μ4-Sulfido-bis(μ2-phenyl­thiol­ato)­tetrakis­(tri­carbonyl­iron)

Hu, M.; Ma, C.; Zhang, X.; Fang, C.; Chen, F.; Chen, C.; Liu, Q.

doi:10.1107/S1600536803000138

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μ₄-Sulfido-bis(μ₂-phenylthiolato)tetrakis(tricarbonyliron)

M. Hu, C. Ma, X. Zhang, C. Fang, F. Chen, C. Chen and Q. Liu

The title complex, C₂₄H₁₀Fe₄O₁₂S₃, contains two Fe₂(PhS)(CO)₆ subclusters connected through an inorganic spiro μ₄-S atom. Each iron atom is coordinated by three carbonyl C atoms [Fe—C 1.786 (9)–1.826 (9) Å], one thiophenyl S atom [Fe—S 2.267 (2)–2.286 (2) Å], one μ₄–S atom [Fe—S 2.235 (2)–2.249 (2) Å], and one Fe—Fe bond [2.526 (16), 2.532 (16) Å], in a distorted octahedral geometry.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803000138/wn6131sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536803000138/wn6131Isup2.hkl Contains datablock I

CCDC reference: 204653

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.016 Å
R factor = 0.069
wR factor = 0.147
Data-to-parameter ratio = 14.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


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General Notes



FORMU_01  There is a discrepancy between the atom counts in the
          _chemical_formula_sum and _chemical_formula_moiety. This is
          usually due to the moiety formula being in the wrong format.
          Atom count from _chemical_formula_sum:   C24 H10 Fe4 O12 S3
          Atom count from _chemical_formula_moiety:

ABSTM_02  When printed, the submitted absorption T values will be replaced
          by the scaled T values. Since the ratio of scaled T's is
          identical to the ratio of reported T values, the scaling does
          not imply a change to the absorption corrections used in the
          study.
          Ratio of Tmax expected/reported      0.467
          Tmax scaled      0.467 Tmin scaled      0.326


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 60 Alert Level C = Please check

Comment top

Hydrogenases are utilized by numerous microorganisms to process hydrogen, both in the production and uptake of molecular hydrogen, in support of their metabolism. Fairly recently, crystallographic investigations of the so-called Fe-only hydrogenases discovered a six-iron H-cluster containing an Fe₂(µ-SR)₂(CN)₂(CO)₃L_n core [R is alkyl, L is H₂O], and a thiolate-linked Fe₄S₄(SR)₄ cluster. The metabolism of hydrogen is facilitated at a novel 2Fe2S center in Fe-only hydrogenase (Peters et al., 1998, Nicolet et al., 1999, Nicolet et al., 2001). To simulate the organometallic structure Fe₂(SR)₂(CN)₂(CO)₄ of the H-cluster, we repeated the preparation of Fe₂(SR)₂(CO)₆ by the reaction of Fe₃(CO)₁₂ with thiophenol, using the method of Rauchfuss (Gloaguen et al., 2001). We obtained the title compound, (I), which represents a new example of an Fe₄S₃ core cluster containing a bridging thiophenyl ligand. However, similar structures have been reported in other complexes, viz. [CH₃SFe₂(CO)₆]₂S (Coleman et al., 1967), [C₆H₉SFe₂(CO)₆]₂S (Kolobkov et al., 1986), and [EtSFe₂(CO)₆]₂S (Song et al., 1988).

Complex (I) contains two Fe₂S(CO)₆ subclusters Fe1,S2,Fe2 and Fe3,S3,Fe4, connected through the inorganic sulfur atom, µ₄-S1, as shown in Fig. 1. Each subcluster has a phenyl group, attached to µ₂-S2 and µ₂-S3, respectively. In each subcluster, two Fe atoms are bridged by the thiophenyl S, with an average Fe—S—Fe angle of 67.48 (7)° and an average Fe—S distance of 2.276 (2) Å. The Fe—Fe separations of 2.526 (16) and 2.532 (16) Å are comparable to those in the H-cluster. The central sulfur atom, S1, connects the two Fe₂S(CO)₆ fragments, with a shorter Fe—S distance, averaging 2.243 (2) Å. The Fe—S1—Fe angles, ranging from 68.44 (7)° to 138.97 (10)°, show that the Fe₄S tetrahedron is very distorted. In addition to the coordination of one thiophenyl S and one µ₄-S, the 18-electron shell of each Fe atom is completed by three terminal carbonyl groups, with an average Fe—C bond length of 1.800 (10) Å.

Experimental top

Reactions were carried out under an atmosphere of purified nitrogen, using standard Schlenk techniques. To 1 g Fe₃(CO)₁₂ suspended in 40 ml toluene was added 2 equiv. of thiophenol. The solution changed from black–green to black–red after stirring for 1 h. Stirring was continued, at 343 K, overnight; the solution was then cooled to room temperature, filtered and evaporated to dryness in vacuo. The residue was extracted with 3 x 10 ml hexane, and the combined extracts were reduced to ca 5 ml in vacuo, yielding a red crystal of (I), at 253 K.

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994); data reduction: XPREP in SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top

Fig. 1. Molecular structure of the title compound, with the atom-labeling scheme and probability displacement ellipsoids drawn at the 30% level.

Bis (mu-phenylthiodiiron-hexacarbonyl) (mu₄-sulfido) top

Crystal data top

[Fe₄C₂₄H₁₀O₁₂S₃]	F(000) = 1608
M_r = 809.90	D_x = 1.754 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 9.0026 (2) Å	Cell parameters from 4211 reflections
b = 12.9509 (4) Å	θ = 2.2–25.1°
c = 26.5409 (2) Å	µ = 2.12 mm⁻¹
β = 97.612 (1)°	T = 293 K
V = 3067.18 (12) Å³	Prism, red
Z = 4	0.50 × 0.38 × 0.36 mm

Data collection top

Siemens SMART CCD area detector diffractometer	5418 independent reflections
Radiation source: fine-focus sealed tube	4103 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.038
ϕ and ω scans	θ_max = 25.1°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→10
T_min = 0.698, T_max = 1.000	k = −10→15
9335 measured reflections	l = −31→17

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.069	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.147	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0017P)² + 30.5273P] where P = (F_o² + 2F_c²)/3
5418 reflections	(Δ/σ)_max < 0.001
388 parameters	Δρ_max = 0.52 e Å⁻³
0 restraints	Δρ_min = −0.41 e Å⁻³

Crystal data top

[Fe₄C₂₄H₁₀O₁₂S₃]	V = 3067.18 (12) Å³
M_r = 809.90	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 9.0026 (2) Å	µ = 2.12 mm⁻¹
b = 12.9509 (4) Å	T = 293 K
c = 26.5409 (2) Å	0.50 × 0.38 × 0.36 mm
β = 97.612 (1)°

Data collection top

Siemens SMART CCD area detector diffractometer	5418 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	4103 reflections with I > 2σ(I)
T_min = 0.698, T_max = 1.000	R_int = 0.038
9335 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.069	0 restraints
wR(F²) = 0.147	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.0017P)² + 30.5273P] where P = (F_o² + 2F_c²)/3
5418 reflections	Δρ_max = 0.52 e Å⁻³
388 parameters	Δρ_min = −0.41 e Å⁻³

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

	x	y	z	U_iso*/U_eq
Fe1	0.09433 (13)	0.24175 (9)	0.23918 (4)	0.0427 (3)
Fe2	−0.10971 (13)	0.37690 (9)	0.23045 (4)	0.0442 (3)
Fe3	0.18804 (13)	0.42252 (9)	0.12543 (4)	0.0429 (3)
Fe4	−0.03081 (13)	0.31485 (10)	0.08524 (4)	0.0469 (3)
S1	0.0292 (2)	0.33728 (15)	0.16897 (7)	0.0397 (4)
S2	0.1285 (2)	0.40790 (16)	0.26679 (7)	0.0458 (5)
S3	0.2084 (2)	0.25558 (16)	0.09927 (7)	0.0464 (5)
O1	−0.0556 (10)	0.0610 (6)	0.1897 (3)	0.097 (3)
O2	0.4086 (8)	0.1824 (6)	0.2350 (3)	0.087 (2)
O3	0.0586 (8)	0.1685 (5)	0.3412 (2)	0.0714 (19)
O4	−0.2400 (9)	0.3402 (6)	0.3241 (3)	0.092 (2)
O5	−0.3472 (8)	0.2529 (6)	0.1733 (3)	0.089 (2)
O6	−0.2307 (8)	0.5863 (6)	0.2104 (3)	0.086 (2)
O7	0.0450 (8)	0.6191 (5)	0.1437 (3)	0.079 (2)
O8	0.3090 (9)	0.5143 (6)	0.0386 (3)	0.099 (3)
O9	0.4564 (8)	0.4401 (5)	0.2017 (3)	0.078 (2)
O10	−0.2788 (8)	0.4590 (7)	0.0881 (3)	0.090 (2)
O11	−0.1958 (10)	0.1183 (7)	0.0711 (3)	0.109 (3)
O12	−0.0093 (10)	0.3753 (7)	−0.0196 (3)	0.100 (3)
C1	0.0040 (11)	0.1305 (7)	0.2090 (3)	0.059 (2)
C2	0.2877 (11)	0.2042 (7)	0.2362 (3)	0.054 (2)
C3	0.0739 (9)	0.1967 (6)	0.3017 (3)	0.048 (2)
C4	−0.1876 (10)	0.3564 (7)	0.2886 (3)	0.058 (2)
C5	−0.2595 (11)	0.3024 (8)	0.1962 (3)	0.059 (2)
C6	−0.1816 (10)	0.5073 (7)	0.2172 (3)	0.052 (2)
C7	0.1010 (10)	0.5427 (7)	0.1367 (3)	0.051 (2)
C8	0.2629 (11)	0.4766 (7)	0.0717 (3)	0.062 (2)
C9	0.3535 (10)	0.4330 (6)	0.1714 (4)	0.051 (2)
C10	−0.1848 (10)	0.4017 (8)	0.0861 (3)	0.058 (2)
C11	−0.1323 (12)	0.1941 (9)	0.0770 (4)	0.073 (3)
C12	−0.0176 (11)	0.3502 (8)	0.0207 (4)	0.065 (3)
C13	0.1567 (11)	0.4226 (6)	0.3344 (3)	0.056 (2)
C14	0.2785 (14)	0.3759 (9)	0.3613 (4)	0.088 (4)
H14A	0.3412	0.3342	0.3448	0.105*
C15	0.3077 (18)	0.3913 (11)	0.4136 (5)	0.113 (5)
H15A	0.3883	0.3583	0.4325	0.136*
C16	0.220 (2)	0.4537 (12)	0.4365 (5)	0.114 (5)
H16A	0.2414	0.4643	0.4714	0.137*
C17	0.0994 (18)	0.5020 (9)	0.4109 (5)	0.100 (4)
H17A	0.0395	0.5449	0.4278	0.120*
C18	0.0666 (12)	0.4864 (7)	0.3585 (3)	0.069 (3)
H18A	−0.0154	0.5190	0.3401	0.082*
C19	0.2912 (10)	0.2437 (7)	0.0416 (3)	0.052 (2)
C20	0.4306 (11)	0.2807 (8)	0.0394 (4)	0.071 (3)
H20A	0.4822	0.3137	0.0675	0.086*
C21	0.4975 (14)	0.2699 (10)	−0.0045 (5)	0.086 (3)
H21A	0.5923	0.2969	−0.0064	0.104*
C22	0.4211 (16)	0.2186 (10)	−0.0452 (4)	0.093 (4)
H22A	0.4644	0.2125	−0.0750	0.112*
C23	0.2810 (15)	0.1758 (10)	−0.0431 (4)	0.091 (4)
H23A	0.2311	0.1398	−0.0706	0.109*
C24	0.2179 (11)	0.1883 (8)	0.0013 (3)	0.065 (3)
H24A	0.1249	0.1591	0.0040	0.078*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0523 (7)	0.0381 (6)	0.0384 (6)	0.0025 (5)	0.0089 (5)	0.0020 (5)
Fe2	0.0454 (7)	0.0475 (7)	0.0409 (6)	0.0031 (5)	0.0098 (5)	0.0005 (5)
Fe3	0.0476 (7)	0.0424 (6)	0.0392 (6)	−0.0010 (5)	0.0070 (5)	0.0046 (5)
Fe4	0.0489 (7)	0.0553 (7)	0.0356 (6)	−0.0014 (6)	0.0022 (5)	−0.0010 (5)
S1	0.0429 (11)	0.0442 (11)	0.0321 (9)	−0.0009 (9)	0.0053 (8)	0.0011 (8)
S2	0.0528 (12)	0.0438 (11)	0.0400 (10)	0.0007 (9)	0.0031 (9)	0.0003 (9)
S3	0.0533 (12)	0.0475 (12)	0.0388 (10)	0.0030 (10)	0.0078 (9)	0.0002 (9)
O1	0.145 (7)	0.062 (5)	0.081 (5)	−0.034 (5)	0.001 (5)	−0.014 (4)
O2	0.066 (5)	0.100 (6)	0.098 (6)	0.026 (4)	0.026 (4)	0.022 (5)
O3	0.108 (5)	0.063 (4)	0.047 (4)	0.001 (4)	0.026 (4)	0.011 (3)
O4	0.111 (6)	0.109 (6)	0.065 (5)	0.005 (5)	0.047 (4)	0.015 (4)
O5	0.068 (5)	0.111 (6)	0.090 (5)	−0.033 (4)	0.015 (4)	−0.027 (5)
O6	0.080 (5)	0.061 (5)	0.116 (6)	0.021 (4)	0.014 (4)	0.009 (4)
O7	0.100 (6)	0.053 (4)	0.088 (5)	0.012 (4)	0.026 (4)	−0.002 (4)
O8	0.122 (7)	0.094 (6)	0.092 (6)	0.009 (5)	0.051 (5)	0.046 (5)
O9	0.060 (4)	0.077 (5)	0.091 (5)	−0.005 (4)	−0.016 (4)	−0.005 (4)
O10	0.069 (5)	0.113 (7)	0.084 (5)	0.029 (5)	−0.005 (4)	−0.007 (5)
O11	0.125 (7)	0.094 (6)	0.103 (6)	−0.040 (6)	−0.007 (5)	−0.008 (5)
O12	0.134 (7)	0.122 (7)	0.044 (4)	0.038 (6)	0.018 (4)	0.027 (4)
C1	0.075 (6)	0.050 (5)	0.049 (5)	−0.010 (5)	0.003 (4)	−0.003 (4)
C2	0.069 (6)	0.051 (5)	0.044 (5)	0.002 (5)	0.014 (4)	0.008 (4)
C3	0.056 (5)	0.041 (5)	0.049 (5)	0.001 (4)	0.010 (4)	0.007 (4)
C4	0.065 (6)	0.058 (6)	0.051 (5)	0.006 (5)	0.005 (4)	−0.001 (4)
C5	0.056 (6)	0.072 (6)	0.053 (5)	0.001 (5)	0.019 (4)	−0.004 (5)
C6	0.052 (5)	0.049 (5)	0.054 (5)	0.005 (4)	0.006 (4)	−0.006 (4)
C7	0.059 (5)	0.046 (5)	0.049 (5)	−0.010 (4)	0.007 (4)	−0.003 (4)
C8	0.082 (7)	0.054 (6)	0.050 (5)	−0.001 (5)	0.014 (5)	0.005 (4)
C9	0.047 (5)	0.040 (5)	0.069 (6)	−0.002 (4)	0.012 (4)	0.003 (4)
C10	0.059 (6)	0.067 (6)	0.045 (5)	0.014 (5)	−0.002 (4)	0.005 (4)
C11	0.082 (7)	0.078 (7)	0.057 (6)	−0.014 (6)	0.001 (5)	−0.010 (5)
C12	0.070 (6)	0.072 (7)	0.053 (6)	0.013 (5)	0.008 (5)	0.008 (5)
C13	0.080 (6)	0.038 (5)	0.045 (5)	−0.010 (5)	−0.006 (4)	0.001 (4)
C14	0.116 (10)	0.081 (8)	0.058 (6)	−0.001 (7)	−0.020 (6)	−0.004 (6)
C15	0.162 (14)	0.085 (9)	0.075 (9)	0.002 (9)	−0.050 (9)	0.009 (7)
C16	0.191 (17)	0.089 (10)	0.057 (8)	−0.037 (11)	−0.008 (9)	−0.011 (7)
C17	0.162 (14)	0.065 (8)	0.075 (8)	−0.022 (8)	0.024 (8)	−0.021 (6)
C18	0.101 (8)	0.059 (6)	0.047 (5)	−0.009 (6)	0.012 (5)	−0.015 (5)
C19	0.056 (5)	0.052 (5)	0.050 (5)	0.011 (4)	0.009 (4)	0.003 (4)
C20	0.068 (6)	0.081 (7)	0.068 (6)	−0.003 (6)	0.019 (5)	−0.006 (5)
C21	0.077 (7)	0.108 (10)	0.080 (8)	−0.002 (7)	0.031 (6)	−0.005 (7)
C22	0.117 (10)	0.105 (10)	0.069 (7)	0.026 (8)	0.051 (7)	0.009 (7)
C23	0.123 (10)	0.101 (9)	0.050 (6)	0.019 (8)	0.018 (6)	−0.019 (6)
C24	0.074 (6)	0.068 (6)	0.056 (6)	0.007 (5)	0.016 (5)	−0.008 (5)

Geometric parameters (Å, º) top

Fe1—C3	1.791 (8)	O6—C6	1.120 (10)
Fe1—C1	1.790 (9)	O7—C7	1.136 (10)
Fe1—C2	1.820 (10)	O8—C8	1.132 (10)
Fe1—S1	2.249 (2)	O9—C9	1.146 (10)
Fe1—S2	2.281 (2)	O10—C10	1.132 (10)
Fe1—Fe2	2.5256 (16)	O11—C11	1.137 (12)
Fe2—C4	1.796 (10)	O12—C12	1.129 (10)
Fe2—C5	1.803 (10)	C13—C18	1.374 (13)
Fe2—C6	1.826 (9)	C13—C14	1.367 (13)
Fe2—S1	2.243 (2)	C14—C15	1.393 (15)
Fe2—S2	2.267 (2)	C14—H14A	0.9300
Fe3—C7	1.786 (9)	C15—C16	1.335 (19)
Fe3—C8	1.798 (9)	C15—H15A	0.9300
Fe3—C9	1.802 (9)	C16—C17	1.353 (18)
Fe3—S1	2.244 (2)	C16—H16A	0.9300
Fe3—S3	2.286 (2)	C17—C18	1.396 (14)
Fe3—Fe4	2.5313 (16)	C17—H17A	0.9300
Fe4—C12	1.793 (10)	C18—H18A	0.9300
Fe4—C10	1.787 (10)	C19—C20	1.352 (12)
Fe4—C11	1.810 (11)	C19—C24	1.381 (12)
Fe4—S1	2.235 (2)	C20—C21	1.387 (14)
Fe4—S3	2.270 (2)	C20—H20A	0.9300
S2—C13	1.790 (8)	C21—C22	1.371 (16)
S3—C19	1.795 (8)	C21—H21A	0.9300
O1—C1	1.135 (10)	C22—C23	1.386 (16)
O2—C2	1.128 (10)	C22—H22A	0.9300
O3—C3	1.135 (9)	C23—C24	1.383 (13)
O4—C4	1.128 (10)	C23—H23A	0.9300
O5—C5	1.130 (10)	C24—H24A	0.9300

C3—Fe1—C1	93.2 (4)	Fe4—S1—Fe2	131.96 (10)
C3—Fe1—C2	99.7 (4)	Fe4—S1—Fe3	68.81 (7)
C1—Fe1—C2	98.4 (4)	Fe2—S1—Fe3	135.79 (10)
C3—Fe1—S1	154.1 (3)	Fe4—S1—Fe1	138.98 (10)
C1—Fe1—S1	91.1 (3)	Fe2—S1—Fe1	68.43 (7)
C2—Fe1—S1	104.9 (3)	Fe3—S1—Fe1	125.67 (9)
C3—Fe1—S2	92.1 (3)	C13—S2—Fe2	116.5 (3)
C1—Fe1—S2	159.5 (3)	C13—S2—Fe1	114.7 (3)
C2—Fe1—S2	100.2 (3)	Fe2—S2—Fe1	67.46 (7)
S1—Fe1—S2	75.90 (8)	C19—S3—Fe4	112.4 (3)
C3—Fe1—Fe2	98.5 (3)	C19—S3—Fe3	113.5 (3)
C1—Fe1—Fe2	103.6 (3)	Fe4—S3—Fe3	67.51 (7)
C2—Fe1—Fe2	150.5 (3)	O1—C1—Fe1	178.7 (10)
S1—Fe1—Fe2	55.67 (6)	O2—C2—Fe1	178.7 (10)
S2—Fe1—Fe2	56.02 (6)	O3—C3—Fe1	178.9 (8)
C4—Fe2—C5	90.2 (4)	O4—C4—Fe2	177.1 (9)
C4—Fe2—C6	97.7 (4)	O5—C5—Fe2	175.9 (9)
C5—Fe2—C6	100.0 (4)	O6—C6—Fe2	176.8 (9)
C4—Fe2—S1	155.4 (3)	O7—C7—Fe3	179.6 (9)
C5—Fe2—S1	87.8 (3)	O8—C8—Fe3	177.4 (9)
C6—Fe2—S1	106.8 (3)	O9—C9—Fe3	178.1 (8)
C4—Fe2—S2	96.6 (3)	O10—C10—Fe4	177.2 (9)
C5—Fe2—S2	155.7 (3)	O11—C11—Fe4	179.1 (10)
C6—Fe2—S2	102.1 (3)	O12—C12—Fe4	178.1 (10)
S1—Fe2—S2	76.29 (8)	C18—C13—C14	120.4 (9)
C4—Fe2—Fe1	100.4 (3)	C18—C13—S2	121.1 (7)
C5—Fe2—Fe1	99.3 (3)	C14—C13—S2	118.2 (8)
C6—Fe2—Fe1	153.3 (3)	C13—C14—C15	119.2 (12)
S1—Fe2—Fe1	55.90 (6)	C13—C14—H14A	120.4
S2—Fe2—Fe1	56.52 (6)	C15—C14—H14A	120.4
C7—Fe3—C8	90.8 (4)	C16—C15—C14	119.8 (13)
C7—Fe3—C9	99.4 (4)	C16—C15—H15A	120.1
C8—Fe3—C9	98.3 (4)	C14—C15—H15A	120.1
C7—Fe3—S1	91.0 (3)	C15—C16—C17	122.3 (13)
C8—Fe3—S1	158.6 (3)	C15—C16—H16A	118.9
C9—Fe3—S1	102.4 (3)	C17—C16—H16A	118.9
C7—Fe3—S3	158.4 (3)	C16—C17—C18	118.9 (13)
C8—Fe3—S3	94.2 (3)	C16—C17—H17A	120.5
C9—Fe3—S3	100.6 (3)	C18—C17—H17A	120.5
S1—Fe3—S3	76.90 (8)	C13—C18—C17	119.3 (11)
C7—Fe3—Fe4	102.5 (3)	C13—C18—H18A	120.3
C8—Fe3—Fe4	103.5 (3)	C17—C18—H18A	120.3
C9—Fe3—Fe4	148.7 (3)	C20—C19—C24	120.0 (9)
S1—Fe3—Fe4	55.43 (6)	C20—C19—S3	120.0 (7)
S3—Fe3—Fe4	55.95 (6)	C24—C19—S3	119.7 (7)
C12—Fe4—C10	90.0 (4)	C19—C20—C21	120.7 (10)
C12—Fe4—C11	101.6 (5)	C19—C20—H20A	119.6
C10—Fe4—C11	99.5 (5)	C21—C20—H20A	119.6
C12—Fe4—S1	151.6 (3)	C22—C21—C20	118.8 (11)
C10—Fe4—S1	89.5 (3)	C22—C21—H21A	120.6
C11—Fe4—S1	106.5 (3)	C20—C21—H21A	120.6
C12—Fe4—S3	93.5 (3)	C21—C22—C23	121.7 (10)
C10—Fe4—S3	158.6 (3)	C21—C22—H22A	119.1
C11—Fe4—S3	100.4 (4)	C23—C22—H22A	119.1
S1—Fe4—S3	77.40 (8)	C22—C23—C24	117.8 (11)
C12—Fe4—Fe3	96.6 (3)	C22—C23—H23A	121.1
C10—Fe4—Fe3	102.1 (3)	C24—C23—H23A	121.1
C11—Fe4—Fe3	151.6 (3)	C19—C24—C23	120.8 (10)
S1—Fe4—Fe3	55.77 (6)	C19—C24—H24A	119.6
S3—Fe4—Fe3	56.54 (6)	C23—C24—H24A	119.6

C3—Fe1—Fe2—C4	−4.4 (4)	C3—Fe1—S2—C13	11.0 (5)
C1—Fe1—Fe2—C4	91.0 (4)	C1—Fe1—S2—C13	115.8 (9)
C2—Fe1—Fe2—C4	−132.0 (6)	C2—Fe1—S2—C13	−89.2 (4)
S1—Fe1—Fe2—C4	172.9 (3)	S1—Fe1—S2—C13	167.8 (4)
S2—Fe1—Fe2—C4	−91.1 (3)	Fe2—Fe1—S2—C13	109.9 (4)
C3—Fe1—Fe2—C5	−96.3 (4)	C3—Fe1—S2—Fe2	−98.9 (3)
C1—Fe1—Fe2—C5	−0.9 (4)	C1—Fe1—S2—Fe2	5.9 (8)
C2—Fe1—Fe2—C5	136.1 (6)	C2—Fe1—S2—Fe2	160.8 (3)
S1—Fe1—Fe2—C5	80.9 (3)	S1—Fe1—S2—Fe2	57.86 (7)
S2—Fe1—Fe2—C5	177.0 (3)	C12—Fe4—S3—C19	−11.6 (5)
C3—Fe1—Fe2—C6	127.6 (7)	C10—Fe4—S3—C19	−110.8 (9)
C1—Fe1—Fe2—C6	−137.1 (7)	C11—Fe4—S3—C19	90.8 (5)
C2—Fe1—Fe2—C6	−0.1 (8)	S1—Fe4—S3—C19	−164.4 (3)
S1—Fe1—Fe2—C6	−55.2 (6)	Fe3—Fe4—S3—C19	−107.3 (3)
S2—Fe1—Fe2—C6	40.8 (6)	C12—Fe4—S3—Fe3	95.6 (3)
C3—Fe1—Fe2—S1	−177.3 (3)	C10—Fe4—S3—Fe3	−3.6 (8)
C1—Fe1—Fe2—S1	−81.9 (3)	C11—Fe4—S3—Fe3	−161.9 (3)
C2—Fe1—Fe2—S1	55.1 (6)	S1—Fe4—S3—Fe3	−57.09 (7)
S2—Fe1—Fe2—S1	96.01 (9)	C7—Fe3—S3—C19	105.2 (8)
C3—Fe1—Fe2—S2	86.7 (3)	C8—Fe3—S3—C19	2.2 (4)
C1—Fe1—Fe2—S2	−177.9 (3)	C9—Fe3—S3—C19	−97.1 (4)
C2—Fe1—Fe2—S2	−40.9 (6)	S1—Fe3—S3—C19	162.6 (3)
S1—Fe1—Fe2—S2	−96.01 (9)	Fe4—Fe3—S3—C19	105.7 (3)
C7—Fe3—Fe4—C12	90.0 (4)	C7—Fe3—S3—Fe4	−0.5 (8)
C8—Fe3—Fe4—C12	−3.9 (4)	C8—Fe3—S3—Fe4	−103.4 (3)
C9—Fe3—Fe4—C12	−136.8 (6)	C9—Fe3—S3—Fe4	157.3 (3)
S1—Fe3—Fe4—C12	172.5 (3)	S1—Fe3—S3—Fe4	56.91 (7)
S3—Fe3—Fe4—C12	−89.9 (3)	C3—Fe1—C1—O1	101 (40)
C7—Fe3—Fe4—C10	−1.5 (4)	C2—Fe1—C1—O1	−159 (100)
C8—Fe3—Fe4—C10	−95.4 (4)	S1—Fe1—C1—O1	−54 (40)
C9—Fe3—Fe4—C10	131.7 (6)	S2—Fe1—C1—O1	−4 (41)
S1—Fe3—Fe4—C10	81.0 (3)	Fe2—Fe1—C1—O1	1 (40)
S3—Fe3—Fe4—C10	178.7 (3)	C3—Fe1—C2—O2	−77 (41)
C7—Fe3—Fe4—C11	−140.2 (8)	C1—Fe1—C2—O2	−172 (100)
C8—Fe3—Fe4—C11	125.9 (8)	S1—Fe1—C2—O2	95 (41)
C9—Fe3—Fe4—C11	−7.0 (9)	S2—Fe1—C2—O2	17 (41)
S1—Fe3—Fe4—C11	−57.7 (7)	Fe2—Fe1—C2—O2	50 (41)
S3—Fe3—Fe4—C11	40.0 (7)	C1—Fe1—C3—O3	−74 (41)
C7—Fe3—Fe4—S1	−82.5 (3)	C2—Fe1—C3—O3	−173 (100)
C8—Fe3—Fe4—S1	−176.4 (3)	S1—Fe1—C3—O3	25 (42)
C9—Fe3—Fe4—S1	50.7 (5)	S2—Fe1—C3—O3	86 (41)
S3—Fe3—Fe4—S1	97.67 (9)	Fe2—Fe1—C3—O3	30 (41)
C7—Fe3—Fe4—S3	179.8 (3)	C5—Fe2—C4—O4	17 (18)
C8—Fe3—Fe4—S3	86.0 (3)	C6—Fe2—C4—O4	117 (18)
C9—Fe3—Fe4—S3	−46.9 (5)	S1—Fe2—C4—O4	−69 (18)
S1—Fe3—Fe4—S3	−97.67 (9)	S2—Fe2—C4—O4	−140 (18)
C12—Fe4—S1—Fe2	117.4 (7)	Fe1—Fe2—C4—O4	−83 (18)
C10—Fe4—S1—Fe2	28.2 (3)	C4—Fe2—C5—O5	−135 (14)
C11—Fe4—S1—Fe2	−71.6 (4)	C6—Fe2—C5—O5	128 (14)
S3—Fe4—S1—Fe2	−168.84 (14)	S1—Fe2—C5—O5	21 (14)
Fe3—Fe4—S1—Fe2	133.25 (15)	S2—Fe2—C5—O5	−28 (14)
C12—Fe4—S1—Fe3	−15.8 (7)	Fe1—Fe2—C5—O5	−34 (14)
C10—Fe4—S1—Fe3	−105.0 (3)	C4—Fe2—C6—O6	−21 (16)
C11—Fe4—S1—Fe3	155.2 (4)	C5—Fe2—C6—O6	70 (16)
S3—Fe4—S1—Fe3	57.91 (7)	S1—Fe2—C6—O6	161 (16)
C12—Fe4—S1—Fe1	−136.3 (7)	S2—Fe2—C6—O6	−120 (16)
C10—Fe4—S1—Fe1	134.5 (3)	Fe1—Fe2—C6—O6	−154 (16)
C11—Fe4—S1—Fe1	34.7 (4)	C8—Fe3—C7—O7	66 (100)
S3—Fe4—S1—Fe1	−62.57 (15)	C9—Fe3—C7—O7	165 (100)
Fe3—Fe4—S1—Fe1	−120.47 (16)	S1—Fe3—C7—O7	−93 (100)
C4—Fe2—S1—Fe4	120.3 (7)	S3—Fe3—C7—O7	−38 (100)
C5—Fe2—S1—Fe4	34.6 (3)	Fe4—Fe3—C7—O7	−38 (100)
C6—Fe2—S1—Fe4	−65.3 (3)	C7—Fe3—C8—O8	16 (21)
S2—Fe2—S1—Fe4	−164.02 (14)	C9—Fe3—C8—O8	−83 (21)
Fe1—Fe2—S1—Fe4	137.35 (15)	S1—Fe3—C8—O8	111 (21)
C4—Fe2—S1—Fe3	−136.6 (7)	S3—Fe3—C8—O8	175 (21)
C5—Fe2—S1—Fe3	137.7 (3)	Fe4—Fe3—C8—O8	119 (21)
C6—Fe2—S1—Fe3	37.8 (3)	C7—Fe3—C9—O9	54 (25)
S2—Fe2—S1—Fe3	−60.89 (14)	C8—Fe3—C9—O9	147 (25)
Fe1—Fe2—S1—Fe3	−119.52 (15)	S1—Fe3—C9—O9	−39 (25)
C4—Fe2—S1—Fe1	−17.1 (7)	S3—Fe3—C9—O9	−118 (25)
C5—Fe2—S1—Fe1	−102.8 (3)	Fe4—Fe3—C9—O9	−80 (25)
C6—Fe2—S1—Fe1	157.4 (3)	C12—Fe4—C10—O10	−116 (20)
S2—Fe2—S1—Fe1	58.63 (7)	C11—Fe4—C10—O10	143 (19)
C7—Fe3—S1—Fe4	104.5 (3)	S1—Fe4—C10—O10	36 (20)
C8—Fe3—S1—Fe4	9.8 (9)	S3—Fe4—C10—O10	−16 (20)
C9—Fe3—S1—Fe4	−155.7 (3)	Fe3—Fe4—C10—O10	−19 (20)
S3—Fe3—S1—Fe4	−57.47 (7)	C12—Fe4—C11—O11	10 (69)
C7—Fe3—S1—Fe2	−24.5 (3)	C10—Fe4—C11—O11	102 (69)
C8—Fe3—S1—Fe2	−119.3 (9)	S1—Fe4—C11—O11	−166 (69)
C9—Fe3—S1—Fe2	75.3 (3)	S3—Fe4—C11—O11	−86 (69)
S3—Fe3—S1—Fe2	173.49 (14)	Fe3—Fe4—C11—O11	−119 (69)
Fe4—Fe3—S1—Fe2	−129.04 (15)	C10—Fe4—C12—O12	51 (27)
C7—Fe3—S1—Fe1	−119.6 (3)	C11—Fe4—C12—O12	151 (27)
C8—Fe3—S1—Fe1	145.6 (9)	S1—Fe4—C12—O12	−38 (27)
C9—Fe3—S1—Fe1	−19.8 (3)	S3—Fe4—C12—O12	−108 (27)
S3—Fe3—S1—Fe1	78.40 (12)	Fe3—Fe4—C12—O12	−51 (27)
Fe4—Fe3—S1—Fe1	135.87 (13)	Fe2—S2—C13—C18	−48.4 (8)
C3—Fe1—S1—Fe4	−123.7 (6)	Fe1—S2—C13—C18	−124.3 (7)
C1—Fe1—S1—Fe4	−24.1 (3)	Fe2—S2—C13—C14	137.4 (7)
C2—Fe1—S1—Fe4	74.9 (3)	Fe1—S2—C13—C14	61.4 (9)
S2—Fe1—S1—Fe4	171.89 (16)	C18—C13—C14—C15	1.9 (17)
Fe2—Fe1—S1—Fe4	−129.87 (16)	S2—C13—C14—C15	176.2 (9)
C3—Fe1—S1—Fe2	6.2 (6)	C13—C14—C15—C16	−2 (2)
C1—Fe1—S1—Fe2	105.8 (3)	C14—C15—C16—C17	1 (2)
C2—Fe1—S1—Fe2	−155.3 (3)	C15—C16—C17—C18	0 (2)
S2—Fe1—S1—Fe2	−58.24 (7)	C14—C13—C18—C17	−0.9 (15)
C3—Fe1—S1—Fe3	137.9 (6)	S2—C13—C18—C17	−175.1 (8)
C1—Fe1—S1—Fe3	−122.6 (3)	C16—C17—C18—C13	0.1 (17)
C2—Fe1—S1—Fe3	−23.6 (3)	Fe4—S3—C19—C20	133.2 (7)
S2—Fe1—S1—Fe3	73.44 (12)	Fe3—S3—C19—C20	58.9 (8)
Fe2—Fe1—S1—Fe3	131.68 (13)	Fe4—S3—C19—C24	−52.7 (8)
C4—Fe2—S2—C13	−9.3 (4)	Fe3—S3—C19—C24	−127.0 (7)
C5—Fe2—S2—C13	−114.7 (8)	C24—C19—C20—C21	4.4 (16)
C6—Fe2—S2—C13	90.1 (4)	S3—C19—C20—C21	178.5 (8)
S1—Fe2—S2—C13	−165.3 (3)	C19—C20—C21—C22	−1.6 (18)
Fe1—Fe2—S2—C13	−107.4 (3)	C20—C21—C22—C23	−1.4 (19)
C4—Fe2—S2—Fe1	98.1 (3)	C21—C22—C23—C24	1.5 (19)
C5—Fe2—S2—Fe1	−7.3 (7)	C20—C19—C24—C23	−4.3 (15)
C6—Fe2—S2—Fe1	−162.5 (3)	S3—C19—C24—C23	−178.4 (8)
S1—Fe2—S2—Fe1	−57.96 (7)	C22—C23—C24—C19	1.3 (17)

Experimental details

Crystal data
Chemical formula	[Fe₄C₂₄H₁₀O₁₂S₃]
M_r	809.90
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	293
a, b, c (Å)	9.0026 (2), 12.9509 (4), 26.5409 (2)
β (°)	97.612 (1)
V (Å³)	3067.18 (12)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.12
Crystal size (mm)	0.50 × 0.38 × 0.36

Data collection
Diffractometer	Siemens SMART CCD area detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.698, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	9335, 5418, 4103
R_int	0.038
(sin θ/λ)_max (Å⁻¹)	0.597

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.069, 0.147, 1.03
No. of reflections	5418
No. of parameters	388
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0017P)² + 30.5273P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	0.52, −0.41

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1994), XPREP in SHELXTL (Siemens, 1994), SHELXTL.

Selected geometric parameters (Å, º) top

Fe1—C3	1.791 (8)	Fe3—C7	1.786 (9)
Fe1—C1	1.790 (9)	Fe3—C8	1.798 (9)
Fe1—C2	1.820 (10)	Fe3—C9	1.802 (9)
Fe1—S1	2.249 (2)	Fe3—S1	2.244 (2)
Fe1—S2	2.281 (2)	Fe3—S3	2.286 (2)
Fe1—Fe2	2.5256 (16)	Fe3—Fe4	2.5313 (16)
Fe2—C4	1.796 (10)	Fe4—C12	1.793 (10)
Fe2—C5	1.803 (10)	Fe4—C10	1.787 (10)
Fe2—C6	1.826 (9)	Fe4—C11	1.810 (11)
Fe2—S1	2.243 (2)	Fe4—S1	2.235 (2)
Fe2—S2	2.267 (2)	Fe4—S3	2.270 (2)

Fe4—S1—Fe2	131.96 (10)	Fe2—S1—Fe1	68.43 (7)
Fe4—S1—Fe3	68.81 (7)	Fe3—S1—Fe1	125.67 (9)
Fe2—S1—Fe3	135.79 (10)	Fe2—S2—Fe1	67.46 (7)
Fe4—S1—Fe1	138.98 (10)	Fe4—S3—Fe3	67.51 (7)

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