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

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ISSN: 2056-9890

Penta­carbonyl-1κ2C,2κ3C-[(di­phenyl­phosphor­yl)di­phenyl­phosphane-1κP]-μ-ethane-1,2-di­thiol­ato-1:2κ4S,S′:S,S′-diiron(I)(Fe—Fe)

aDepartment of Chemical Engineering, Ningbo University of Technology, Ningbo 315016, People's Republic of China
*Correspondence e-mail: nkxfliu@yahoo.com.cn

(Received 7 October 2011; accepted 12 October 2011; online 22 October 2011)

The dinuclear title compound, [Fe2(C2H4S2)(C24H20OP2)(CO)5] or (μ-SCH2CH2S-μ)Fe2(CO)5[Ph2PP(O)Ph2], con­tains a butterfly-shaped Fe2S2 core in which the Fe⋯Fe separation is 2.5275 (6) Å. One of the Fe atoms is also coordinated to three carbonyl ligands and the other to two carbonyl ligands and one phosphane ligand [Ph2PP(O)Ph2]. Both Fe-atom geometries could be described as grossly distorted octa­hedral and the Ph2PP(O)Ph2 ligand lies trans to the Fe⋯Fe link.

Related literature

For more details about diiron dithiol­ate 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.]); Wang et al. (2009[Wang, N., Wang, M., Liu, J., Jin, K., Chen, L. & Sun, L. (2009). Inorg. Chem. 48, 11551-11558.]); Yin et al. (2011[Yin, B. S., Li, T. B. & Yang, M. S. (2011). J. Coord. Chem. 64, 2066-2074.]).

[Scheme 1]

Experimental

Crystal data
  • [Fe2(C2H4S2)(C24H20OP2)(CO)5]

  • Mr = 730.26

  • Monoclinic, P 21 /n

  • a = 13.865 (4) Å

  • b = 15.398 (4) Å

  • c = 14.459 (5) Å

  • β = 98.357 (4)°

  • V = 3054.1 (16) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.24 mm−1

  • T = 113 K

  • 0.20 × 0.18 × 0.10 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 = 0.790, Tmax = 0.886

  • 31351 measured reflections

  • 7281 independent reflections

  • 6102 reflections with I > 2σ(I)

  • Rint = 0.039

Refinement
  • R[F2 > 2σ(F2)] = 0.026

  • wR(F2) = 0.059

  • S = 1.06

  • 7281 reflections

  • 388 parameters

  • H-atom parameters constrained

  • Δρmax = 0.36 e Å−3

  • Δρmin = −0.36 e Å−3

Table 1
Selected bond lengths (Å)

Fe1—C2 1.7855 (18)
Fe1—C1 1.7981 (17)
Fe1—C3 1.8006 (18)
Fe1—S1 2.2484 (6)
Fe1—S2 2.2495 (8)
Fe2—C4 1.7733 (17)
Fe2—C5 1.7742 (17)
Fe2—P1 2.2426 (7)
Fe2—S1 2.2495 (7)
Fe2—S2 2.2530 (7)

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: 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

Diiron dithiolate complexes have received much attention in recent years due to their structures close to the active site of [FeFe]-hydrogenases (Song et al. (2005), Wang et al. (2009), Yin et al. (2011)). In continuation of our work in this area, the title complex, (I), was synthesized and its strucuture was determined by X-ray crstallography.

As shown in Fig. 1, the title complex contains five carbonyls and one Ph2PP(O)Ph2 ligands. The diiron ethanedithiolate cluster consists of two fused five-membered rings. The Ph2PP(O)Ph2 ligands occupies an axial position of the square-pyramidal geometry of the Fe atom.

Related literature top

For more details about diiron dithiolate complexes, see: Song et al. (2005); Wang et al. (2009); Yin et al. (2011).

Experimental top

The title complex was prepared from (µ-SCH2CH2S-µ)Fe2(CO)6 and 1,2-bis(diphenylphosphino)cyclopentane in the presence of Me3NO. Colourless prisms 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).
Pentacarbonyl-1κ2C,2κ3C- [(diphenylphosphoryl)diphenylphosphane-1κP]-µ-ethane-1,2-dithiolato- 1:2κ4S,S':S,S'-diiron(I)(FeFe) top
Crystal data top
[Fe2(C2H4S2)(C24H20OP2)(CO)5]F(000) = 1488
Mr = 730.26Dx = 1.588 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 11006 reflections
a = 13.865 (4) Åθ = 1.4–27.9°
b = 15.398 (4) ŵ = 1.24 mm1
c = 14.459 (5) ÅT = 113 K
β = 98.357 (4)°Prism, colorless
V = 3054.1 (16) Å30.20 × 0.18 × 0.10 mm
Z = 4
Data collection top
Rigaku Saturn724 CCD
diffractometer
7281 independent reflections
Radiation source: rotating anode6102 reflections with I > 2σ(I)
Multilayer monochromatorRint = 0.039
Detector resolution: 14.22 pixels mm-1θmax = 27.9°, θmin = 1.9°
ω and ϕ scansh = 1818
Absorption correction: multi-scan
(CrystalClear; Rigaku/MSC, 2005)
k = 1720
Tmin = 0.790, Tmax = 0.886l = 1919
31351 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)] = 0.026Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.059H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.024P)2]
where P = (Fo2 + 2Fc2)/3
7281 reflections(Δ/σ)max = 0.002
388 parametersΔρmax = 0.36 e Å3
0 restraintsΔρmin = 0.36 e Å3
Crystal data top
[Fe2(C2H4S2)(C24H20OP2)(CO)5]V = 3054.1 (16) Å3
Mr = 730.26Z = 4
Monoclinic, P21/nMo Kα radiation
a = 13.865 (4) ŵ = 1.24 mm1
b = 15.398 (4) ÅT = 113 K
c = 14.459 (5) Å0.20 × 0.18 × 0.10 mm
β = 98.357 (4)°
Data collection top
Rigaku Saturn724 CCD
diffractometer
7281 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku/MSC, 2005)
6102 reflections with I > 2σ(I)
Tmin = 0.790, Tmax = 0.886Rint = 0.039
31351 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0260 restraints
wR(F2) = 0.059H-atom parameters constrained
S = 1.06Δρmax = 0.36 e Å3
7281 reflectionsΔρmin = 0.36 e Å3
388 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
Fe11.261528 (16)0.058771 (14)0.331352 (16)0.01557 (6)
Fe21.133418 (15)0.174298 (14)0.288051 (14)0.01275 (6)
P10.99707 (3)0.24364 (3)0.31226 (3)0.01291 (9)
P20.86096 (3)0.16331 (3)0.27704 (3)0.01404 (9)
S11.18853 (3)0.13327 (3)0.43559 (3)0.01697 (9)
S21.10474 (3)0.03046 (2)0.27533 (3)0.01596 (9)
O11.30120 (9)0.10606 (7)0.43282 (8)0.0300 (3)
O21.43873 (9)0.15892 (8)0.39375 (10)0.0411 (4)
O31.32473 (9)0.01325 (8)0.15188 (9)0.0366 (3)
O41.26144 (9)0.32544 (8)0.29575 (9)0.0321 (3)
O51.12828 (9)0.17617 (8)0.08534 (8)0.0298 (3)
O60.86136 (7)0.09157 (6)0.34670 (7)0.0177 (2)
C11.28842 (11)0.04173 (11)0.39306 (11)0.0209 (4)
C21.36981 (12)0.11973 (11)0.36834 (13)0.0250 (4)
C31.29927 (12)0.03076 (10)0.22113 (12)0.0232 (4)
C41.20985 (12)0.26713 (10)0.29551 (11)0.0193 (3)
C51.12641 (11)0.17650 (10)0.16457 (11)0.0185 (3)
C61.09760 (11)0.05588 (10)0.46439 (11)0.0209 (4)
H6A1.12660.02000.51820.025*
H6B1.04180.08810.48330.025*
C71.06081 (12)0.00340 (10)0.38252 (11)0.0195 (3)
H7A0.98860.00310.37240.023*
H7B1.08270.06360.39790.023*
C80.99500 (11)0.27904 (10)0.43317 (10)0.0167 (3)
C91.05975 (13)0.34539 (11)0.46564 (12)0.0259 (4)
H91.10290.36760.42600.031*
C101.06217 (14)0.37937 (12)0.55452 (12)0.0328 (4)
H101.10680.42440.57560.039*
C110.99951 (13)0.34765 (12)0.61251 (12)0.0310 (4)
H111.00010.37160.67310.037*
C120.93619 (13)0.28118 (12)0.58215 (12)0.0303 (4)
H120.89400.25890.62260.036*
C130.93332 (11)0.24635 (11)0.49297 (11)0.0209 (4)
H130.88950.20040.47290.025*
C140.96328 (11)0.34554 (9)0.24976 (11)0.0151 (3)
C151.00002 (11)0.36534 (10)0.16773 (11)0.0186 (3)
H151.04640.32790.14620.022*
C160.96935 (12)0.43952 (10)0.11709 (12)0.0247 (4)
H160.99380.45170.06040.030*
C170.90373 (12)0.49556 (11)0.14854 (12)0.0258 (4)
H170.88300.54620.11370.031*
C180.86815 (12)0.47762 (11)0.23126 (12)0.0254 (4)
H180.82330.51630.25350.031*
C190.89793 (11)0.40335 (10)0.28154 (11)0.0210 (4)
H190.87350.39160.33840.025*
C200.86646 (11)0.12448 (10)0.16014 (10)0.0167 (3)
C210.85652 (12)0.03529 (10)0.14617 (11)0.0235 (4)
H210.84660.00130.19680.028*
C220.86095 (14)0.00041 (12)0.05905 (12)0.0327 (4)
H220.85250.06120.04980.039*
C230.87764 (13)0.05197 (12)0.01452 (12)0.0308 (4)
H230.88170.02720.07400.037*
C240.88851 (12)0.14079 (12)0.00128 (12)0.0257 (4)
H240.90030.17690.05170.031*
C250.88221 (11)0.17707 (11)0.08506 (11)0.0214 (4)
H250.88860.23810.09340.026*
C260.75306 (11)0.22975 (10)0.27313 (10)0.0156 (3)
C270.70310 (11)0.22562 (10)0.35030 (11)0.0185 (3)
H270.72700.18970.40200.022*
C280.61916 (11)0.27358 (10)0.35174 (12)0.0224 (4)
H280.58550.27040.40430.027*
C290.58382 (12)0.32645 (10)0.27659 (12)0.0252 (4)
H290.52630.35970.27770.030*
C300.63304 (12)0.33036 (11)0.20009 (12)0.0265 (4)
H300.60880.36620.14850.032*
C310.71692 (11)0.28270 (10)0.19801 (11)0.0216 (4)
H310.75020.28600.14510.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.01547 (12)0.01379 (12)0.01783 (12)0.00070 (9)0.00372 (9)0.00033 (9)
Fe20.01568 (12)0.01181 (12)0.01079 (11)0.00046 (8)0.00202 (8)0.00040 (8)
P10.0163 (2)0.0118 (2)0.01058 (19)0.00003 (15)0.00202 (15)0.00057 (15)
P20.0160 (2)0.0135 (2)0.01251 (19)0.00015 (15)0.00168 (15)0.00074 (15)
S10.0216 (2)0.0164 (2)0.01245 (19)0.00252 (16)0.00080 (15)0.00018 (15)
S20.0180 (2)0.0133 (2)0.0166 (2)0.00165 (15)0.00262 (15)0.00067 (15)
O10.0367 (7)0.0210 (7)0.0332 (7)0.0076 (5)0.0084 (6)0.0089 (6)
O20.0249 (7)0.0301 (8)0.0672 (11)0.0091 (6)0.0033 (7)0.0059 (7)
O30.0429 (8)0.0386 (8)0.0332 (8)0.0044 (6)0.0223 (7)0.0082 (6)
O40.0317 (7)0.0245 (7)0.0378 (8)0.0127 (6)0.0031 (6)0.0043 (6)
O50.0450 (8)0.0307 (7)0.0149 (6)0.0051 (6)0.0088 (6)0.0003 (5)
O60.0208 (6)0.0153 (6)0.0174 (6)0.0001 (4)0.0044 (5)0.0040 (5)
C10.0178 (9)0.0233 (10)0.0224 (9)0.0015 (7)0.0059 (7)0.0028 (7)
C20.0224 (10)0.0193 (9)0.0341 (10)0.0032 (7)0.0069 (8)0.0000 (8)
C30.0235 (9)0.0171 (9)0.0303 (10)0.0024 (7)0.0083 (8)0.0009 (7)
C40.0229 (9)0.0187 (9)0.0152 (8)0.0021 (7)0.0007 (6)0.0022 (7)
C50.0231 (9)0.0126 (8)0.0201 (9)0.0006 (6)0.0038 (7)0.0004 (7)
C60.0242 (9)0.0216 (9)0.0190 (9)0.0043 (7)0.0100 (7)0.0081 (7)
C70.0198 (9)0.0160 (9)0.0241 (9)0.0004 (6)0.0083 (7)0.0062 (7)
C80.0216 (8)0.0162 (8)0.0117 (8)0.0048 (6)0.0002 (6)0.0015 (6)
C90.0349 (10)0.0230 (9)0.0198 (9)0.0062 (7)0.0040 (7)0.0029 (7)
C100.0465 (12)0.0260 (10)0.0241 (10)0.0026 (8)0.0007 (8)0.0094 (8)
C110.0419 (12)0.0354 (11)0.0147 (9)0.0088 (9)0.0010 (8)0.0093 (8)
C120.0296 (10)0.0450 (12)0.0175 (9)0.0072 (8)0.0078 (7)0.0010 (8)
C130.0216 (9)0.0253 (10)0.0158 (8)0.0043 (7)0.0023 (7)0.0009 (7)
C140.0170 (8)0.0127 (8)0.0148 (8)0.0018 (6)0.0008 (6)0.0007 (6)
C150.0203 (9)0.0150 (8)0.0205 (8)0.0011 (6)0.0032 (7)0.0012 (7)
C160.0294 (10)0.0226 (9)0.0215 (9)0.0025 (7)0.0014 (7)0.0079 (7)
C170.0284 (10)0.0150 (9)0.0312 (10)0.0007 (7)0.0050 (8)0.0072 (7)
C180.0252 (10)0.0165 (9)0.0336 (10)0.0052 (7)0.0007 (8)0.0004 (7)
C190.0239 (9)0.0174 (9)0.0219 (9)0.0002 (7)0.0040 (7)0.0006 (7)
C200.0152 (8)0.0194 (9)0.0150 (8)0.0009 (6)0.0005 (6)0.0022 (6)
C210.0318 (10)0.0195 (9)0.0186 (9)0.0011 (7)0.0021 (7)0.0014 (7)
C220.0524 (13)0.0205 (10)0.0243 (10)0.0032 (8)0.0018 (9)0.0067 (8)
C230.0390 (11)0.0365 (11)0.0164 (9)0.0011 (8)0.0022 (8)0.0093 (8)
C240.0270 (10)0.0329 (11)0.0170 (9)0.0052 (8)0.0028 (7)0.0006 (7)
C250.0240 (9)0.0211 (9)0.0186 (8)0.0040 (7)0.0012 (7)0.0015 (7)
C260.0156 (8)0.0138 (8)0.0171 (8)0.0016 (6)0.0011 (6)0.0003 (6)
C270.0192 (8)0.0180 (9)0.0179 (8)0.0032 (6)0.0018 (6)0.0001 (7)
C280.0196 (9)0.0245 (9)0.0239 (9)0.0035 (7)0.0057 (7)0.0054 (7)
C290.0183 (9)0.0213 (9)0.0348 (10)0.0037 (7)0.0002 (7)0.0053 (8)
C300.0247 (9)0.0248 (10)0.0282 (10)0.0065 (7)0.0019 (8)0.0062 (8)
C310.0220 (9)0.0231 (9)0.0197 (9)0.0006 (7)0.0031 (7)0.0022 (7)
Geometric parameters (Å, º) top
Fe1—C21.7855 (18)C12—C131.392 (2)
Fe1—C11.7981 (17)C12—H120.9500
Fe1—C31.8006 (18)C13—H130.9500
Fe1—S12.2484 (6)C14—C151.391 (2)
Fe1—S22.2495 (8)C14—C191.395 (2)
Fe1—Fe22.5275 (6)C15—C161.390 (2)
Fe2—C41.7733 (17)C15—H150.9500
Fe2—C51.7742 (17)C16—C171.378 (2)
Fe2—P12.2426 (7)C16—H160.9500
Fe2—S12.2495 (7)C17—C181.386 (2)
Fe2—S22.2530 (7)C17—H170.9500
P1—C81.8353 (16)C18—C191.386 (2)
P1—C141.8371 (16)C18—H180.9500
P1—P22.2519 (8)C19—H190.9500
P2—O61.4943 (11)C20—C211.392 (2)
P2—C201.8049 (16)C20—C251.397 (2)
P2—C261.8066 (16)C21—C221.384 (2)
S1—C61.8264 (16)C21—H210.9500
S2—C71.8219 (16)C22—C231.381 (2)
O1—C11.1461 (19)C22—H220.9500
O2—C21.145 (2)C23—C241.386 (2)
O3—C31.1414 (19)C23—H230.9500
O4—C41.1476 (18)C24—C251.382 (2)
O5—C51.1496 (19)C24—H240.9500
C6—C71.523 (2)C25—H250.9500
C6—H6A0.9900C26—C311.392 (2)
C6—H6B0.9900C26—C271.398 (2)
C7—H7A0.9900C27—C281.381 (2)
C7—H7B0.9900C27—H270.9500
C8—C91.396 (2)C28—C291.389 (2)
C8—C131.396 (2)C28—H280.9500
C9—C101.383 (2)C29—C301.383 (2)
C9—H90.9500C29—H290.9500
C10—C111.381 (2)C30—C311.379 (2)
C10—H100.9500C30—H300.9500
C11—C121.378 (3)C31—H310.9500
C11—H110.9500
C2—Fe1—C1101.48 (8)C10—C9—H9119.4
C2—Fe1—C392.93 (8)C8—C9—H9119.4
C1—Fe1—C399.62 (7)C11—C10—C9119.85 (17)
C2—Fe1—S188.39 (6)C11—C10—H10120.1
C1—Fe1—S1100.81 (5)C9—C10—H10120.1
C3—Fe1—S1158.84 (6)C12—C11—C10119.80 (16)
C2—Fe1—S2159.44 (5)C12—C11—H11120.1
C1—Fe1—S297.57 (5)C10—C11—H11120.1
C3—Fe1—S291.43 (6)C11—C12—C13120.83 (16)
S1—Fe1—S280.48 (2)C11—C12—H12119.6
C2—Fe1—Fe2103.55 (6)C13—C12—H12119.6
C1—Fe1—Fe2144.71 (5)C12—C13—C8119.83 (16)
C3—Fe1—Fe2103.51 (6)C12—C13—H13120.1
S1—Fe1—Fe255.831 (19)C8—C13—H13120.1
S2—Fe1—Fe255.91 (2)C15—C14—C19118.50 (14)
C4—Fe2—C589.47 (7)C15—C14—P1120.51 (11)
C4—Fe2—P196.70 (6)C19—C14—P1120.96 (12)
C5—Fe2—P1102.94 (5)C16—C15—C14120.49 (15)
C4—Fe2—S192.92 (5)C16—C15—H15119.8
C5—Fe2—S1157.08 (5)C14—C15—H15119.8
P1—Fe2—S199.41 (2)C17—C16—C15120.46 (16)
C4—Fe2—S2153.40 (5)C17—C16—H16119.8
C5—Fe2—S287.33 (5)C15—C16—H16119.8
P1—Fe2—S2109.75 (2)C16—C17—C18119.65 (15)
S1—Fe2—S280.385 (18)C16—C17—H17120.2
C4—Fe2—Fe199.20 (6)C18—C17—H17120.2
C5—Fe2—Fe1101.33 (5)C19—C18—C17120.06 (15)
P1—Fe2—Fe1150.983 (16)C19—C18—H18120.0
S1—Fe2—Fe155.791 (13)C17—C18—H18120.0
S2—Fe2—Fe155.79 (2)C18—C19—C14120.81 (15)
C8—P1—C14100.18 (7)C18—C19—H19119.6
C8—P1—Fe2114.85 (5)C14—C19—H19119.6
C14—P1—Fe2119.36 (5)C21—C20—C25118.86 (14)
C8—P1—P2104.48 (5)C21—C20—P2116.48 (12)
C14—P1—P2102.27 (5)C25—C20—P2124.64 (12)
Fe2—P1—P2113.64 (3)C22—C21—C20120.49 (16)
O6—P2—C20112.94 (7)C22—C21—H21119.8
O6—P2—C26111.20 (6)C20—C21—H21119.8
C20—P2—C26107.80 (7)C23—C22—C21120.24 (17)
O6—P2—P1109.43 (5)C23—C22—H22119.9
C20—P2—P1104.22 (5)C21—C22—H22119.9
C26—P2—P1111.04 (6)C22—C23—C24119.80 (16)
C6—S1—Fe1102.29 (6)C22—C23—H23120.1
C6—S1—Fe2104.41 (6)C24—C23—H23120.1
Fe1—S1—Fe268.38 (2)C25—C24—C23120.25 (16)
C7—S2—Fe1100.03 (6)C25—C24—H24119.9
C7—S2—Fe2106.78 (5)C23—C24—H24119.9
Fe1—S2—Fe268.299 (13)C24—C25—C20120.35 (16)
O1—C1—Fe1176.91 (14)C24—C25—H25119.8
O2—C2—Fe1178.68 (16)C20—C25—H25119.8
O3—C3—Fe1178.89 (16)C31—C26—C27119.05 (14)
O4—C4—Fe2175.95 (15)C31—C26—P2123.97 (12)
O5—C5—Fe2175.41 (15)C27—C26—P2116.97 (12)
C7—C6—S1112.22 (10)C28—C27—C26120.28 (15)
C7—C6—H6A109.2C28—C27—H27119.9
S1—C6—H6A109.2C26—C27—H27119.9
C7—C6—H6B109.2C27—C28—C29120.26 (15)
S1—C6—H6B109.2C27—C28—H28119.9
H6A—C6—H6B107.9C29—C28—H28119.9
C6—C7—S2111.97 (10)C30—C29—C28119.49 (15)
C6—C7—H7A109.2C30—C29—H29120.3
S2—C7—H7A109.2C28—C29—H29120.3
C6—C7—H7B109.2C31—C30—C29120.67 (16)
S2—C7—H7B109.2C31—C30—H30119.7
H7A—C7—H7B107.9C29—C30—H30119.7
C9—C8—C13118.54 (14)C30—C31—C26120.25 (15)
C9—C8—P1116.08 (12)C30—C31—H31119.9
C13—C8—P1125.37 (12)C26—C31—H31119.9
C10—C9—C8121.13 (16)
C2—Fe1—Fe2—C48.72 (8)C5—Fe2—S2—C7160.02 (8)
C1—Fe1—Fe2—C4142.75 (11)P1—Fe2—S2—C757.23 (6)
C3—Fe1—Fe2—C487.70 (7)S1—Fe2—S2—C739.40 (6)
S1—Fe1—Fe2—C487.27 (5)Fe1—Fe2—S2—C794.35 (6)
S2—Fe1—Fe2—C4170.14 (5)C4—Fe2—S2—Fe122.18 (11)
C2—Fe1—Fe2—C5100.03 (8)C5—Fe2—S2—Fe1105.64 (5)
C1—Fe1—Fe2—C5125.94 (11)P1—Fe2—S2—Fe1151.57 (2)
C3—Fe1—Fe2—C53.60 (7)S1—Fe2—S2—Fe154.945 (14)
S1—Fe1—Fe2—C5178.57 (5)C4—Fe2—C5—O570.8 (18)
S2—Fe1—Fe2—C578.83 (5)P1—Fe2—C5—O5167.5 (18)
C2—Fe1—Fe2—P1113.67 (7)S1—Fe2—C5—O525.5 (19)
C1—Fe1—Fe2—P120.35 (10)S2—Fe2—C5—O582.8 (18)
C3—Fe1—Fe2—P1149.90 (6)Fe1—Fe2—C5—O528.5 (18)
S1—Fe1—Fe2—P135.13 (3)Fe1—S1—C6—C731.06 (12)
S2—Fe1—Fe2—P167.46 (4)Fe2—S1—C6—C739.46 (12)
C2—Fe1—Fe2—S178.54 (6)S1—C6—C7—S28.36 (15)
C1—Fe1—Fe2—S155.48 (9)Fe1—S2—C7—C643.88 (11)
C3—Fe1—Fe2—S1174.97 (6)Fe2—S2—C7—C626.31 (12)
S2—Fe1—Fe2—S1102.59 (2)C14—P1—C8—C960.76 (14)
C2—Fe1—Fe2—S2178.86 (6)Fe2—P1—C8—C968.45 (13)
C1—Fe1—Fe2—S247.11 (9)P2—P1—C8—C9166.39 (12)
C3—Fe1—Fe2—S282.44 (5)C14—P1—C8—C13117.87 (14)
S1—Fe1—Fe2—S2102.59 (2)Fe2—P1—C8—C13112.92 (13)
C4—Fe2—P1—C873.60 (8)P2—P1—C8—C1312.24 (14)
C5—Fe2—P1—C8164.59 (8)C13—C8—C9—C101.0 (3)
S1—Fe2—P1—C820.50 (6)P1—C8—C9—C10177.70 (14)
S2—Fe2—P1—C8103.59 (6)C8—C9—C10—C110.2 (3)
Fe1—Fe2—P1—C849.34 (7)C9—C10—C11—C121.2 (3)
C4—Fe2—P1—C1445.35 (8)C10—C11—C12—C131.1 (3)
C5—Fe2—P1—C1445.64 (8)C11—C12—C13—C80.2 (3)
S1—Fe2—P1—C14139.45 (6)C9—C8—C13—C121.2 (2)
S2—Fe2—P1—C14137.46 (6)P1—C8—C13—C12177.41 (13)
Fe1—Fe2—P1—C14168.29 (6)C8—P1—C14—C15147.58 (13)
C4—Fe2—P1—P2166.17 (5)Fe2—P1—C14—C1521.35 (15)
C5—Fe2—P1—P275.18 (5)P2—P1—C14—C15105.03 (13)
S1—Fe2—P1—P299.72 (2)C8—P1—C14—C1934.57 (14)
S2—Fe2—P1—P216.64 (3)Fe2—P1—C14—C19160.80 (11)
Fe1—Fe2—P1—P270.88 (4)P2—P1—C14—C1972.82 (13)
C8—P1—P2—O656.30 (7)C19—C14—C15—C162.3 (2)
C14—P1—P2—O6160.36 (6)P1—C14—C15—C16175.62 (12)
Fe2—P1—P2—O669.63 (5)C14—C15—C16—C171.5 (2)
C8—P1—P2—C20177.36 (7)C15—C16—C17—C180.0 (3)
C14—P1—P2—C2078.58 (7)C16—C17—C18—C190.5 (3)
Fe2—P1—P2—C2051.43 (6)C17—C18—C19—C140.4 (3)
C8—P1—P2—C2666.83 (7)C15—C14—C19—C181.7 (2)
C14—P1—P2—C2637.23 (7)P1—C14—C19—C18176.14 (13)
Fe2—P1—P2—C26167.24 (5)O6—P2—C20—C218.73 (15)
C2—Fe1—S1—C6151.58 (8)C26—P2—C20—C21114.53 (13)
C1—Fe1—S1—C650.20 (8)P1—P2—C20—C21127.42 (12)
C3—Fe1—S1—C6114.47 (16)O6—P2—C20—C25169.59 (13)
S2—Fe1—S1—C645.77 (6)C26—P2—C20—C2567.16 (15)
Fe2—Fe1—S1—C6100.81 (6)P1—P2—C20—C2550.90 (14)
C2—Fe1—S1—Fe2107.60 (6)C25—C20—C21—C220.8 (2)
C1—Fe1—S1—Fe2151.01 (5)P2—C20—C21—C22179.23 (14)
C3—Fe1—S1—Fe213.65 (15)C20—C21—C22—C231.6 (3)
S2—Fe1—S1—Fe255.042 (18)C21—C22—C23—C241.0 (3)
C4—Fe2—S1—C6163.12 (7)C22—C23—C24—C250.3 (3)
C5—Fe2—S1—C6101.33 (14)C23—C24—C25—C201.1 (3)
P1—Fe2—S1—C665.83 (6)C21—C20—C25—C240.5 (2)
S2—Fe2—S1—C642.79 (5)P2—C20—C25—C24177.80 (13)
Fe1—Fe2—S1—C697.73 (6)O6—P2—C26—C31159.14 (13)
C4—Fe2—S1—Fe199.14 (6)C20—P2—C26—C3134.83 (16)
C5—Fe2—S1—Fe13.59 (13)P1—P2—C26—C3178.75 (14)
P1—Fe2—S1—Fe1163.565 (15)O6—P2—C26—C2719.76 (14)
S2—Fe2—S1—Fe154.94 (2)C20—P2—C26—C27144.07 (12)
C2—Fe1—S2—C7107.34 (17)P1—P2—C26—C27102.35 (12)
C1—Fe1—S2—C750.53 (7)C31—C26—C27—C280.1 (2)
C3—Fe1—S2—C7150.43 (7)P2—C26—C27—C28179.03 (12)
S1—Fe1—S2—C749.23 (5)C26—C27—C28—C290.1 (2)
Fe2—Fe1—S2—C7104.19 (5)C27—C28—C29—C300.3 (2)
C2—Fe1—S2—Fe23.15 (16)C28—C29—C30—C310.3 (3)
C1—Fe1—S2—Fe2154.72 (5)C29—C30—C31—C260.1 (3)
C3—Fe1—S2—Fe2105.38 (5)C27—C26—C31—C300.1 (2)
S1—Fe1—S2—Fe254.960 (17)P2—C26—C31—C30178.96 (13)
C4—Fe2—S2—C7116.53 (12)

Experimental details

Crystal data
Chemical formula[Fe2(C2H4S2)(C24H20OP2)(CO)5]
Mr730.26
Crystal system, space groupMonoclinic, P21/n
Temperature (K)113
a, b, c (Å)13.865 (4), 15.398 (4), 14.459 (5)
β (°) 98.357 (4)
V3)3054.1 (16)
Z4
Radiation typeMo Kα
µ (mm1)1.24
Crystal size (mm)0.20 × 0.18 × 0.10
Data collection
DiffractometerRigaku Saturn724 CCD
diffractometer
Absorption correctionMulti-scan
(CrystalClear; Rigaku/MSC, 2005)
Tmin, Tmax0.790, 0.886
No. of measured, independent and
observed [I > 2σ(I)] reflections
31351, 7281, 6102
Rint0.039
(sin θ/λ)max1)0.658
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.059, 1.06
No. of reflections7281
No. of parameters388
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.36, 0.36

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—C21.7855 (18)Fe2—C41.7733 (17)
Fe1—C11.7981 (17)Fe2—C51.7742 (17)
Fe1—C31.8006 (18)Fe2—P12.2426 (7)
Fe1—S12.2484 (6)Fe2—S12.2495 (7)
Fe1—S22.2495 (8)Fe2—S22.2530 (7)
 

Acknowledgements

This work was supported by the Ningbo petrochemical application-oriented base projects (Jd080109 and Jd090110).

References

First citationRigaku/MSC (2005). CrystalClear and CrystalStructure. Rigaku/MSC Inc. The Woodlands, Texas, USA.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
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
First citationWang, N., Wang, M., Liu, J., Jin, K., Chen, L. & Sun, L. (2009). Inorg. Chem. 48, 11551–11558.  Web of Science CSD CrossRef CAS PubMed Google Scholar
First citationYin, B. S., Li, T. B. & Yang, M. S. (2011). J. Coord. Chem. 64, 2066–2074.  Web of Science CSD CrossRef CAS Google Scholar

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