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Acta Crystallogr Sect E Struct Rep Online. 2009 December 1; 65(Pt 12): m1542.
Published online 2009 November 7. doi:  10.1107/S1600536809045735
PMCID: PMC2972053

Tri-μ-ethanethiol­ato-bis­{[η5-1,2,3,4-tetra­methyl-5-(trimethyl­silyl)cyclo­penta­dien­yl]iron(II,III)}(FeIIFeIII)

Abstract

The title complex, [Fe2(C2H5S)3(C12H21Si)2], has an unusual Fe2S3 core. The two 1,2,3,4-tetra­methyl-5-(trimethyl­silyl)cyclo­penta­dienyl (Cp′) ligands coordinate to the Fe atoms with their C5 planes perpendicular [dihedral angles = 88.23 (7) and 88.55 (7)°] to the Fe—Fe vector, building two Cp′Fe subunits. These two subunits are bridged by three thiol­ate ligands. There are no significant differences in the coordination geometries between the two Fe atoms. The short Fe—Fe distance of 2.7842 (5) Å is clear evidence of an inter­metallic bond. Such a diiron–sulfur structure might act as a model of active sites in some metalloproteins.

Related literature

For related diiron clusters, [CpFe(μ-SR)3FeCp*] (Cp = η5-C5Me5, R = Me, Et and Ph) and [CpFe(μ-SMe)3FeCp], see: Chen et al. (2008a [triangle],b [triangle]); Madec et al. (1999 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-m1542-scheme1.jpg

Experimental

Crystal data

  • [Fe2(C2H5S)3(C12H21Si)2]
  • M r = 681.82
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-65-m1542-efi1.jpg
  • a = 17.7426 (19) Å
  • b = 19.874 (2) Å
  • c = 20.493 (2) Å
  • V = 7226.2 (13) Å3
  • Z = 8
  • Mo Kα radiation
  • μ = 1.06 mm−1
  • T = 293 K
  • 0.55 × 0.43 × 0.21 mm

Data collection

  • Bruker SMART APEX CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.593, T max = 0.808
  • 43018 measured reflections
  • 6541 independent reflections
  • 4961 reflections with I > 2σ(I)
  • R int = 0.055

Refinement

  • R[F 2 > 2σ(F 2)] = 0.034
  • wR(F 2) = 0.095
  • S = 1.02
  • 6541 reflections
  • 334 parameters
  • H-atom parameters constrained
  • Δρmax = 0.45 e Å−3
  • Δρmin = −0.25 e Å−3

Data collection: SMART (Bruker, 2007 [triangle]); cell refinement: SAINT (Bruker, 2007 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Table 1
Selected bond lengths (Å)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809045735/hy2242sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809045735/hy2242Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The author is grateful for funding support (20060418) from Tianjin University of Science and Technology.

supplementary crystallographic information

Comment

As shown in Fig. 1, the title compound is a dimeric complex, in which each Fe atom is coordinated by a 1,2,3,4-tetramethyl-5-(trimethylsilyl)cyclopentadienyl (Cp') ligand and three ethanethiolate ligands. The C5 planes of the two Cp' ligands are perpendicular to the Fe—Fe vector, with angles of 1.89 (7) and 1.45 (7)° between the normals of the planes and the vector. Three thiolate ligands bridge two Fe atoms (Table 1). The plane of the three S atoms is approximately parallel to the Cp' planes with dihedral angles of 1.77 (8) and 1.55 (8)°, respectively, and bisects the Fe—Fe bond. There are no significant differences in the coordination geometries between the two Fe centers. The short Fe—Fe distance of 2.7842 (5) Å is clear evidence of intermetallic bond.

Experimental

To a stirred suspension of Cp'Li (1.28 g, 6.38 mmol) in 50 ml THF was added anhydrous FeCl2 (0.81 g, 6.38 mmol) at 0°C, followed by stirring for 1 h. The resultant olive-green [Cp'FeCl]2 solution was cooled to -78°C. Then, a suspension of LiSEt in THF, which was prepared by reaction of n-BuLi (2.20 ml, 2.9 M solution in n-hexane) and HSEt (0.48 ml, 6.38 mmol) at 0°C, was transferred via a cannula to the cooled solution of [Cp'FeCl]2. The mixture was placed in a -78°C bath for 1 h and stirred overnight as it warmed to ambient temperature. The resulting red-violet solution was evaporated to dryness, and the residue was purified by column chromatography on neutral alumina with n-hexane as the eluent to give complex [Cp'Fe(µ-SEt)3FeCp'] (yield 0.42 g, 19%) as violet microcrystalline solid. The crystals of the title complex suitable for X-ray analysis were obtained from a benzene solution layered with acetonitrile.

Refinement

H atoms were visible in difference Fourier maps and were subsequently treated as riding atoms, with C—H = 0.96 (CH3) and 0.97 (CH2) Å and with Uiso(H) = 1.2(1.5 for methyl)Ueq(C).

Figures

Fig. 1.
The molecular structure of the title compound, showing displacement ellipsoids at the 30% probability level.
Fig. 2.
Packing diagram viewed along the a axis.

Crystal data

[Fe2(C2H5S)3(C12H21Si)2]F(000) = 2920
Mr = 681.82Dx = 1.253 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 6361 reflections
a = 17.7426 (19) Åθ = 2.3–25.3°
b = 19.874 (2) ŵ = 1.06 mm1
c = 20.493 (2) ÅT = 293 K
V = 7226.2 (13) Å3Prism, violet-red
Z = 80.55 × 0.43 × 0.21 mm

Data collection

Bruker SMART APEX CCD diffractometer6541 independent reflections
Radiation source: fine-focus sealed tube4961 reflections with I > 2σ(I)
graphiteRint = 0.055
[var phi] and ω scansθmax = 25.3°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −21→21
Tmin = 0.593, Tmax = 0.808k = −23→23
43018 measured reflectionsl = −24→24

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095H-atom parameters constrained
S = 1.02w = 1/[σ2(Fo2) + (0.0482P)2 + 2.1955P] where P = (Fo2 + 2Fc2)/3
6541 reflections(Δ/σ)max = 0.001
334 parametersΔρmax = 0.45 e Å3
0 restraintsΔρmin = −0.25 e Å3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Fe10.736349 (19)0.186763 (16)0.096497 (15)0.03463 (10)
Fe20.728449 (18)0.184706 (16)0.232172 (15)0.03427 (10)
S10.82127 (3)0.22827 (3)0.16907 (3)0.04064 (15)
S20.74171 (4)0.09562 (3)0.16363 (3)0.04026 (15)
S30.63846 (3)0.21575 (3)0.16057 (3)0.03643 (14)
Si10.60803 (5)0.08543 (4)0.00400 (4)0.0579 (2)
Si20.60737 (5)0.06522 (4)0.31233 (4)0.0592 (2)
C10.67711 (15)0.13606 (13)0.31210 (11)0.0447 (6)
C20.75840 (15)0.13379 (14)0.31891 (12)0.0473 (6)
C30.78633 (16)0.20045 (16)0.32168 (12)0.0523 (7)
C40.72446 (16)0.24564 (14)0.31789 (12)0.0493 (6)
C50.65749 (15)0.20626 (13)0.31313 (11)0.0457 (6)
C60.6515 (3)−0.01943 (17)0.3035 (2)0.0983 (13)
H6A0.6130−0.05330.30400.147*
H6B0.6857−0.02700.33910.147*
H6C0.6786−0.02150.26300.147*
C70.5588 (2)0.0664 (2)0.39283 (18)0.0925 (12)
H7A0.52260.03060.39460.139*
H7B0.53360.10870.39850.139*
H7C0.59520.06050.42700.139*
C80.5375 (2)0.0728 (2)0.24510 (19)0.0990 (13)
H8A0.50300.03560.24700.149*
H8B0.56330.07240.20390.149*
H8C0.51020.11420.24970.149*
C90.8061 (2)0.07234 (18)0.33032 (15)0.0738 (10)
H9A0.80830.06290.37620.111*
H9B0.85620.08030.31420.111*
H9C0.78450.03460.30780.111*
C100.86772 (19)0.2199 (2)0.33088 (15)0.0799 (11)
H10A0.87860.22350.37660.120*
H10B0.87690.26250.31020.120*
H10C0.89950.18620.31170.120*
C110.7284 (2)0.32007 (16)0.33017 (15)0.0752 (11)
H11A0.72510.32850.37620.113*
H11B0.68730.34200.30830.113*
H11C0.77530.33730.31380.113*
C120.57926 (17)0.23407 (16)0.31318 (14)0.0616 (8)
H12A0.56170.23810.35730.092*
H12B0.54660.20440.28940.092*
H12C0.57920.27760.29290.092*
C130.68795 (15)0.14699 (12)0.01108 (11)0.0445 (6)
C140.76750 (16)0.13311 (15)0.01178 (12)0.0513 (7)
C150.80807 (16)0.19429 (16)0.01372 (12)0.0558 (7)
C160.75472 (18)0.24840 (15)0.01263 (12)0.0540 (7)
C170.68159 (16)0.21948 (13)0.01000 (11)0.0472 (6)
C180.6325 (3)0.00125 (19)0.0373 (2)0.1132 (17)
H18A0.6769−0.01530.01590.170*
H18B0.5915−0.02930.02970.170*
H18C0.64170.00480.08330.170*
C190.5210 (2)0.1144 (2)0.0469 (2)0.1054 (15)
H19A0.48200.08130.04180.158*
H19B0.50460.15630.02850.158*
H19C0.53170.12050.09250.158*
C200.58613 (19)0.07463 (16)−0.08434 (14)0.0691 (9)
H20A0.63030.0592−0.10680.104*
H20B0.57040.1169−0.10240.104*
H20C0.54640.0422−0.08930.104*
C210.8032 (2)0.06465 (18)0.00316 (16)0.0859 (11)
H21A0.80980.0556−0.04250.129*
H21B0.77110.03090.02200.129*
H21C0.85130.06390.02450.129*
C220.89283 (18)0.2019 (2)0.01279 (16)0.0888 (12)
H22A0.91010.2038−0.03160.133*
H22B0.91550.16410.03440.133*
H22C0.90670.24260.03500.133*
C230.7726 (2)0.32161 (17)0.00420 (16)0.0849 (12)
H23A0.77740.3317−0.04140.127*
H23B0.81910.33180.02600.127*
H23C0.73280.34820.02260.127*
C240.61042 (19)0.25890 (17)0.00099 (15)0.0740 (9)
H24A0.60110.2652−0.04480.111*
H24B0.61540.30190.02180.111*
H24C0.56910.23480.02020.111*
C250.82319 (17)0.32059 (13)0.17175 (14)0.0532 (7)
H25A0.79060.33830.13790.064*
H25B0.80390.33580.21350.064*
C260.90144 (19)0.34718 (17)0.16224 (19)0.0828 (11)
H26A0.90060.39540.16390.124*
H26B0.92030.33280.12060.124*
H26C0.93360.33030.19620.124*
C270.83986 (17)0.06546 (14)0.16658 (14)0.0586 (7)
H27A0.86700.08210.12880.070*
H27B0.86430.08310.20530.070*
C280.8435 (2)−0.01107 (17)0.1676 (2)0.0931 (13)
H28A0.8953−0.02520.16920.140*
H28B0.8202−0.02860.12900.140*
H28C0.8175−0.02760.20540.140*
C290.62541 (15)0.30762 (12)0.16122 (13)0.0470 (6)
H29A0.64730.32610.20070.056*
H29B0.65150.32720.12420.056*
C300.54183 (17)0.32631 (15)0.15798 (17)0.0676 (9)
H30A0.53670.37440.15840.101*
H30B0.51610.30760.19500.101*
H30C0.52030.30860.11860.101*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Fe10.0387 (2)0.03572 (19)0.02946 (18)−0.00254 (14)0.00126 (13)−0.00052 (13)
Fe20.0365 (2)0.03658 (19)0.02974 (18)−0.00070 (14)−0.00060 (13)−0.00037 (13)
S10.0380 (3)0.0448 (3)0.0391 (3)−0.0054 (3)0.0007 (3)−0.0013 (2)
S20.0494 (4)0.0343 (3)0.0371 (3)0.0012 (3)−0.0001 (3)−0.0009 (2)
S30.0367 (3)0.0374 (3)0.0351 (3)0.0004 (2)−0.0010 (2)0.0004 (2)
Si10.0693 (5)0.0598 (5)0.0447 (4)−0.0209 (4)−0.0060 (4)−0.0041 (3)
Si20.0644 (5)0.0614 (5)0.0518 (5)−0.0157 (4)0.0047 (4)0.0094 (4)
C10.0519 (16)0.0523 (15)0.0298 (12)−0.0016 (12)0.0021 (11)0.0045 (10)
C20.0490 (15)0.0613 (17)0.0315 (12)0.0037 (13)−0.0039 (11)0.0073 (11)
C30.0518 (16)0.0732 (19)0.0318 (13)−0.0079 (15)−0.0071 (11)−0.0038 (12)
C40.0638 (18)0.0518 (15)0.0323 (12)−0.0061 (14)0.0031 (12)−0.0078 (11)
C50.0519 (16)0.0539 (15)0.0313 (12)0.0043 (13)0.0066 (11)−0.0011 (11)
C60.132 (4)0.057 (2)0.106 (3)−0.017 (2)0.020 (3)−0.0030 (19)
C70.100 (3)0.099 (3)0.078 (2)−0.024 (2)0.031 (2)0.015 (2)
C80.087 (3)0.117 (3)0.093 (3)−0.050 (2)−0.022 (2)0.021 (2)
C90.076 (2)0.087 (2)0.0587 (19)0.0257 (19)−0.0049 (16)0.0209 (16)
C100.058 (2)0.128 (3)0.0535 (18)−0.026 (2)−0.0131 (15)−0.0047 (19)
C110.113 (3)0.0591 (19)0.0535 (19)−0.0160 (18)0.0105 (17)−0.0199 (14)
C120.0612 (18)0.0756 (19)0.0480 (15)0.0186 (16)0.0116 (14)−0.0002 (14)
C130.0559 (16)0.0465 (14)0.0312 (12)−0.0038 (12)−0.0022 (11)−0.0059 (10)
C140.0590 (18)0.0614 (17)0.0336 (13)0.0050 (14)0.0056 (12)−0.0072 (12)
C150.0519 (17)0.083 (2)0.0326 (13)−0.0102 (15)0.0078 (12)−0.0002 (13)
C160.077 (2)0.0521 (16)0.0330 (13)−0.0184 (15)0.0013 (13)0.0045 (12)
C170.0601 (17)0.0506 (14)0.0307 (12)−0.0005 (13)−0.0033 (11)0.0040 (11)
C180.152 (4)0.072 (2)0.116 (3)−0.049 (3)−0.061 (3)0.032 (2)
C190.080 (3)0.135 (4)0.101 (3)−0.051 (3)0.024 (2)−0.045 (3)
C200.083 (2)0.069 (2)0.0545 (17)−0.0225 (17)−0.0116 (16)−0.0048 (14)
C210.109 (3)0.088 (2)0.061 (2)0.038 (2)0.0071 (19)−0.0238 (18)
C220.055 (2)0.154 (4)0.0571 (19)−0.022 (2)0.0145 (16)0.000 (2)
C230.137 (4)0.066 (2)0.0508 (19)−0.037 (2)0.0057 (19)0.0144 (15)
C240.088 (2)0.078 (2)0.0553 (18)0.0249 (19)−0.0211 (17)0.0074 (15)
C250.0558 (17)0.0467 (14)0.0571 (17)−0.0115 (13)0.0026 (13)−0.0053 (12)
C260.059 (2)0.061 (2)0.128 (3)−0.0248 (17)−0.0004 (19)0.0077 (19)
C270.0600 (18)0.0551 (16)0.0606 (18)0.0218 (14)0.0013 (14)−0.0018 (13)
C280.106 (3)0.057 (2)0.116 (3)0.035 (2)0.000 (2)−0.0008 (19)
C290.0433 (14)0.0387 (13)0.0589 (16)0.0031 (11)−0.0022 (12)−0.0003 (11)
C300.0507 (18)0.0540 (17)0.098 (3)0.0115 (14)−0.0022 (16)0.0028 (16)

Geometric parameters (Å, °)

Fe1—C132.104 (2)C11—H11B0.9600
Fe1—C142.111 (2)C11—H11C0.9600
Fe1—C152.126 (3)C12—H12A0.9600
Fe1—C162.136 (3)C12—H12B0.9600
Fe1—C172.123 (2)C12—H12C0.9600
Fe1—S12.2721 (7)C13—C141.438 (4)
Fe1—S22.2765 (7)C13—C171.445 (4)
Fe1—S32.2522 (7)C14—C151.414 (4)
Fe2—C12.109 (2)C14—C211.511 (4)
Fe2—C22.113 (2)C15—C161.433 (4)
Fe2—C32.125 (2)C15—C221.512 (4)
Fe2—C42.135 (2)C16—C171.420 (4)
Fe2—C52.126 (2)C16—C231.499 (4)
Fe2—S12.2659 (7)C17—C241.497 (4)
Fe2—S22.2723 (7)C18—H18A0.9600
Fe2—S32.2545 (7)C18—H18B0.9600
Fe1—Fe22.7842 (5)C18—H18C0.9600
S1—C251.836 (3)C19—H19A0.9600
S2—C271.843 (3)C19—H19B0.9600
S3—C291.841 (2)C19—H19C0.9600
Si1—C181.858 (4)C20—H20A0.9600
Si1—C201.864 (3)C20—H20B0.9600
Si1—C191.867 (4)C20—H20C0.9600
Si1—C131.878 (3)C21—H21A0.9600
Si2—C81.859 (4)C21—H21B0.9600
Si2—C71.861 (3)C21—H21C0.9600
Si2—C61.865 (4)C22—H22A0.9600
Si2—C11.874 (3)C22—H22B0.9600
C1—C51.438 (4)C22—H22C0.9600
C1—C21.450 (4)C23—H23A0.9600
C2—C31.416 (4)C23—H23B0.9600
C2—C91.505 (4)C23—H23C0.9600
C3—C41.421 (4)C24—H24A0.9600
C3—C101.507 (4)C24—H24B0.9600
C4—C51.426 (4)C24—H24C0.9600
C4—C111.502 (4)C25—C261.498 (4)
C5—C121.494 (4)C25—H25A0.9700
C6—H6A0.9600C25—H25B0.9700
C6—H6B0.9600C26—H26A0.9600
C6—H6C0.9600C26—H26B0.9600
C7—H7A0.9600C26—H26C0.9600
C7—H7B0.9600C27—C281.522 (4)
C7—H7C0.9600C27—H27A0.9700
C8—H8A0.9600C27—H27B0.9700
C8—H8B0.9600C28—H28A0.9600
C8—H8C0.9600C28—H28B0.9600
C9—H9A0.9600C28—H28C0.9600
C9—H9B0.9600C29—C301.530 (4)
C9—H9C0.9600C29—H29A0.9700
C10—H10A0.9600C29—H29B0.9700
C10—H10B0.9600C30—H30A0.9600
C10—H10C0.9600C30—H30B0.9600
C11—H11A0.9600C30—H30C0.9600
C13—Fe1—C1439.90 (10)H8A—C8—H8B109.5
C13—Fe1—C1739.98 (10)Si2—C8—H8C109.5
C14—Fe1—C1765.67 (10)H8A—C8—H8C109.5
C13—Fe1—C1566.85 (10)H8B—C8—H8C109.5
C14—Fe1—C1538.98 (11)C2—C9—H9A109.5
C17—Fe1—C1565.56 (11)C2—C9—H9B109.5
C13—Fe1—C1666.94 (10)H9A—C9—H9B109.5
C14—Fe1—C1665.66 (11)C2—C9—H9C109.5
C17—Fe1—C1638.96 (10)H9A—C9—H9C109.5
C15—Fe1—C1639.29 (12)H9B—C9—H9C109.5
C13—Fe1—S3105.45 (7)C3—C10—H10A109.5
C14—Fe1—S3144.15 (8)C3—C10—H10B109.5
C17—Fe1—S393.18 (8)H10A—C10—H10B109.5
C15—Fe1—S3155.34 (9)C3—C10—H10C109.5
C16—Fe1—S3116.12 (9)H10A—C10—H10C109.5
C13—Fe1—S1162.12 (7)H10B—C10—H10C109.5
C14—Fe1—S1123.23 (8)C4—C11—H11A109.5
C17—Fe1—S1137.62 (7)C4—C11—H11B109.5
C15—Fe1—S195.73 (8)H11A—C11—H11B109.5
C16—Fe1—S1102.55 (8)C4—C11—H11C109.5
S3—Fe1—S192.12 (3)H11A—C11—H11C109.5
C13—Fe1—S2102.76 (7)H11B—C11—H11C109.5
C14—Fe1—S294.83 (8)C5—C12—H12A109.5
C17—Fe1—S2140.11 (7)C5—C12—H12B109.5
C15—Fe1—S2120.88 (9)H12A—C12—H12B109.5
C16—Fe1—S2159.45 (9)C5—C12—H12C109.5
S3—Fe1—S283.31 (2)H12A—C12—H12C109.5
S1—Fe1—S282.28 (2)H12B—C12—H12C109.5
C13—Fe1—Fe2143.59 (7)C14—C13—C17105.5 (2)
C14—Fe1—Fe2145.80 (8)C14—C13—Si1128.1 (2)
C17—Fe1—Fe2144.60 (7)C17—C13—Si1126.1 (2)
C15—Fe1—Fe2145.90 (8)C14—C13—Fe170.31 (14)
C16—Fe1—Fe2145.06 (8)C17—C13—Fe170.73 (13)
S3—Fe1—Fe251.882 (17)Si1—C13—Fe1128.11 (13)
S1—Fe1—Fe252.053 (18)C15—C14—C13109.6 (2)
S2—Fe1—Fe252.191 (17)C15—C14—C21124.4 (3)
C1—Fe2—C240.17 (10)C13—C14—C21125.6 (3)
C1—Fe2—C366.79 (11)C15—C14—Fe171.08 (15)
C2—Fe2—C339.02 (11)C13—C14—Fe169.78 (13)
C1—Fe2—C539.70 (10)C21—C14—Fe1131.4 (2)
C2—Fe2—C565.74 (10)C14—C15—C16108.0 (2)
C3—Fe2—C565.35 (11)C14—C15—C22126.3 (3)
C1—Fe2—C466.83 (10)C16—C15—C22125.6 (3)
C2—Fe2—C465.66 (11)C14—C15—Fe169.94 (14)
C3—Fe2—C438.95 (11)C16—C15—Fe170.72 (15)
C5—Fe2—C439.10 (10)C22—C15—Fe1127.8 (2)
C1—Fe2—S3108.97 (7)C17—C16—C15107.5 (2)
C2—Fe2—S3148.93 (8)C17—C16—C23125.6 (3)
C3—Fe2—S3149.72 (9)C15—C16—C23126.2 (3)
C5—Fe2—S391.91 (7)C17—C16—Fe170.06 (14)
C4—Fe2—S3110.91 (8)C15—C16—Fe169.99 (15)
C1—Fe2—S1158.81 (7)C23—C16—Fe1133.0 (2)
C2—Fe2—S1118.70 (8)C16—C17—C13109.4 (2)
C3—Fe2—S194.88 (8)C16—C17—C24124.3 (3)
C5—Fe2—S1143.01 (8)C13—C17—C24126.1 (3)
C4—Fe2—S1106.08 (8)C16—C17—Fe170.99 (15)
S3—Fe2—S192.22 (3)C13—C17—Fe169.28 (13)
C1—Fe2—S299.65 (7)C24—C17—Fe1130.47 (19)
C2—Fe2—S296.94 (8)Si1—C18—H18A109.5
C3—Fe2—S2126.74 (9)Si1—C18—H18B109.5
C5—Fe2—S2134.48 (8)H18A—C18—H18B109.5
C4—Fe2—S2162.58 (8)Si1—C18—H18C109.5
S3—Fe2—S283.35 (2)H18A—C18—H18C109.5
S1—Fe2—S282.51 (2)H18B—C18—H18C109.5
C1—Fe2—Fe1143.52 (7)Si1—C19—H19A109.5
C2—Fe2—Fe1146.54 (8)Si1—C19—H19B109.5
C3—Fe2—Fe1146.66 (8)H19A—C19—H19B109.5
C5—Fe2—Fe1143.71 (7)Si1—C19—H19C109.5
C4—Fe2—Fe1144.59 (8)H19A—C19—H19C109.5
S3—Fe2—Fe151.807 (18)H19B—C19—H19C109.5
S1—Fe2—Fe152.256 (17)Si1—C20—H20A109.5
S2—Fe2—Fe152.330 (18)Si1—C20—H20B109.5
C25—S1—Fe2112.23 (9)H20A—C20—H20B109.5
C25—S1—Fe1113.25 (10)Si1—C20—H20C109.5
Fe2—S1—Fe175.69 (2)H20A—C20—H20C109.5
C27—S2—Fe2109.33 (10)H20B—C20—H20C109.5
C27—S2—Fe1108.55 (10)C14—C21—H21A109.5
Fe2—S2—Fe175.48 (2)C14—C21—H21B109.5
C29—S3—Fe1110.79 (9)H21A—C21—H21B109.5
C29—S3—Fe2110.84 (9)C14—C21—H21C109.5
Fe1—S3—Fe276.31 (2)H21A—C21—H21C109.5
C18—Si1—C20107.53 (17)H21B—C21—H21C109.5
C18—Si1—C19107.3 (2)C15—C22—H22A109.5
C20—Si1—C19108.69 (18)C15—C22—H22B109.5
C18—Si1—C13112.45 (16)H22A—C22—H22B109.5
C20—Si1—C13107.90 (12)C15—C22—H22C109.5
C19—Si1—C13112.76 (14)H22A—C22—H22C109.5
C8—Si2—C7110.3 (2)H22B—C22—H22C109.5
C8—Si2—C6106.3 (2)C16—C23—H23A109.5
C7—Si2—C6106.96 (18)C16—C23—H23B109.5
C8—Si2—C1112.19 (14)H23A—C23—H23B109.5
C7—Si2—C1107.36 (15)C16—C23—H23C109.5
C6—Si2—C1113.59 (16)H23A—C23—H23C109.5
C5—C1—C2105.6 (2)H23B—C23—H23C109.5
C5—C1—Si2124.7 (2)C17—C24—H24A109.5
C2—C1—Si2129.3 (2)C17—C24—H24B109.5
C5—C1—Fe270.80 (14)H24A—C24—H24B109.5
C2—C1—Fe270.08 (14)C17—C24—H24C109.5
Si2—C1—Fe2129.16 (13)H24A—C24—H24C109.5
C3—C2—C1108.8 (2)H24B—C24—H24C109.5
C3—C2—C9123.8 (3)C26—C25—S1111.5 (2)
C1—C2—C9126.9 (3)C26—C25—H25A109.3
C3—C2—Fe270.95 (15)S1—C25—H25A109.3
C1—C2—Fe269.75 (13)C26—C25—H25B109.3
C9—C2—Fe2131.4 (2)S1—C25—H25B109.3
C2—C3—C4108.6 (2)H25A—C25—H25B108.0
C2—C3—C10125.5 (3)C25—C26—H26A109.5
C4—C3—C10125.8 (3)C25—C26—H26B109.5
C2—C3—Fe270.03 (14)H26A—C26—H26B109.5
C4—C3—Fe270.88 (14)C25—C26—H26C109.5
C10—C3—Fe2127.51 (19)H26A—C26—H26C109.5
C3—C4—C5107.5 (2)H26B—C26—H26C109.5
C3—C4—C11125.3 (3)C28—C27—S2111.5 (3)
C5—C4—C11126.2 (3)C28—C27—H27A109.3
C3—C4—Fe270.16 (14)S2—C27—H27A109.3
C5—C4—Fe270.12 (14)C28—C27—H27B109.3
C11—C4—Fe2134.0 (2)S2—C27—H27B109.3
C4—C5—C1109.4 (2)H27A—C27—H27B108.0
C4—C5—C12124.8 (3)C27—C28—H28A109.5
C1—C5—C12125.7 (3)C27—C28—H28B109.5
C4—C5—Fe270.77 (14)H28A—C28—H28B109.5
C1—C5—Fe269.50 (13)C27—C28—H28C109.5
C12—C5—Fe2128.69 (18)H28A—C28—H28C109.5
Si2—C6—H6A109.5H28B—C28—H28C109.5
Si2—C6—H6B109.5C30—C29—S3111.25 (19)
H6A—C6—H6B109.5C30—C29—H29A109.4
Si2—C6—H6C109.5S3—C29—H29A109.4
H6A—C6—H6C109.5C30—C29—H29B109.4
H6B—C6—H6C109.5S3—C29—H29B109.4
Si2—C7—H7A109.5H29A—C29—H29B108.0
Si2—C7—H7B109.5C29—C30—H30A109.5
H7A—C7—H7B109.5C29—C30—H30B109.5
Si2—C7—H7C109.5H30A—C30—H30B109.5
H7A—C7—H7C109.5C29—C30—H30C109.5
H7B—C7—H7C109.5H30A—C30—H30C109.5
Si2—C8—H8A109.5H30B—C30—H30C109.5
Si2—C8—H8B109.5

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2242).

References

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  • Chen, Y.-H., Zhou, Y.-H. & Qu, J.-P. (2008b). Organometallics, 27, 666–671.
  • Madec, P., Muir, K. W., Pétillon, F. Y., Rumin, R., Scaon, Y., Schollhammer, P. & Talarmin, J. (1999). J. Chem. Soc. Dalton Trans. pp. 2371–2383.
  • Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
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