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2005); cell refinement: CrystalClear (Rigaku/MSC, 2005); data reduction: CrystalClear (Rigaku/MSC, 2005); 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: CrystalStructure (Rigaku/MSC, 2005).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I). Displacement ellipsoids are drawn at the 30% probability level and H atoms are shown as small spheres of arbitrary radii.
[Figure 2] Fig. 2. The crystal packing for (I).
µ-Propane-1,3-dithiolato-κ4S,S':S,S'- bis[dicarbonyl(triphenylphosphane-κP)iron(II)](FeFe) top
Crystal data top
[Fe2(C3H6S2)(C18H15P)2(CO)4]Z = 2
Mr = 854.48F(000) = 880
Triclinic, P1Dx = 1.486 Mg m3
a = 9.139 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.480 (5) ÅCell parameters from 5985 reflections
c = 16.786 (10) Åθ = 1.6–26.1°
α = 77.773 (19)°µ = 1.00 mm1
β = 89.50 (2)°T = 113 K
γ = 71.187 (18)°Prism, colorless
V = 1909.1 (17) Å30.06 × 0.04 × 0.04 mm
Data collection top
Rigaku Saturn724 CCD
diffractometer
6709 independent reflections
Radiation source: rotating anode2718 reflections with I > 2σ(I)
Multilayer monochromatorRint = 0.124
Detector resolution: 14.22 pixels mm-1θmax = 25.0°, θmin = 1.6°
ω and ϕ scansh = 1010
Absorption correction: multi-scan
(CrystalClear; Rigaku/MSC, 2005)
k = 1612
Tmin = 0.943, Tmax = 0.961l = 1919
15996 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)] = 0.075Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.146H-atom parameters constrained
S = 0.97 w = 1/[σ2(Fo2) + (0.0041P)2]
where P = (Fo2 + 2Fc2)/3
6709 reflections(Δ/σ)max = 0.001
478 parametersΔρmax = 1.35 e Å3
0 restraintsΔρmin = 0.66 e Å3
Crystal data top
[Fe2(C3H6S2)(C18H15P)2(CO)4]γ = 71.187 (18)°
Mr = 854.48V = 1909.1 (17) Å3
Triclinic, P1Z = 2
a = 9.139 (5) ÅMo Kα radiation
b = 13.480 (5) ŵ = 1.00 mm1
c = 16.786 (10) ÅT = 113 K
α = 77.773 (19)°0.06 × 0.04 × 0.04 mm
β = 89.50 (2)°
Data collection top
Rigaku Saturn724 CCD
diffractometer
6709 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku/MSC, 2005)
2718 reflections with I > 2σ(I)
Tmin = 0.943, Tmax = 0.961Rint = 0.124
15996 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0750 restraints
wR(F2) = 0.146H-atom parameters constrained
S = 0.97Δρmax = 1.35 e Å3
6709 reflectionsΔρmin = 0.66 e Å3
478 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
Fe10.87669 (12)1.09597 (7)0.19524 (6)0.0333 (3)
Fe21.07650 (12)0.91292 (7)0.24157 (6)0.0341 (3)
P10.6388 (2)1.21710 (14)0.18129 (12)0.0316 (5)
P21.1691 (2)0.74053 (13)0.30622 (12)0.0314 (5)
S10.9131 (2)0.99887 (13)0.32702 (11)0.0359 (5)
S20.8517 (2)0.94621 (13)0.16626 (12)0.0356 (5)
O10.9526 (7)1.1484 (4)0.0249 (3)0.0531 (16)
O21.0428 (6)1.2238 (4)0.2488 (3)0.0423 (14)
O31.2386 (6)0.9101 (4)0.0911 (3)0.0574 (17)
O41.3209 (6)0.9648 (4)0.3122 (3)0.0482 (15)
C10.9215 (8)1.1291 (5)0.0921 (5)0.035 (2)
C20.9700 (9)1.1748 (5)0.2264 (4)0.037 (2)
C31.1720 (8)0.9076 (5)0.1509 (5)0.040 (2)
C41.2219 (9)0.9448 (5)0.2834 (4)0.0342 (19)
C50.7706 (8)0.9347 (5)0.3615 (4)0.038 (2)
H5A0.80290.89360.41830.045*
H5B0.67120.99210.36320.045*
C60.7389 (8)0.8584 (5)0.3127 (5)0.039 (2)
H6A0.83170.79350.31900.047*
H6B0.65230.83530.33620.047*
C70.6992 (8)0.9069 (5)0.2232 (5)0.040 (2)
H7A0.60560.97120.21720.049*
H7B0.67250.85450.19780.049*
C80.6245 (8)1.3568 (5)0.1372 (4)0.0308 (18)
C90.7434 (9)1.3833 (5)0.0962 (5)0.037 (2)
H90.83711.32710.09380.045*
C100.7330 (9)1.4864 (5)0.0589 (4)0.042 (2)
H100.81801.50170.03230.051*
C110.5929 (9)1.5688 (5)0.0612 (4)0.039 (2)
H110.58041.64080.03430.047*
C120.4745 (9)1.5446 (6)0.1024 (5)0.043 (2)
H120.38081.60060.10510.051*
C130.4893 (9)1.4402 (5)0.1400 (4)0.044 (2)
H130.40551.42530.16820.052*
C140.4933 (8)1.2007 (5)0.1161 (5)0.0325 (19)
C150.5438 (8)1.1447 (5)0.0520 (4)0.036 (2)
H150.65121.11100.04730.043*
C160.4372 (8)1.1397 (5)0.0023 (4)0.0322 (18)
H160.47301.10510.04590.039*
C170.2815 (9)1.1824 (5)0.0038 (5)0.042 (2)
H170.20951.17470.03300.050*
C180.2319 (9)1.2374 (5)0.0653 (5)0.041 (2)
H180.12401.26930.07010.049*
C190.3360 (8)1.2466 (5)0.1195 (5)0.040 (2)
H190.29831.28570.16050.048*
C200.5427 (8)1.2287 (5)0.2775 (4)0.0261 (17)
C210.5778 (9)1.2937 (5)0.3258 (5)0.043 (2)
H210.64231.33550.30650.051*
C220.5154 (9)1.2951 (6)0.4027 (5)0.044 (2)
H220.53501.33990.43500.053*
C230.4285 (9)1.2335 (6)0.4304 (5)0.044 (2)
H230.38911.23460.48290.053*
C240.3951 (8)1.1701 (5)0.3862 (5)0.042 (2)
H240.33341.12680.40730.051*
C250.4529 (9)1.1688 (5)0.3083 (5)0.041 (2)
H250.42841.12500.27660.049*
C261.1264 (8)0.6384 (5)0.2631 (4)0.0314 (18)
C271.0331 (9)0.6666 (5)0.1930 (5)0.037 (2)
H270.99040.74040.16710.045*
C280.9989 (8)0.5915 (5)0.1585 (5)0.039 (2)
H280.93610.61390.10900.047*
C291.0557 (8)0.4852 (5)0.1959 (5)0.037 (2)
H291.02860.43320.17440.044*
C301.1545 (8)0.4541 (5)0.2664 (4)0.037 (2)
H301.19750.38010.29170.044*
C311.1907 (8)0.5291 (5)0.2998 (4)0.0325 (19)
H311.25870.50670.34740.039*
C321.1094 (8)0.7174 (5)0.4129 (4)0.0304 (19)
C331.0258 (8)0.6510 (5)0.4409 (4)0.0336 (19)
H331.00120.61010.40660.040*
C340.9755 (8)0.6434 (5)0.5219 (5)0.037 (2)
H340.92050.59550.54280.044*
C351.0078 (9)0.7065 (5)0.5695 (4)0.040 (2)
H350.97100.70380.62270.048*
C361.0909 (8)0.7721 (6)0.5418 (5)0.041 (2)
H361.11320.81400.57600.049*
C371.1437 (8)0.7786 (5)0.4640 (5)0.037 (2)
H371.20290.82430.44500.044*
C381.3813 (8)0.6816 (5)0.3197 (4)0.0302 (18)
C391.4600 (9)0.6203 (5)0.3913 (5)0.044 (2)
H391.40420.61030.43870.053*
C401.6209 (10)0.5719 (6)0.3968 (5)0.051 (2)
H401.67420.53240.44780.061*
C411.7028 (9)0.5819 (5)0.3263 (5)0.047 (2)
H411.81160.54750.32830.056*
C421.6247 (9)0.6408 (5)0.2565 (5)0.042 (2)
H421.68010.64870.20870.050*
C431.4680 (9)0.6905 (5)0.2509 (5)0.038 (2)
H431.41720.73160.19960.045*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0382 (7)0.0381 (6)0.0270 (7)0.0102 (5)0.0135 (5)0.0182 (5)
Fe20.0353 (7)0.0404 (6)0.0284 (7)0.0078 (5)0.0130 (5)0.0191 (5)
P10.0332 (12)0.0366 (10)0.0252 (12)0.0072 (9)0.0094 (10)0.0142 (9)
P20.0324 (12)0.0381 (10)0.0254 (12)0.0074 (9)0.0083 (9)0.0177 (9)
S10.0384 (12)0.0419 (11)0.0294 (12)0.0086 (9)0.0137 (10)0.0201 (9)
S20.0384 (12)0.0385 (10)0.0311 (13)0.0080 (9)0.0100 (10)0.0181 (9)
O10.062 (4)0.068 (4)0.036 (4)0.026 (3)0.024 (3)0.020 (3)
O20.050 (4)0.054 (3)0.033 (3)0.024 (3)0.014 (3)0.022 (3)
O30.044 (4)0.099 (4)0.033 (4)0.020 (3)0.023 (3)0.028 (3)
O40.039 (4)0.056 (3)0.049 (4)0.014 (3)0.009 (3)0.013 (3)
C10.033 (5)0.034 (4)0.044 (6)0.014 (4)0.005 (4)0.014 (4)
C20.045 (5)0.037 (4)0.026 (5)0.013 (4)0.019 (4)0.005 (4)
C30.028 (5)0.049 (5)0.042 (6)0.010 (4)0.008 (4)0.016 (4)
C40.030 (5)0.042 (4)0.028 (5)0.007 (4)0.017 (4)0.009 (4)
C50.031 (4)0.041 (4)0.029 (5)0.002 (4)0.020 (4)0.006 (4)
C60.033 (5)0.035 (4)0.045 (6)0.006 (4)0.010 (4)0.007 (4)
C70.048 (5)0.022 (4)0.057 (6)0.010 (4)0.005 (5)0.023 (4)
C80.033 (5)0.036 (4)0.025 (5)0.009 (4)0.005 (4)0.016 (3)
C90.040 (5)0.030 (4)0.044 (6)0.010 (4)0.012 (4)0.016 (4)
C100.045 (5)0.057 (5)0.034 (5)0.024 (4)0.015 (4)0.018 (4)
C110.056 (6)0.034 (4)0.026 (5)0.014 (4)0.003 (4)0.000 (4)
C120.049 (6)0.045 (5)0.030 (5)0.005 (4)0.001 (4)0.017 (4)
C130.048 (6)0.041 (4)0.037 (5)0.005 (4)0.014 (4)0.013 (4)
C140.034 (5)0.029 (4)0.038 (5)0.011 (3)0.009 (4)0.012 (3)
C150.032 (5)0.038 (4)0.030 (5)0.002 (4)0.007 (4)0.016 (4)
C160.034 (5)0.037 (4)0.025 (5)0.007 (4)0.012 (4)0.015 (3)
C170.042 (5)0.049 (5)0.044 (6)0.020 (4)0.002 (4)0.023 (4)
C180.029 (5)0.064 (5)0.043 (6)0.023 (4)0.020 (4)0.029 (4)
C190.036 (5)0.043 (4)0.054 (6)0.018 (4)0.025 (4)0.032 (4)
C200.026 (4)0.026 (4)0.027 (5)0.008 (3)0.009 (4)0.009 (3)
C210.050 (5)0.041 (4)0.038 (6)0.012 (4)0.016 (4)0.017 (4)
C220.043 (5)0.063 (5)0.032 (5)0.014 (4)0.008 (4)0.029 (4)
C230.045 (6)0.055 (5)0.023 (5)0.003 (4)0.012 (4)0.013 (4)
C240.038 (5)0.036 (4)0.038 (6)0.002 (4)0.021 (4)0.001 (4)
C250.044 (5)0.035 (4)0.029 (5)0.009 (4)0.006 (4)0.012 (4)
C260.035 (5)0.034 (4)0.027 (5)0.007 (4)0.022 (4)0.019 (3)
C270.043 (5)0.032 (4)0.038 (5)0.006 (4)0.016 (4)0.021 (4)
C280.037 (5)0.046 (4)0.040 (5)0.013 (4)0.013 (4)0.023 (4)
C290.038 (5)0.036 (4)0.044 (6)0.013 (4)0.018 (4)0.022 (4)
C300.040 (5)0.035 (4)0.032 (5)0.002 (4)0.015 (4)0.017 (4)
C310.028 (4)0.049 (4)0.024 (5)0.010 (4)0.008 (4)0.021 (4)
C320.019 (4)0.035 (4)0.033 (5)0.003 (3)0.002 (4)0.016 (4)
C330.030 (5)0.033 (4)0.032 (5)0.000 (4)0.003 (4)0.013 (4)
C340.034 (5)0.033 (4)0.034 (5)0.001 (3)0.017 (4)0.004 (4)
C350.043 (5)0.055 (5)0.022 (5)0.011 (4)0.018 (4)0.017 (4)
C360.037 (5)0.060 (5)0.031 (5)0.011 (4)0.016 (4)0.027 (4)
C370.034 (5)0.038 (4)0.037 (5)0.005 (4)0.003 (4)0.016 (4)
C380.041 (5)0.032 (4)0.020 (5)0.014 (4)0.013 (4)0.009 (3)
C390.036 (5)0.053 (5)0.043 (6)0.012 (4)0.014 (4)0.015 (4)
C400.050 (6)0.063 (5)0.037 (6)0.008 (5)0.004 (5)0.019 (4)
C410.037 (5)0.050 (5)0.052 (6)0.002 (4)0.014 (5)0.028 (5)
C420.043 (5)0.050 (5)0.033 (5)0.013 (4)0.014 (4)0.015 (4)
C430.042 (5)0.045 (4)0.023 (5)0.009 (4)0.002 (4)0.010 (4)
Geometric parameters (Å, º) top
Fe1—C21.719 (8)C17—H170.9500
Fe1—C11.773 (8)C18—C191.374 (9)
Fe1—P12.237 (2)C18—H180.9500
Fe1—S22.254 (2)C19—H190.9500
Fe1—S12.285 (2)C20—C251.355 (9)
Fe1—Fe22.5167 (16)C20—C211.419 (9)
Fe2—C41.720 (8)C21—C221.408 (9)
Fe2—C31.750 (8)C21—H210.9500
Fe2—P22.230 (2)C22—C231.339 (10)
Fe2—S12.276 (2)C22—H220.9500
Fe2—S22.287 (2)C23—C241.349 (9)
P1—C141.826 (7)C23—H230.9500
P1—C81.834 (7)C24—C251.407 (9)
P1—C201.843 (7)C24—H240.9500
P2—C261.829 (7)C25—H250.9500
P2—C381.839 (7)C26—C271.369 (9)
P2—C321.859 (8)C26—C311.399 (8)
S1—C51.812 (7)C27—C281.382 (8)
S2—C71.837 (8)C27—H270.9500
O1—C11.156 (8)C28—C291.365 (8)
O2—C21.189 (8)C28—H280.9500
O3—C31.171 (9)C29—C301.398 (9)
O4—C41.160 (8)C29—H290.9500
C5—C61.538 (8)C30—C311.380 (8)
C5—H5A0.9900C30—H300.9500
C5—H5B0.9900C31—H310.9500
C6—C71.502 (9)C32—C331.366 (9)
C6—H6A0.9900C32—C371.409 (9)
C6—H6B0.9900C33—C341.425 (9)
C7—H7A0.9900C33—H330.9500
C7—H7B0.9900C34—C351.380 (9)
C8—C91.384 (9)C34—H340.9500
C8—C131.385 (9)C35—C361.352 (9)
C9—C101.372 (8)C35—H350.9500
C9—H90.9500C36—C371.384 (9)
C10—C111.405 (9)C36—H360.9500
C10—H100.9500C37—H370.9500
C11—C121.369 (10)C38—C391.362 (9)
C11—H110.9500C38—C431.402 (9)
C12—C131.378 (9)C39—C401.398 (10)
C12—H120.9500C39—H390.9500
C13—H130.9500C40—C411.400 (10)
C14—C191.376 (9)C40—H400.9500
C14—C151.432 (9)C41—C421.329 (10)
C15—C161.367 (9)C41—H410.9500
C15—H150.9500C42—C431.366 (9)
C16—C171.364 (9)C42—H420.9500
C16—H160.9500C43—H430.9500
C17—C181.387 (9)
C2—Fe1—C193.2 (3)C19—C14—P1124.3 (6)
C2—Fe1—P196.3 (2)C15—C14—P1118.7 (6)
C1—Fe1—P196.4 (2)C16—C15—C14119.9 (7)
C2—Fe1—S2156.9 (2)C16—C15—H15120.0
C1—Fe1—S286.5 (2)C14—C15—H15120.0
P1—Fe1—S2106.71 (9)C17—C16—C15122.5 (7)
C2—Fe1—S187.4 (2)C17—C16—H16118.7
C1—Fe1—S1156.3 (2)C15—C16—H16118.7
P1—Fe1—S1107.06 (8)C16—C17—C18117.8 (7)
S2—Fe1—S183.84 (8)C16—C17—H17121.1
C2—Fe1—Fe2100.6 (2)C18—C17—H17121.1
C1—Fe1—Fe2100.5 (2)C19—C18—C17121.1 (7)
P1—Fe1—Fe2155.34 (8)C19—C18—H18119.4
S2—Fe1—Fe256.98 (6)C17—C18—H18119.4
S1—Fe1—Fe256.33 (6)C18—C19—C14121.8 (7)
C4—Fe2—C390.2 (3)C18—C19—H19119.1
C4—Fe2—P293.3 (2)C14—C19—H19119.1
C3—Fe2—P2100.2 (2)C25—C20—C21118.4 (7)
C4—Fe2—S188.2 (2)C25—C20—P1122.5 (5)
C3—Fe2—S1153.7 (2)C21—C20—P1118.7 (6)
P2—Fe2—S1106.10 (9)C22—C21—C20118.8 (7)
C4—Fe2—S2156.0 (2)C22—C21—H21120.6
C3—Fe2—S287.6 (3)C20—C21—H21120.6
P2—Fe2—S2110.61 (8)C23—C22—C21120.3 (7)
S1—Fe2—S283.30 (8)C23—C22—H22119.8
C4—Fe2—Fe1101.1 (2)C21—C22—H22119.8
C3—Fe2—Fe198.0 (2)C22—C23—C24122.0 (8)
P2—Fe2—Fe1156.70 (8)C22—C23—H23119.0
S1—Fe2—Fe156.69 (6)C24—C23—H23119.0
S2—Fe2—Fe155.71 (6)C23—C24—C25119.0 (8)
C14—P1—C8100.7 (3)C23—C24—H24120.5
C14—P1—C20103.1 (3)C25—C24—H24120.5
C8—P1—C20102.0 (3)C20—C25—C24121.5 (7)
C14—P1—Fe1117.7 (2)C20—C25—H25119.3
C8—P1—Fe1116.2 (2)C24—C25—H25119.3
C20—P1—Fe1114.9 (2)C27—C26—C31118.1 (6)
C26—P2—C3899.4 (3)C27—C26—P2120.9 (5)
C26—P2—C32104.5 (3)C31—C26—P2121.0 (6)
C38—P2—C32102.6 (3)C26—C27—C28122.5 (6)
C26—P2—Fe2119.9 (2)C26—C27—H27118.8
C38—P2—Fe2115.9 (2)C28—C27—H27118.8
C32—P2—Fe2112.5 (2)C29—C28—C27119.8 (7)
C5—S1—Fe2112.2 (2)C29—C28—H28120.1
C5—S1—Fe1116.5 (2)C27—C28—H28120.1
Fe2—S1—Fe166.98 (7)C28—C29—C30118.8 (6)
C7—S2—Fe1111.5 (2)C28—C29—H29120.6
C7—S2—Fe2115.3 (2)C30—C29—H29120.6
Fe1—S2—Fe267.31 (7)C31—C30—C29121.2 (6)
O1—C1—Fe1178.5 (6)C31—C30—H30119.4
O2—C2—Fe1175.9 (6)C29—C30—H30119.4
O3—C3—Fe2175.3 (7)C30—C31—C26119.6 (7)
O4—C4—Fe2179.0 (7)C30—C31—H31120.2
C6—C5—S1118.7 (5)C26—C31—H31120.2
C6—C5—H5A107.6C33—C32—C37119.7 (7)
S1—C5—H5A107.6C33—C32—P2123.1 (5)
C6—C5—H5B107.6C37—C32—P2117.0 (6)
S1—C5—H5B107.6C32—C33—C34119.6 (7)
H5A—C5—H5B107.1C32—C33—H33120.2
C7—C6—C5114.1 (5)C34—C33—H33120.2
C7—C6—H6A108.7C35—C34—C33119.1 (7)
C5—C6—H6A108.7C35—C34—H34120.5
C7—C6—H6B108.7C33—C34—H34120.5
C5—C6—H6B108.7C36—C35—C34121.3 (7)
H6A—C6—H6B107.6C36—C35—H35119.4
C6—C7—S2115.6 (5)C34—C35—H35119.4
C6—C7—H7A108.4C35—C36—C37120.3 (7)
S2—C7—H7A108.4C35—C36—H36119.8
C6—C7—H7B108.4C37—C36—H36119.8
S2—C7—H7B108.4C36—C37—C32119.9 (7)
H7A—C7—H7B107.4C36—C37—H37120.0
C9—C8—C13117.2 (7)C32—C37—H37120.0
C9—C8—P1122.0 (5)C39—C38—C43117.0 (7)
C13—C8—P1120.7 (6)C39—C38—P2124.0 (6)
C10—C9—C8123.4 (7)C43—C38—P2118.6 (6)
C10—C9—H9118.3C38—C39—C40121.6 (8)
C8—C9—H9118.3C38—C39—H39119.2
C9—C10—C11118.0 (7)C40—C39—H39119.2
C9—C10—H10121.0C39—C40—C41119.5 (8)
C11—C10—H10121.0C39—C40—H40120.3
C12—C11—C10119.6 (7)C41—C40—H40120.3
C12—C11—H11120.2C42—C41—C40118.5 (8)
C10—C11—H11120.2C42—C41—H41120.8
C11—C12—C13121.0 (7)C40—C41—H41120.8
C11—C12—H12119.5C41—C42—C43122.6 (8)
C13—C12—H12119.5C41—C42—H42118.7
C12—C13—C8120.9 (8)C43—C42—H42118.7
C12—C13—H13119.6C42—C43—C38120.9 (7)
C8—C13—H13119.6C42—C43—H43119.6
C19—C14—C15116.8 (7)C38—C43—H43119.6
C2—Fe1—Fe2—C40.7 (3)Fe1—S1—C5—C655.4 (5)
C1—Fe1—Fe2—C494.6 (3)S1—C5—C6—C753.4 (8)
P1—Fe1—Fe2—C4133.1 (3)C5—C6—C7—S262.7 (7)
S2—Fe1—Fe2—C4173.4 (3)Fe1—S2—C7—C673.7 (5)
S1—Fe1—Fe2—C480.4 (3)Fe2—S2—C7—C60.5 (5)
C2—Fe1—Fe2—C392.5 (4)C14—P1—C8—C9112.5 (7)
C1—Fe1—Fe2—C32.8 (3)C20—P1—C8—C9141.5 (6)
P1—Fe1—Fe2—C3135.1 (3)Fe1—P1—C8—C915.8 (7)
S2—Fe1—Fe2—C381.6 (3)C14—P1—C8—C1363.9 (6)
S1—Fe1—Fe2—C3172.2 (3)C20—P1—C8—C1342.1 (6)
C2—Fe1—Fe2—P2126.3 (3)Fe1—P1—C8—C13167.8 (5)
C1—Fe1—Fe2—P2138.4 (3)C13—C8—C9—C100.1 (11)
P1—Fe1—Fe2—P26.0 (3)P1—C8—C9—C10176.4 (5)
S2—Fe1—Fe2—P259.59 (19)C8—C9—C10—C111.4 (11)
S1—Fe1—Fe2—P246.63 (18)C9—C10—C11—C122.2 (11)
C2—Fe1—Fe2—S179.7 (3)C10—C11—C12—C131.6 (12)
C1—Fe1—Fe2—S1175.0 (2)C11—C12—C13—C80.1 (12)
P1—Fe1—Fe2—S152.67 (18)C9—C8—C13—C120.7 (11)
S2—Fe1—Fe2—S1106.21 (10)P1—C8—C13—C12175.8 (6)
C2—Fe1—Fe2—S2174.1 (3)C8—P1—C14—C1972.6 (7)
C1—Fe1—Fe2—S278.8 (2)C20—P1—C14—C1932.5 (7)
P1—Fe1—Fe2—S253.54 (18)Fe1—P1—C14—C19160.1 (5)
S1—Fe1—Fe2—S2106.21 (10)C8—P1—C14—C15101.6 (6)
C2—Fe1—P1—C14159.2 (4)C20—P1—C14—C15153.3 (5)
C1—Fe1—P1—C1465.3 (4)Fe1—P1—C14—C1525.7 (7)
S2—Fe1—P1—C1423.0 (3)C19—C14—C15—C160.6 (11)
S1—Fe1—P1—C14111.6 (3)P1—C14—C15—C16174.0 (5)
Fe2—Fe1—P1—C1467.8 (3)C14—C15—C16—C173.0 (11)
C2—Fe1—P1—C839.7 (4)C15—C16—C17—C183.4 (11)
C1—Fe1—P1—C854.2 (3)C16—C17—C18—C191.4 (12)
S2—Fe1—P1—C8142.5 (3)C17—C18—C19—C140.9 (12)
S1—Fe1—P1—C8129.0 (3)C15—C14—C19—C181.3 (11)
Fe2—Fe1—P1—C8172.8 (3)P1—C14—C19—C18175.6 (6)
C2—Fe1—P1—C2079.1 (3)C14—P1—C20—C2539.2 (6)
C1—Fe1—P1—C20173.1 (3)C8—P1—C20—C25143.4 (6)
S2—Fe1—P1—C2098.7 (3)Fe1—P1—C20—C2590.1 (6)
S1—Fe1—P1—C2010.1 (3)C14—P1—C20—C21148.0 (5)
Fe2—Fe1—P1—C2053.9 (3)C8—P1—C20—C2143.9 (6)
C4—Fe2—P2—C26154.4 (4)Fe1—P1—C20—C2182.7 (5)
C3—Fe2—P2—C2663.6 (4)C25—C20—C21—C221.3 (10)
S1—Fe2—P2—C26116.5 (3)P1—C20—C21—C22174.4 (5)
S2—Fe2—P2—C2627.7 (3)C20—C21—C22—C232.0 (11)
Fe1—Fe2—P2—C2677.3 (3)C21—C22—C23—C241.2 (12)
C4—Fe2—P2—C3835.2 (3)C22—C23—C24—C250.2 (11)
C3—Fe2—P2—C3855.6 (4)C21—C20—C25—C240.1 (10)
S1—Fe2—P2—C38124.3 (3)P1—C20—C25—C24172.7 (5)
S2—Fe2—P2—C38146.9 (3)C23—C24—C25—C200.9 (10)
Fe1—Fe2—P2—C38163.6 (3)C38—P2—C26—C27129.7 (6)
C4—Fe2—P2—C3282.3 (3)C32—P2—C26—C27124.6 (6)
C3—Fe2—P2—C32173.1 (4)Fe2—P2—C26—C272.5 (7)
S1—Fe2—P2—C326.8 (3)C38—P2—C26—C3148.9 (6)
S2—Fe2—P2—C3295.5 (3)C32—P2—C26—C3156.8 (6)
Fe1—Fe2—P2—C3246.0 (3)Fe2—P2—C26—C31176.1 (5)
C4—Fe2—S1—C5145.0 (3)C31—C26—C27—C281.1 (11)
C3—Fe2—S1—C5128.1 (6)P2—C26—C27—C28179.7 (5)
P2—Fe2—S1—C552.1 (3)C26—C27—C28—C291.8 (11)
S2—Fe2—S1—C557.5 (3)C27—C28—C29—C303.4 (11)
Fe1—Fe2—S1—C5110.5 (3)C28—C29—C30—C312.2 (11)
C4—Fe2—S1—Fe1104.5 (2)C29—C30—C31—C260.6 (11)
C3—Fe2—S1—Fe117.6 (6)C27—C26—C31—C302.2 (10)
P2—Fe2—S1—Fe1162.59 (8)P2—C26—C31—C30179.2 (5)
S2—Fe2—S1—Fe153.01 (7)C26—P2—C32—C3311.0 (6)
C2—Fe1—S1—C5151.2 (3)C38—P2—C32—C33114.3 (5)
C1—Fe1—S1—C5116.7 (6)Fe2—P2—C32—C33120.5 (5)
P1—Fe1—S1—C555.4 (2)C26—P2—C32—C37173.8 (5)
S2—Fe1—S1—C550.2 (2)C38—P2—C32—C3770.6 (5)
Fe2—Fe1—S1—C5104.3 (2)Fe2—P2—C32—C3754.6 (5)
C2—Fe1—S1—Fe2104.5 (2)C37—C32—C33—C340.7 (9)
C1—Fe1—S1—Fe212.4 (6)P2—C32—C33—C34175.7 (4)
P1—Fe1—S1—Fe2159.70 (8)C32—C33—C34—C352.3 (9)
S2—Fe1—S1—Fe254.07 (7)C33—C34—C35—C362.5 (10)
C2—Fe1—S2—C7124.4 (7)C34—C35—C36—C371.0 (11)
C1—Fe1—S2—C7145.6 (3)C35—C36—C37—C320.7 (10)
P1—Fe1—S2—C750.0 (3)C33—C32—C37—C360.8 (9)
S1—Fe1—S2—C756.0 (3)P2—C32—C37—C36174.5 (5)
Fe2—Fe1—S2—C7109.5 (3)C26—P2—C38—C3996.6 (6)
C2—Fe1—S2—Fe214.9 (6)C32—P2—C38—C3910.7 (6)
C1—Fe1—S2—Fe2104.9 (2)Fe2—P2—C38—C39133.6 (5)
P1—Fe1—S2—Fe2159.49 (8)C26—P2—C38—C4376.7 (6)
S1—Fe1—S2—Fe253.49 (7)C32—P2—C38—C43176.1 (5)
C4—Fe2—S2—C7120.2 (6)Fe2—P2—C38—C4353.2 (6)
C3—Fe2—S2—C7154.6 (3)C43—C38—C39—C402.5 (10)
P2—Fe2—S2—C754.6 (2)P2—C38—C39—C40175.8 (5)
S1—Fe2—S2—C750.1 (2)C38—C39—C40—C413.2 (11)
Fe1—Fe2—S2—C7104.0 (2)C39—C40—C41—C422.3 (11)
C4—Fe2—S2—Fe116.2 (6)C40—C41—C42—C430.9 (12)
C3—Fe2—S2—Fe1101.4 (2)C41—C42—C43—C380.2 (11)
P2—Fe2—S2—Fe1158.63 (8)C39—C38—C43—C421.0 (10)
S1—Fe2—S2—Fe153.90 (7)P2—C38—C43—C42174.7 (5)
Fe2—S1—C5—C619.0 (6)

Experimental details

Crystal data
Chemical formula[Fe2(C3H6S2)(C18H15P)2(CO)4]
Mr854.48
Crystal system, space groupTriclinic, P1
Temperature (K)113
a, b, c (Å)9.139 (5), 13.480 (5), 16.786 (10)
α, β, γ (°)77.773 (19), 89.50 (2), 71.187 (18)
V3)1909.1 (17)
Z2
Radiation typeMo Kα
µ (mm1)1.00
Crystal size (mm)0.06 × 0.04 × 0.04
Data collection
DiffractometerRigaku Saturn724 CCD
diffractometer
Absorption correctionMulti-scan
(CrystalClear; Rigaku/MSC, 2005)
Tmin, Tmax0.943, 0.961
No. of measured, independent and
observed [I > 2σ(I)] reflections
15996, 6709, 2718
Rint0.124
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.075, 0.146, 0.97
No. of reflections6709
No. of parameters478
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.35, 0.66

Computer programs: CrystalClear (Rigaku/MSC, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), CrystalStructure (Rigaku/MSC, 2005).

Selected bond lengths (Å) top
Fe1—C21.719 (8)Fe2—C41.720 (8)
Fe1—C11.773 (8)Fe2—C31.750 (8)
Fe1—P12.237 (2)Fe2—P22.230 (2)
Fe1—S22.254 (2)Fe2—S12.276 (2)
Fe1—S12.285 (2)Fe2—S22.287 (2)
 

Acknowledgements

This work was supported by the start-up foundation of Hunan Normal University.

References

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First citationSong, L. C., Yang, Z. Y., Bian, H. Z., Liu, Y., Wang, H. T., Liu, X. F. & Hu, Q. M. (2005). Organometallics, 24, 6126–6135.  Web of Science CSD CrossRef CAS Google Scholar

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