supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportsimilar papers Open access

hy2242 scheme

Acta Cryst. (2009). E65, m1542    [ doi:10.1107/S1600536809045735 ]

Tri-[mu]-ethanethiolato-bis{[[eta]5-1,2,3,4-tetramethyl-5-(trimethylsilyl)cyclopentadienyl]iron(II,III)}(FeII-FeIII)

J. Li

Abstract top

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.

Comment top

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.

Related literature top

For related diiron clusters, [Cp*Fe(µ-SR)3FeCp*] (Cp* = η5-C5Me5, R = Me, Et and Ph) and [CpFe(µ-SMe)3FeCp] (Cp = η5-C5H5), see: Chen et al. (2008a,b); Madec et al. (1999).

Experimental top

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 top

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).

Computing details top

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); 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 molecular structure of the title compound, showing displacement ellipsoids at the 30% probability level.
[Figure 2] Fig. 2. Packing diagram viewed along the a axis.
Tri-µ-ethanethiolato-bis{[η5-1,2,3,4-tetramethyl-5- (trimethylsilyl)cyclopentadienyl]iron(II,III)}(FeII–FeIII) top
Crystal data top
[Fe2(C2H5S)3(C12H21Si)2]F(000) = 2920
Mr = 681.82Dx = 1.253 Mg m−3
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 mm−1
c = 20.493 (2) ÅT = 293 K
V = 7226.2 (13) Å3Prism, violet-red
Z = 80.55 × 0.43 × 0.21 mm
Data collection top
Bruker SMART APEX CCD
diffractometer		6541 independent reflections
Radiation source: fine-focus sealed tube4961 reflections with I > 2σ(I)
graphiteRint = 0.055
φ 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 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)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095H-atom parameters constrained
S = 1.02 w = 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 Å−3
0 restraintsΔρmin = −0.25 e Å−3
Crystal data top
[Fe2(C2H5S)3(C12H21Si)2]V = 7226.2 (13) Å3
Mr = 681.82Z = 8
Orthorhombic, PbcaMo Kα radiation
a = 17.7426 (19) ŵ = 1.06 mm−1
b = 19.874 (2) ÅT = 293 K
c = 20.493 (2) Å0.55 × 0.43 × 0.21 mm
Data collection top
Bruker SMART APEX CCD
diffractometer		6541 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		4961 reflections with I > 2σ(I)
Tmin = 0.593, Tmax = 0.808Rint = 0.055
43018 measured reflectionsθmax = 25.3°
Refinement top
R[F2 > 2σ(F2)] = 0.034H-atom parameters constrained
wR(F2) = 0.095Δρmax = 0.45 e Å−3
S = 1.02Δρmin = −0.25 e Å−3
6541 reflectionsAbsolute structure: ?
334 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
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) top
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, °) top
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
Table 1
Selected geometric parameters (Å) top
Fe1—C132.104 (2)Fe2—C22.113 (2)
Fe1—C142.111 (2)Fe2—C32.125 (2)
Fe1—C152.126 (3)Fe2—C42.135 (2)
Fe1—C162.136 (3)Fe2—C52.126 (2)
Fe1—C172.123 (2)Fe2—S12.2659 (7)
Fe1—S12.2721 (7)Fe2—S22.2723 (7)
Fe1—S22.2765 (7)Fe2—S32.2545 (7)
Fe1—S32.2522 (7)Fe1—Fe22.7842 (5)
Fe2—C12.109 (2)
Acknowledgements top

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

references
References top

Bruker (2007). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.

Chen, Y.-H., Zhou, Y.-H., Chen, P.-P., Tao, Y.-S., Li, Y. & Qu, J.-P. (2008a). J. Am. Chem. Soc. 130, 15250–15251.

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.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.