μ4-Orthothio­carbonato-tetra­kis­[tri­carbonyl­iron(I)](2 Fe—Fe)

Shi, Y.-C.; Cheng, H.-R.; Yuan, L.-M.; Li, Q.-K.

doi:10.1107/S1600536811041936

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 11| November 2011| Page m1534

doi:10.1107/S1600536811041936

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μ₄-Orthothiocarbonato-tetrakis[tricarbonyliron(I)](2 Fe—Fe)

Yao-Cheng Shi,^a ^* Huan-Ren Cheng,^a Li-Min Yuan ^b and Qian-Kun Li ^c

^aCollege of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225002, People's Republic of China, ^bTesting Center, Yangzhou University, Yangzhou 225009, People's Republic of China, and ^cHubei Research Institue of Geophysics Survey and Design, Wuhan 430056, People's Republic of China
^*Correspondence e-mail: ycshi@yzu.edu.cn

(Received 28 September 2011; accepted 11 October 2011; online 12 October 2011)

The fused bis-butterfly-shaped title compound, [Fe₄(CS₄)(CO)₁₂], possesses an orthothiocarbonate (CS₄⁴⁻) ligand that acts as a bridge between two Fe₂(CO)₆ units. A short intramolecular S⋯S contact [2.6984 (8) and 2.6977 (8) Å] occurs in each S₂Fe₂(CO)₆ fragment.

Related literature

For general background to related complexes, see: Mathur et al. (2009 ). For uses of R₃P/CS₂ in coordination chemistry and organometallic chemistry, see: Galindo et al. (1999 ). For the synthesis of butterfly S₂Fe₂(CO)₆ complexes, see: Song (2005 ). For related structures, see: Shaver et al. (1979 ); Ortega-Alfaro et al. (2004 ).

Experimental

Crystal data

[Fe₄(CS₄)(CO)₁₂]
M_r = 699.81
Triclinic, $[P \overline 1]$
a = 9.0875 (9) Å
b = 10.9002 (11) Å
c = 12.6448 (13) Å
α = 101.8859 (12)°
β = 92.4964 (12)°
γ = 110.0857 (12)°
V = 1142.2 (2) Å³
Z = 2
Mo Kα radiation
μ = 2.91 mm⁻¹
T = 296 K
0.15 × 0.12 × 0.11 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ) T_min = 0.658, T_max = 0.721
10006 measured reflections
5128 independent reflections
4237 reflections with I > 2σ(I)
R_int = 0.025

Refinement

R[F² > 2σ(F²)] = 0.026
wR(F²) = 0.070
S = 1.04
5128 reflections
298 parameters
6 restraints
Δρ_max = 0.35 e Å⁻³
Δρ_min = −0.27 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

C13—S1	1.827 (2)
C13—S2	1.8300 (19)
C13—S3	1.830 (2)
C13—S4	1.837 (2)
Fe1—S1	2.2730 (6)
Fe1—S2	2.2688 (7)
Fe1—Fe2	2.4949 (5)
Fe2—S1	2.2723 (6)
Fe2—S2	2.2685 (7)
Fe3—S3	2.2676 (6)
Fe3—S4	2.2680 (6)
Fe3—Fe4	2.5007 (5)
Fe4—S3	2.2712 (7)
Fe4—S4	2.2626 (6)

S1—C13—S2	95.10 (10)
S3—C13—S4	94.73 (9)

Data collection: SMART (Bruker, 2002 ); cell refinement: SAINT-Plus (Bruker, 2003 ); data reduction: SAINT-Plus; program(s) used to solve structure: SIR2004 (Burla et al., 2005 ); program(s) used to refine structure: SHELXTL (Sheldrick, 2008 ); molecular graphics: PLATON (Spek, 2009 ) and WinGX (Farrugia, 1999 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811041936/ng5239sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811041936/ng5239Isup2.hkl

checkCIF report

Comment top

The activation and cleavage of selected bonds of small molecules by transition metal complexes is one of the challenging subjects of recent researches. CS₂ has been shown to undergo a variety of reactions with transition metals, including insertion and disproportionation, and there is a growing interest in the activation of CS₂ from catalytic and biological points of view. The cleavage of the C—S bonds is often observed in various transition metal complexes in which chemistry has been explored for the hydrosulfurization of fossil products. In these complexes, the S^2- ion derived from the C—S bond scission functions as a bridging ligand to link metal ions and metal cluster fragments and is generally of use in various cluster growth processes (Mathur et al., 2009).

Interestingly, the reaction of Et₃P/CS₂ and Fe₃(CO)₁₂ in THF under inert atmosphere at room temperature leads to the formation of a novel complex (Scheme 1). The molecular structure of the novel complex (Fig. 1) consists of two butterfly Fe₂(CO)₆ units connected by a bridging CS₄ ligand in axial C—S bond fashions similar to the related complex Fe₂(CO)₆(µ-S)₂CH₂ (Shaver et al., 1979). The Fe—Fe bond lengths are 2.4949 (5) and 2.5007 (5) Å and close to 2.485 (1) Å in Fe₂(CO)₆(µ-S)₂CH₂, but slightly shorter than 2.511 (1) Å in the complex Fe₂(CO)₆(µ-SCH₃)₂ (Table 1) (Ortega-Alfaro et al., 2004), the corresponding C—S bond lengths are 1.827 (2), 1.830 (2) and 1.830 (2), 1.837 (2)°, respectively, which are longer than those in the complex Fe₂(CO)₆(µ-SCH₃)₂. For each S₂Fe₂(CO)₆ butterfly core, the S—C—S bond angle is 95.10 (10) and 94.73 (9)° and close to 94.55 (3)° in Fe₂(CO)₆(µ-S)₂CH₂ (Table 1). As compared with 2.744 (1)–2.773 (1) Å in Fe₂(CO)₆(µ-SCH₃)₂, the S···S distance (2.6984 (8) and 2.6977 (8) Å) indicates an intramolecular short contact in each S₂Fe₂(CO)₆ butterfly core.

Related literature top

For general background to related complexes, see: Mathur et al. (2009). For uses of R₃P/CS₂ in coordination chemistry and organometallic chemistry, see: Galindo et al. (1999). For the synthesis of butterfly S₂Fe₂(CO)₆ complexes, see: Song (2005). For related structures, see: Shaver et al. (1979); Ortega-Alfaro et al. (2004).

Experimental top

A THF solution of Et₃P/CS₂ (1 mmol) and Fe₃(CO)₁₂ (1 mmol) under inert atmosphere is stirred for 24 h at room temperature. After removal of the solvent, the mixture was purified by chromatography on silica gel with dichloromethane-petroleum ether (v/v, 1:3) as eluant to give the red-orange solid. Single crystals were grown from ether solution of the title compound.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SIR2004 (Burla et al., 2005); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009) and WinGX (Farrugia, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

Fig. 1. The molecule of the title compound, showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 30% probability level.

µ₄-Orthothiocarbonato-tetrakis[tricarbonyliron(I)](2 Fe—Fe) top

Crystal data top

[Fe₄(CS₄)(CO)₁₂]	Z = 2
M_r = 699.81	F(000) = 684
Triclinic, P1	D_x = 2.035 Mg m⁻³
a = 9.0875 (9) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.9002 (11) Å	Cell parameters from 4237 reflections
c = 12.6448 (13) Å	θ = 1.7–27.5°
α = 101.8859 (12)°	µ = 2.91 mm⁻¹
β = 92.4964 (12)°	T = 296 K
γ = 110.0857 (12)°	Prism, red
V = 1142.2 (2) Å³	0.15 × 0.12 × 0.11 mm

Data collection top

Bruker SMART APEX CCD diffractometer	5128 independent reflections
Radiation source: fine-focus sealed tube	4237 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.025
ω and ϕ scans	θ_max = 27.5°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	h = −11→11
T_min = 0.658, T_max = 0.721	k = −14→14
10006 measured reflections	l = −16→16

Refinement top

Refinement on F²	6 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.026	Secondary atom site location: difference Fourier map
wR(F²) = 0.070	w = 1/[σ²(F_o²) + (0.0332P)²] where P = (F_o² + 2F_c²)/3
S = 1.04	(Δ/σ)_max < 0.001
5128 reflections	Δρ_max = 0.35 e Å⁻³
298 parameters	Δρ_min = −0.27 e Å⁻³

Crystal data top

[Fe₄(CS₄)(CO)₁₂]	γ = 110.0857 (12)°
M_r = 699.81	V = 1142.2 (2) Å³
Triclinic, P1	Z = 2
a = 9.0875 (9) Å	Mo Kα radiation
b = 10.9002 (11) Å	µ = 2.91 mm⁻¹
c = 12.6448 (13) Å	T = 296 K
α = 101.8859 (12)°	0.15 × 0.12 × 0.11 mm
β = 92.4964 (12)°

Data collection top

Bruker SMART APEX CCD diffractometer	5128 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2004)	4237 reflections with I > 2σ(I)
T_min = 0.658, T_max = 0.721	R_int = 0.025
10006 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	298 parameters
wR(F²) = 0.070	6 restraints
S = 1.04	Δρ_max = 0.35 e Å⁻³
5128 reflections	Δρ_min = −0.27 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
C1	0.6561 (3)	0.7935 (2)	0.77984 (18)	0.0440 (5)
C2	0.8526 (3)	0.8863 (3)	0.6347 (2)	0.0506 (6)
C3	0.9578 (3)	0.9654 (3)	0.8400 (2)	0.0495 (6)
C4	1.1219 (3)	0.7705 (3)	0.5832 (2)	0.0576 (7)
C5	1.2260 (3)	0.8567 (3)	0.7869 (2)	0.0499 (6)
C6	1.1533 (3)	0.5863 (3)	0.6883 (2)	0.0520 (6)
C7	0.7715 (3)	0.4656 (3)	1.0044 (2)	0.0518 (6)
C8	0.6869 (3)	0.2015 (3)	0.9062 (2)	0.0571 (7)
C9	0.4644 (3)	0.2955 (2)	0.94124 (17)	0.0461 (6)
C10	0.5449 (3)	0.1072 (3)	0.6532 (2)	0.0533 (6)
C11	0.3306 (3)	0.2117 (3)	0.69401 (19)	0.0538 (6)
C12	0.5320 (3)	0.3000 (2)	0.54991 (19)	0.0461 (5)
C13	0.7801 (2)	0.5349 (2)	0.75626 (15)	0.0326 (4)
Fe1	0.85275 (4)	0.80727 (3)	0.74597 (2)	0.03532 (9)
Fe2	1.06610 (4)	0.71578 (3)	0.70503 (2)	0.03858 (9)
Fe3	0.64765 (4)	0.34558 (3)	0.88425 (2)	0.03604 (9)
Fe4	0.54035 (4)	0.27424 (3)	0.68685 (2)	0.03649 (9)
O1	0.5347 (2)	0.7883 (2)	0.80095 (16)	0.0652 (5)
O2	0.8523 (3)	0.9343 (2)	0.56303 (17)	0.0808 (7)
O3	1.0252 (3)	1.0659 (2)	0.89976 (17)	0.0801 (6)
O4	1.1562 (3)	0.8060 (3)	0.50561 (17)	0.0906 (8)
O5	1.3234 (2)	0.9495 (2)	0.83931 (18)	0.0764 (6)
O6	1.2101 (3)	0.5078 (2)	0.67522 (19)	0.0802 (6)
O7	0.8437 (3)	0.5364 (2)	1.08183 (16)	0.0849 (7)
O8	0.7108 (3)	0.1096 (2)	0.9194 (2)	0.0923 (7)
O9	0.3472 (2)	0.2622 (2)	0.97500 (15)	0.0716 (6)
O10	0.5481 (3)	0.0019 (2)	0.63331 (18)	0.0840 (7)
O11	0.1982 (3)	0.1726 (3)	0.69931 (18)	0.0901 (7)
O12	0.5245 (2)	0.3122 (2)	0.46352 (14)	0.0717 (6)
S1	0.92568 (6)	0.68363 (5)	0.84778 (4)	0.03454 (12)
S2	0.80928 (7)	0.60300 (6)	0.63482 (4)	0.03789 (13)
S3	0.80213 (6)	0.37272 (5)	0.74843 (4)	0.03674 (12)
S4	0.57807 (6)	0.47963 (5)	0.79267 (4)	0.03420 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0464 (14)	0.0398 (13)	0.0478 (12)	0.0174 (11)	0.0032 (10)	0.0116 (10)
C2	0.0482 (15)	0.0460 (14)	0.0586 (14)	0.0159 (12)	0.0062 (12)	0.0168 (12)
C3	0.0446 (14)	0.0430 (14)	0.0568 (14)	0.0113 (12)	0.0098 (11)	0.0103 (12)
C4	0.0577 (17)	0.0620 (17)	0.0653 (17)	0.0292 (14)	0.0259 (14)	0.0241 (14)
C5	0.0368 (14)	0.0484 (15)	0.0656 (16)	0.0140 (12)	0.0142 (12)	0.0163 (13)
C6	0.0452 (15)	0.0523 (15)	0.0623 (15)	0.0179 (12)	0.0168 (12)	0.0189 (13)
C7	0.0536 (16)	0.0528 (15)	0.0469 (13)	0.0150 (13)	0.0004 (11)	0.0155 (12)
C8	0.0601 (17)	0.0545 (16)	0.0633 (16)	0.0241 (14)	0.0094 (13)	0.0218 (13)
C9	0.0510 (15)	0.0453 (14)	0.0360 (11)	0.0114 (12)	0.0063 (10)	0.0065 (10)
C10	0.0601 (17)	0.0402 (14)	0.0502 (14)	0.0095 (12)	0.0063 (12)	0.0057 (11)
C11	0.0481 (16)	0.0526 (16)	0.0440 (13)	0.0020 (13)	0.0040 (11)	0.0040 (11)
C12	0.0436 (14)	0.0401 (13)	0.0434 (13)	0.0046 (11)	0.0000 (10)	0.0049 (10)
C13	0.0291 (11)	0.0319 (10)	0.0341 (10)	0.0089 (9)	0.0031 (8)	0.0057 (8)
Fe1	0.03283 (18)	0.03237 (17)	0.03938 (17)	0.00973 (13)	0.00397 (13)	0.00912 (13)
Fe2	0.03253 (18)	0.03943 (18)	0.04416 (18)	0.01127 (14)	0.01067 (13)	0.01241 (14)
Fe3	0.03703 (18)	0.03452 (17)	0.03534 (16)	0.01093 (14)	0.00442 (13)	0.00903 (13)
Fe4	0.03603 (18)	0.03052 (17)	0.03559 (16)	0.00580 (13)	0.00263 (13)	0.00313 (13)
O1	0.0438 (11)	0.0676 (13)	0.0955 (14)	0.0303 (10)	0.0199 (10)	0.0237 (11)
O2	0.0919 (17)	0.0883 (16)	0.0771 (13)	0.0311 (14)	0.0146 (12)	0.0530 (13)
O3	0.0750 (15)	0.0484 (12)	0.0894 (15)	0.0052 (11)	0.0037 (12)	−0.0119 (11)
O4	0.112 (2)	0.112 (2)	0.0796 (14)	0.0537 (16)	0.0579 (14)	0.0566 (15)
O5	0.0456 (12)	0.0589 (13)	0.1025 (16)	0.0024 (10)	0.0007 (11)	0.0014 (12)
O6	0.0805 (16)	0.0736 (15)	0.1125 (17)	0.0495 (13)	0.0371 (13)	0.0347 (13)
O7	0.0857 (16)	0.0882 (16)	0.0530 (11)	0.0075 (13)	−0.0226 (11)	0.0045 (11)
O8	0.1114 (19)	0.0722 (15)	0.1227 (19)	0.0545 (15)	0.0225 (15)	0.0475 (15)
O9	0.0573 (13)	0.0795 (15)	0.0636 (12)	0.0077 (11)	0.0265 (10)	0.0115 (11)
O10	0.1131 (19)	0.0391 (11)	0.0960 (16)	0.0283 (12)	0.0166 (14)	0.0056 (11)
O11	0.0473 (13)	0.1058 (19)	0.0861 (15)	−0.0053 (12)	0.0126 (11)	0.0119 (14)
O12	0.0788 (14)	0.0732 (14)	0.0428 (10)	0.0033 (11)	−0.0061 (9)	0.0147 (9)
S1	0.0314 (3)	0.0334 (3)	0.0332 (2)	0.0058 (2)	0.0010 (2)	0.0063 (2)
S2	0.0398 (3)	0.0375 (3)	0.0317 (3)	0.0086 (2)	0.0031 (2)	0.0077 (2)
S3	0.0338 (3)	0.0338 (3)	0.0430 (3)	0.0135 (2)	0.0070 (2)	0.0071 (2)
S4	0.0298 (3)	0.0309 (3)	0.0400 (3)	0.0097 (2)	0.0045 (2)	0.0062 (2)

Geometric parameters (Å, º) top

C1—O1	1.131 (3)	C10—Fe4	1.798 (3)
C1—Fe1	1.819 (3)	C11—O11	1.140 (3)
C2—O2	1.136 (3)	C11—Fe4	1.804 (3)
C2—Fe1	1.795 (2)	C12—O12	1.129 (3)
C3—O3	1.142 (3)	C12—Fe4	1.813 (2)
C3—Fe1	1.796 (3)	C13—S1	1.827 (2)
C4—O4	1.145 (3)	C13—S2	1.8300 (19)
C4—Fe2	1.795 (3)	C13—S3	1.830 (2)
C5—O5	1.142 (3)	C13—S4	1.837 (2)
C5—Fe2	1.795 (3)	Fe1—S1	2.2730 (6)
C6—O6	1.130 (3)	Fe1—S2	2.2688 (7)
C6—Fe2	1.824 (3)	Fe1—Fe2	2.4949 (5)
C7—O7	1.127 (3)	Fe2—S1	2.2723 (6)
C7—Fe3	1.818 (3)	Fe2—S2	2.2685 (7)
C8—O8	1.138 (3)	Fe3—S3	2.2676 (6)
C8—Fe3	1.796 (3)	Fe3—S4	2.2680 (6)
C9—O9	1.134 (3)	Fe3—Fe4	2.5007 (5)
C9—Fe3	1.798 (3)	Fe4—S3	2.2712 (7)
C10—O10	1.135 (3)	Fe4—S4	2.2626 (6)

S1···S2	2.6984 (8)	S3···S4	2.6977 (8)

O1—C1—Fe1	178.3 (2)	C6—Fe2—Fe1	154.51 (8)
O2—C2—Fe1	178.8 (2)	S2—Fe2—Fe1	56.649 (18)
O3—C3—Fe1	179.6 (3)	S1—Fe2—Fe1	56.723 (17)
O4—C4—Fe2	179.2 (3)	C8—Fe3—C9	91.66 (12)
O5—C5—Fe2	177.0 (2)	C8—Fe3—C7	97.13 (12)
O6—C6—Fe2	177.6 (2)	C9—Fe3—C7	98.48 (11)
O7—C7—Fe3	176.7 (2)	C8—Fe3—S3	93.97 (9)
O8—C8—Fe3	179.5 (3)	C9—Fe3—S3	155.51 (7)
O9—C9—Fe3	178.5 (2)	C7—Fe3—S3	104.42 (8)
O10—C10—Fe4	179.2 (3)	C8—Fe3—S4	158.63 (9)
O11—C11—Fe4	179.5 (3)	C9—Fe3—S4	93.86 (8)
O12—C12—Fe4	178.0 (2)	C7—Fe3—S4	102.43 (8)
S1—C13—S3	118.10 (10)	S3—Fe3—S4	72.99 (2)
S1—C13—S2	95.10 (10)	C8—Fe3—Fe4	102.35 (9)
S3—C13—S2	117.13 (11)	C9—Fe3—Fe4	98.88 (7)
S1—C13—S4	116.95 (11)	C7—Fe3—Fe4	153.39 (8)
S3—C13—S4	94.73 (9)	S3—Fe3—Fe4	56.635 (18)
S2—C13—S4	116.62 (10)	S4—Fe3—Fe4	56.394 (17)
C2—Fe1—C3	92.20 (12)	C10—Fe4—C11	92.11 (13)
C2—Fe1—C1	97.54 (11)	C10—Fe4—C12	97.98 (11)
C3—Fe1—C1	96.81 (11)	C11—Fe4—C12	97.54 (11)
C2—Fe1—S2	93.44 (9)	C10—Fe4—S4	157.10 (8)
C3—Fe1—S2	158.89 (8)	C11—Fe4—S4	93.60 (9)
C1—Fe1—S2	102.58 (8)	C12—Fe4—S4	103.21 (8)
C2—Fe1—S1	156.74 (8)	C10—Fe4—S3	94.03 (9)
C3—Fe1—S1	94.58 (8)	C11—Fe4—S3	157.73 (8)
C1—Fe1—S1	103.69 (7)	C12—Fe4—S3	102.76 (8)
S2—Fe1—S1	72.90 (2)	S4—Fe4—S3	73.03 (2)
C2—Fe1—Fe2	100.11 (8)	C10—Fe4—Fe3	100.52 (8)
C3—Fe1—Fe2	102.33 (8)	C11—Fe4—Fe3	101.33 (8)
C1—Fe1—Fe2	153.30 (7)	C12—Fe4—Fe3	152.93 (8)
S2—Fe1—Fe2	56.636 (18)	S4—Fe4—Fe3	56.600 (16)
S1—Fe1—Fe2	56.695 (17)	S3—Fe4—Fe3	56.499 (16)
C5—Fe2—C4	91.26 (13)	C13—S1—Fe2	88.02 (6)
C5—Fe2—C6	100.64 (12)	C13—S1—Fe1	87.12 (6)
C4—Fe2—C6	96.91 (11)	Fe2—S1—Fe1	66.582 (18)
C5—Fe2—S2	153.65 (8)	C13—S2—Fe2	88.06 (7)
C4—Fe2—S2	93.88 (9)	C13—S2—Fe1	87.17 (7)
C6—Fe2—S2	104.35 (9)	Fe2—S2—Fe1	66.715 (19)
C5—Fe2—S1	93.23 (8)	C13—S3—Fe3	87.77 (7)
C4—Fe2—S1	157.61 (9)	C13—S3—Fe4	87.52 (7)
C6—Fe2—S1	103.77 (8)	Fe3—S3—Fe4	66.867 (19)
S2—Fe2—S1	72.92 (2)	C13—S4—Fe4	87.60 (7)
C5—Fe2—Fe1	97.00 (8)	C13—S4—Fe3	87.58 (6)
C4—Fe2—Fe1	100.96 (8)	Fe4—S4—Fe3	67.006 (19)

Experimental details

Crystal data
Chemical formula	[Fe₄(CS₄)(CO)₁₂]
M_r	699.81
Crystal system, space group	Triclinic, P1
Temperature (K)	296
a, b, c (Å)	9.0875 (9), 10.9002 (11), 12.6448 (13)
α, β, γ (°)	101.8859 (12), 92.4964 (12), 110.0857 (12)
V (Å³)	1142.2 (2)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.91
Crystal size (mm)	0.15 × 0.12 × 0.11

Data collection
Diffractometer	Bruker SMART APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2004)
T_min, T_max	0.658, 0.721
No. of measured, independent and observed [I > 2σ(I)] reflections	10006, 5128, 4237
R_int	0.025
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.070, 1.04
No. of reflections	5128
No. of parameters	298
No. of restraints	6
Δρ_max, Δρ_min (e Å⁻³)	0.35, −0.27

Computer programs: SMART (Bruker, 2002), SAINT-Plus (Bruker, 2003), SIR2004 (Burla et al., 2005), SHELXTL (Sheldrick, 2008), PLATON (Spek, 2009) and WinGX (Farrugia, 1999), publCIF (Westrip, 2010).

Selected geometric parameters (Å, º) top

C13—S1	1.827 (2)	Fe2—S1	2.2723 (6)
C13—S2	1.8300 (19)	Fe2—S2	2.2685 (7)
C13—S3	1.830 (2)	Fe3—S3	2.2676 (6)
C13—S4	1.837 (2)	Fe3—S4	2.2680 (6)
Fe1—S1	2.2730 (6)	Fe3—Fe4	2.5007 (5)
Fe1—S2	2.2688 (7)	Fe4—S3	2.2712 (7)
Fe1—Fe2	2.4949 (5)	Fe4—S4	2.2626 (6)

S1—C13—S2	95.10 (10)	S3—C13—S4	94.73 (9)

Acknowledgements

The authors thank the Natural Science Foundation of China (No. 20572091) and the Natural Science Foundation of Jiangsu Province (No. 05KJB150151) for financial support of this work.

References

Bruker (2002). SMART. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2003). SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381–388. Web of Science CrossRef CAS IUCr Journals Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Galindo, A., Miguel, D. & Perez, J. (1999). Coord. Chem. Rev. 193–195, 643–690. Web of Science CrossRef CAS Google Scholar
Mathur, P., Boodida, S., Ji, R. S. & Mobin, S. M. (2009). J. Organomet. Chem. 694, 3043–3045. Web of Science CSD CrossRef CAS Google Scholar
Ortega-Alfaro, M. C., Hernández, N., Cerna, I., López-Cortés, J. G., Gómez, E., Toscano, R. A. & Alvarez-Toledano, C. (2004). J. Organomet. Chem. 689, 885–893. CAS Google Scholar
Shaver, A., Fitzpatrick, P. J., Steliou, K. & Butler, I. S. (1979). J. Am. Chem. Soc. 101, 1313–1315. CSD CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Song, L.-C. (2005). Acc. Chem. Res. 38, 21–28. Web of Science CrossRef PubMed CAS Google Scholar
Spek, A. L. (2009). Acta Cryst. D65, 148–155. Web of Science CrossRef CAS IUCr Journals Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar