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

Liu, X.-F.; Yu, X.-Y.

doi:10.1107/S1600536811042139

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 11| November 2011| Page m1552

doi:10.1107/S1600536811042139

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

Xu-Feng Liu ^a ^* and Xiao-Yong Yu ^a

^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 ); Wang et al. (2009 ); Yin et al. (2011 ).

Experimental

Crystal data

[Fe₂(C₂H₄S₂)(C₂₄H₂₀OP₂)(CO)₅]
M_r = 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 ) T_min = 0.790, T_max = 0.886
31351 measured reflections
7281 independent reflections
6102 reflections with I > 2σ(I)
R_int = 0.039

Refinement

R[F² > 2σ(F²)] = 0.026
wR(F²) = 0.059
S = 1.06
7281 reflections
388 parameters
H-atom parameters constrained
Δρ_max = 0.36 e Å⁻³
Δρ_min = −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); cell refinement: CrystalClear; data reduction: CrystalClear; 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).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811042139/hb6442sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811042139/hb6442Isup2.hkl

checkCIF report

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.

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

	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.
	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)(Fe—Fe) top

Crystal data top

[Fe₂(C₂H₄S₂)(C₂₄H₂₀OP₂)(CO)₅]	F(000) = 1488
M_r = 730.26	D_x = 1.588 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 11006 reflections
a = 13.865 (4) Å	θ = 1.4–27.9°
b = 15.398 (4) Å	µ = 1.24 mm⁻¹
c = 14.459 (5) Å	T = 113 K
β = 98.357 (4)°	Prism, colorless
V = 3054.1 (16) Å³	0.20 × 0.18 × 0.10 mm
Z = 4

Data collection top

Rigaku Saturn724 CCD diffractometer	7281 independent reflections
Radiation source: rotating anode	6102 reflections with I > 2σ(I)
Multilayer monochromator	R_int = 0.039
Detector resolution: 14.22 pixels mm^-1	θ_max = 27.9°, θ_min = 1.9°
ω and ϕ scans	h = −18→18
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2005)	k = −17→20
T_min = 0.790, T_max = 0.886	l = −19→19
31351 measured reflections

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)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.059	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.024P)²] where P = (F_o² + 2F_c²)/3
7281 reflections	(Δ/σ)_max = 0.002
388 parameters	Δρ_max = 0.36 e Å⁻³
0 restraints	Δρ_min = −0.36 e Å⁻³

Crystal data top

[Fe₂(C₂H₄S₂)(C₂₄H₂₀OP₂)(CO)₅]	V = 3054.1 (16) Å³
M_r = 730.26	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 13.865 (4) Å	µ = 1.24 mm⁻¹
b = 15.398 (4) Å	T = 113 K
c = 14.459 (5) Å	0.20 × 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)
T_min = 0.790, T_max = 0.886	R_int = 0.039
31351 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	0 restraints
wR(F²) = 0.059	H-atom parameters constrained
S = 1.06	Δρ_max = 0.36 e Å⁻³
7281 reflections	Δρ_min = −0.36 e Å⁻³
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

	x	y	z	U_iso*/U_eq
Fe1	1.261528 (16)	0.058771 (14)	0.331352 (16)	0.01557 (6)
Fe2	1.133418 (15)	0.174298 (14)	0.288051 (14)	0.01275 (6)
P1	0.99707 (3)	0.24364 (3)	0.31226 (3)	0.01291 (9)
P2	0.86096 (3)	0.16331 (3)	0.27704 (3)	0.01404 (9)
S1	1.18853 (3)	0.13327 (3)	0.43559 (3)	0.01697 (9)
S2	1.10474 (3)	0.03046 (2)	0.27533 (3)	0.01596 (9)
O1	1.30120 (9)	−0.10606 (7)	0.43282 (8)	0.0300 (3)
O2	1.43873 (9)	0.15892 (8)	0.39375 (10)	0.0411 (4)
O3	1.32473 (9)	0.01325 (8)	0.15188 (9)	0.0366 (3)
O4	1.26144 (9)	0.32544 (8)	0.29575 (9)	0.0321 (3)
O5	1.12828 (9)	0.17617 (8)	0.08534 (8)	0.0298 (3)
O6	0.86136 (7)	0.09157 (6)	0.34670 (7)	0.0177 (2)
C1	1.28842 (11)	−0.04173 (11)	0.39306 (11)	0.0209 (4)
C2	1.36981 (12)	0.11973 (11)	0.36834 (13)	0.0250 (4)
C3	1.29927 (12)	0.03076 (10)	0.22113 (12)	0.0232 (4)
C4	1.20985 (12)	0.26713 (10)	0.29551 (11)	0.0193 (3)
C5	1.12641 (11)	0.17650 (10)	0.16457 (11)	0.0185 (3)
C6	1.09760 (11)	0.05588 (10)	0.46439 (11)	0.0209 (4)
H6A	1.1266	0.0200	0.5182	0.025*
H6B	1.0418	0.0881	0.4833	0.025*
C7	1.06081 (12)	−0.00340 (10)	0.38252 (11)	0.0195 (3)
H7A	0.9886	−0.0031	0.3724	0.023*
H7B	1.0827	−0.0636	0.3979	0.023*
C8	0.99500 (11)	0.27904 (10)	0.43317 (10)	0.0167 (3)
C9	1.05975 (13)	0.34539 (11)	0.46564 (12)	0.0259 (4)
H9	1.1029	0.3676	0.4260	0.031*
C10	1.06217 (14)	0.37937 (12)	0.55452 (12)	0.0328 (4)
H10	1.1068	0.4244	0.5756	0.039*
C11	0.99951 (13)	0.34765 (12)	0.61251 (12)	0.0310 (4)
H11	1.0001	0.3716	0.6731	0.037*
C12	0.93619 (13)	0.28118 (12)	0.58215 (12)	0.0303 (4)
H12	0.8940	0.2589	0.6226	0.036*
C13	0.93332 (11)	0.24635 (11)	0.49297 (11)	0.0209 (4)
H13	0.8895	0.2004	0.4729	0.025*
C14	0.96328 (11)	0.34554 (9)	0.24976 (11)	0.0151 (3)
C15	1.00002 (11)	0.36534 (10)	0.16773 (11)	0.0186 (3)
H15	1.0464	0.3279	0.1462	0.022*
C16	0.96935 (12)	0.43952 (10)	0.11709 (12)	0.0247 (4)
H16	0.9938	0.4517	0.0604	0.030*
C17	0.90373 (12)	0.49556 (11)	0.14854 (12)	0.0258 (4)
H17	0.8830	0.5462	0.1137	0.031*
C18	0.86815 (12)	0.47762 (11)	0.23126 (12)	0.0254 (4)
H18	0.8233	0.5163	0.2535	0.031*
C19	0.89793 (11)	0.40335 (10)	0.28154 (11)	0.0210 (4)
H19	0.8735	0.3916	0.3384	0.025*
C20	0.86646 (11)	0.12448 (10)	0.16014 (10)	0.0167 (3)
C21	0.85652 (12)	0.03529 (10)	0.14617 (11)	0.0235 (4)
H21	0.8466	−0.0013	0.1968	0.028*
C22	0.86095 (14)	−0.00041 (12)	0.05905 (12)	0.0327 (4)
H22	0.8525	−0.0612	0.0498	0.039*
C23	0.87764 (13)	0.05197 (12)	−0.01452 (12)	0.0308 (4)
H23	0.8817	0.0272	−0.0740	0.037*
C24	0.88851 (12)	0.14079 (12)	−0.00128 (12)	0.0257 (4)
H24	0.9003	0.1769	−0.0517	0.031*
C25	0.88221 (11)	0.17707 (11)	0.08506 (11)	0.0214 (4)
H25	0.8886	0.2381	0.0934	0.026*
C26	0.75306 (11)	0.22975 (10)	0.27313 (10)	0.0156 (3)
C27	0.70310 (11)	0.22562 (10)	0.35030 (11)	0.0185 (3)
H27	0.7270	0.1897	0.4020	0.022*
C28	0.61916 (11)	0.27358 (10)	0.35174 (12)	0.0224 (4)
H28	0.5855	0.2704	0.4043	0.027*
C29	0.58382 (12)	0.32645 (10)	0.27659 (12)	0.0252 (4)
H29	0.5263	0.3597	0.2777	0.030*
C30	0.63304 (12)	0.33036 (11)	0.20009 (12)	0.0265 (4)
H30	0.6088	0.3662	0.1485	0.032*
C31	0.71692 (11)	0.28270 (10)	0.19801 (11)	0.0216 (4)
H31	0.7502	0.2860	0.1451	0.026*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.01547 (12)	0.01379 (12)	0.01783 (12)	0.00070 (9)	0.00372 (9)	0.00033 (9)
Fe2	0.01568 (12)	0.01181 (12)	0.01079 (11)	−0.00046 (8)	0.00202 (8)	0.00040 (8)
P1	0.0163 (2)	0.0118 (2)	0.01058 (19)	−0.00003 (15)	0.00202 (15)	0.00057 (15)
P2	0.0160 (2)	0.0135 (2)	0.01251 (19)	−0.00015 (15)	0.00168 (15)	0.00074 (15)
S1	0.0216 (2)	0.0164 (2)	0.01245 (19)	0.00252 (16)	0.00080 (15)	0.00018 (15)
S2	0.0180 (2)	0.0133 (2)	0.0166 (2)	−0.00165 (15)	0.00262 (15)	−0.00067 (15)
O1	0.0367 (7)	0.0210 (7)	0.0332 (7)	0.0076 (5)	0.0084 (6)	0.0089 (6)
O2	0.0249 (7)	0.0301 (8)	0.0672 (11)	−0.0091 (6)	0.0033 (7)	−0.0059 (7)
O3	0.0429 (8)	0.0386 (8)	0.0332 (8)	−0.0044 (6)	0.0223 (7)	−0.0082 (6)
O4	0.0317 (7)	0.0245 (7)	0.0378 (8)	−0.0127 (6)	−0.0031 (6)	0.0043 (6)
O5	0.0450 (8)	0.0307 (7)	0.0149 (6)	0.0051 (6)	0.0088 (6)	0.0003 (5)
O6	0.0208 (6)	0.0153 (6)	0.0174 (6)	−0.0001 (4)	0.0044 (5)	0.0040 (5)
C1	0.0178 (9)	0.0233 (10)	0.0224 (9)	0.0015 (7)	0.0059 (7)	−0.0028 (7)
C2	0.0224 (10)	0.0193 (9)	0.0341 (10)	0.0032 (7)	0.0069 (8)	0.0000 (8)
C3	0.0235 (9)	0.0171 (9)	0.0303 (10)	−0.0024 (7)	0.0083 (8)	0.0009 (7)
C4	0.0229 (9)	0.0187 (9)	0.0152 (8)	0.0021 (7)	−0.0007 (6)	0.0022 (7)
C5	0.0231 (9)	0.0126 (8)	0.0201 (9)	0.0006 (6)	0.0038 (7)	0.0004 (7)
C6	0.0242 (9)	0.0216 (9)	0.0190 (9)	0.0043 (7)	0.0100 (7)	0.0081 (7)
C7	0.0198 (9)	0.0160 (9)	0.0241 (9)	−0.0004 (6)	0.0083 (7)	0.0062 (7)
C8	0.0216 (8)	0.0162 (8)	0.0117 (8)	0.0048 (6)	−0.0002 (6)	−0.0015 (6)
C9	0.0349 (10)	0.0230 (9)	0.0198 (9)	−0.0062 (7)	0.0040 (7)	−0.0029 (7)
C10	0.0465 (12)	0.0260 (10)	0.0241 (10)	−0.0026 (8)	−0.0007 (8)	−0.0094 (8)
C11	0.0419 (12)	0.0354 (11)	0.0147 (9)	0.0088 (9)	0.0010 (8)	−0.0093 (8)
C12	0.0296 (10)	0.0450 (12)	0.0175 (9)	0.0072 (8)	0.0078 (7)	−0.0010 (8)
C13	0.0216 (9)	0.0253 (10)	0.0158 (8)	0.0043 (7)	0.0023 (7)	−0.0009 (7)
C14	0.0170 (8)	0.0127 (8)	0.0148 (8)	−0.0018 (6)	−0.0008 (6)	0.0007 (6)
C15	0.0203 (9)	0.0150 (8)	0.0205 (8)	−0.0011 (6)	0.0032 (7)	0.0012 (7)
C16	0.0294 (10)	0.0226 (9)	0.0215 (9)	−0.0025 (7)	0.0014 (7)	0.0079 (7)
C17	0.0284 (10)	0.0150 (9)	0.0312 (10)	0.0007 (7)	−0.0050 (8)	0.0072 (7)
C18	0.0252 (10)	0.0165 (9)	0.0336 (10)	0.0052 (7)	0.0007 (8)	−0.0004 (7)
C19	0.0239 (9)	0.0174 (9)	0.0219 (9)	0.0002 (7)	0.0040 (7)	0.0006 (7)
C20	0.0152 (8)	0.0194 (9)	0.0150 (8)	0.0009 (6)	0.0005 (6)	−0.0022 (6)
C21	0.0318 (10)	0.0195 (9)	0.0186 (9)	0.0011 (7)	0.0021 (7)	−0.0014 (7)
C22	0.0524 (13)	0.0205 (10)	0.0243 (10)	0.0032 (8)	0.0018 (9)	−0.0067 (8)
C23	0.0390 (11)	0.0365 (11)	0.0164 (9)	0.0011 (8)	0.0022 (8)	−0.0093 (8)
C24	0.0270 (10)	0.0329 (11)	0.0170 (9)	−0.0052 (8)	0.0028 (7)	−0.0006 (7)
C25	0.0240 (9)	0.0211 (9)	0.0186 (8)	−0.0040 (7)	0.0012 (7)	−0.0015 (7)
C26	0.0156 (8)	0.0138 (8)	0.0171 (8)	−0.0016 (6)	0.0011 (6)	−0.0003 (6)
C27	0.0192 (8)	0.0180 (9)	0.0179 (8)	−0.0032 (6)	0.0018 (6)	0.0001 (7)
C28	0.0196 (9)	0.0245 (9)	0.0239 (9)	−0.0035 (7)	0.0057 (7)	−0.0054 (7)
C29	0.0183 (9)	0.0213 (9)	0.0348 (10)	0.0037 (7)	0.0002 (7)	−0.0053 (8)
C30	0.0247 (9)	0.0248 (10)	0.0282 (10)	0.0065 (7)	−0.0019 (8)	0.0062 (8)
C31	0.0220 (9)	0.0231 (9)	0.0197 (9)	0.0006 (7)	0.0031 (7)	0.0022 (7)

Geometric parameters (Å, º) top

Fe1—C2	1.7855 (18)	C12—C13	1.392 (2)
Fe1—C1	1.7981 (17)	C12—H12	0.9500
Fe1—C3	1.8006 (18)	C13—H13	0.9500
Fe1—S1	2.2484 (6)	C14—C15	1.391 (2)
Fe1—S2	2.2495 (8)	C14—C19	1.395 (2)
Fe1—Fe2	2.5275 (6)	C15—C16	1.390 (2)
Fe2—C4	1.7733 (17)	C15—H15	0.9500
Fe2—C5	1.7742 (17)	C16—C17	1.378 (2)
Fe2—P1	2.2426 (7)	C16—H16	0.9500
Fe2—S1	2.2495 (7)	C17—C18	1.386 (2)
Fe2—S2	2.2530 (7)	C17—H17	0.9500
P1—C8	1.8353 (16)	C18—C19	1.386 (2)
P1—C14	1.8371 (16)	C18—H18	0.9500
P1—P2	2.2519 (8)	C19—H19	0.9500
P2—O6	1.4943 (11)	C20—C21	1.392 (2)
P2—C20	1.8049 (16)	C20—C25	1.397 (2)
P2—C26	1.8066 (16)	C21—C22	1.384 (2)
S1—C6	1.8264 (16)	C21—H21	0.9500
S2—C7	1.8219 (16)	C22—C23	1.381 (2)
O1—C1	1.1461 (19)	C22—H22	0.9500
O2—C2	1.145 (2)	C23—C24	1.386 (2)
O3—C3	1.1414 (19)	C23—H23	0.9500
O4—C4	1.1476 (18)	C24—C25	1.382 (2)
O5—C5	1.1496 (19)	C24—H24	0.9500
C6—C7	1.523 (2)	C25—H25	0.9500
C6—H6A	0.9900	C26—C31	1.392 (2)
C6—H6B	0.9900	C26—C27	1.398 (2)
C7—H7A	0.9900	C27—C28	1.381 (2)
C7—H7B	0.9900	C27—H27	0.9500
C8—C9	1.396 (2)	C28—C29	1.389 (2)
C8—C13	1.396 (2)	C28—H28	0.9500
C9—C10	1.383 (2)	C29—C30	1.383 (2)
C9—H9	0.9500	C29—H29	0.9500
C10—C11	1.381 (2)	C30—C31	1.379 (2)
C10—H10	0.9500	C30—H30	0.9500
C11—C12	1.378 (3)	C31—H31	0.9500
C11—H11	0.9500

C2—Fe1—C1	101.48 (8)	C10—C9—H9	119.4
C2—Fe1—C3	92.93 (8)	C8—C9—H9	119.4
C1—Fe1—C3	99.62 (7)	C11—C10—C9	119.85 (17)
C2—Fe1—S1	88.39 (6)	C11—C10—H10	120.1
C1—Fe1—S1	100.81 (5)	C9—C10—H10	120.1
C3—Fe1—S1	158.84 (6)	C12—C11—C10	119.80 (16)
C2—Fe1—S2	159.44 (5)	C12—C11—H11	120.1
C1—Fe1—S2	97.57 (5)	C10—C11—H11	120.1
C3—Fe1—S2	91.43 (6)	C11—C12—C13	120.83 (16)
S1—Fe1—S2	80.48 (2)	C11—C12—H12	119.6
C2—Fe1—Fe2	103.55 (6)	C13—C12—H12	119.6
C1—Fe1—Fe2	144.71 (5)	C12—C13—C8	119.83 (16)
C3—Fe1—Fe2	103.51 (6)	C12—C13—H13	120.1
S1—Fe1—Fe2	55.831 (19)	C8—C13—H13	120.1
S2—Fe1—Fe2	55.91 (2)	C15—C14—C19	118.50 (14)
C4—Fe2—C5	89.47 (7)	C15—C14—P1	120.51 (11)
C4—Fe2—P1	96.70 (6)	C19—C14—P1	120.96 (12)
C5—Fe2—P1	102.94 (5)	C16—C15—C14	120.49 (15)
C4—Fe2—S1	92.92 (5)	C16—C15—H15	119.8
C5—Fe2—S1	157.08 (5)	C14—C15—H15	119.8
P1—Fe2—S1	99.41 (2)	C17—C16—C15	120.46 (16)
C4—Fe2—S2	153.40 (5)	C17—C16—H16	119.8
C5—Fe2—S2	87.33 (5)	C15—C16—H16	119.8
P1—Fe2—S2	109.75 (2)	C16—C17—C18	119.65 (15)
S1—Fe2—S2	80.385 (18)	C16—C17—H17	120.2
C4—Fe2—Fe1	99.20 (6)	C18—C17—H17	120.2
C5—Fe2—Fe1	101.33 (5)	C19—C18—C17	120.06 (15)
P1—Fe2—Fe1	150.983 (16)	C19—C18—H18	120.0
S1—Fe2—Fe1	55.791 (13)	C17—C18—H18	120.0
S2—Fe2—Fe1	55.79 (2)	C18—C19—C14	120.81 (15)
C8—P1—C14	100.18 (7)	C18—C19—H19	119.6
C8—P1—Fe2	114.85 (5)	C14—C19—H19	119.6
C14—P1—Fe2	119.36 (5)	C21—C20—C25	118.86 (14)
C8—P1—P2	104.48 (5)	C21—C20—P2	116.48 (12)
C14—P1—P2	102.27 (5)	C25—C20—P2	124.64 (12)
Fe2—P1—P2	113.64 (3)	C22—C21—C20	120.49 (16)
O6—P2—C20	112.94 (7)	C22—C21—H21	119.8
O6—P2—C26	111.20 (6)	C20—C21—H21	119.8
C20—P2—C26	107.80 (7)	C23—C22—C21	120.24 (17)
O6—P2—P1	109.43 (5)	C23—C22—H22	119.9
C20—P2—P1	104.22 (5)	C21—C22—H22	119.9
C26—P2—P1	111.04 (6)	C22—C23—C24	119.80 (16)
C6—S1—Fe1	102.29 (6)	C22—C23—H23	120.1
C6—S1—Fe2	104.41 (6)	C24—C23—H23	120.1
Fe1—S1—Fe2	68.38 (2)	C25—C24—C23	120.25 (16)
C7—S2—Fe1	100.03 (6)	C25—C24—H24	119.9
C7—S2—Fe2	106.78 (5)	C23—C24—H24	119.9
Fe1—S2—Fe2	68.299 (13)	C24—C25—C20	120.35 (16)
O1—C1—Fe1	176.91 (14)	C24—C25—H25	119.8
O2—C2—Fe1	178.68 (16)	C20—C25—H25	119.8
O3—C3—Fe1	178.89 (16)	C31—C26—C27	119.05 (14)
O4—C4—Fe2	175.95 (15)	C31—C26—P2	123.97 (12)
O5—C5—Fe2	175.41 (15)	C27—C26—P2	116.97 (12)
C7—C6—S1	112.22 (10)	C28—C27—C26	120.28 (15)
C7—C6—H6A	109.2	C28—C27—H27	119.9
S1—C6—H6A	109.2	C26—C27—H27	119.9
C7—C6—H6B	109.2	C27—C28—C29	120.26 (15)
S1—C6—H6B	109.2	C27—C28—H28	119.9
H6A—C6—H6B	107.9	C29—C28—H28	119.9
C6—C7—S2	111.97 (10)	C30—C29—C28	119.49 (15)
C6—C7—H7A	109.2	C30—C29—H29	120.3
S2—C7—H7A	109.2	C28—C29—H29	120.3
C6—C7—H7B	109.2	C31—C30—C29	120.67 (16)
S2—C7—H7B	109.2	C31—C30—H30	119.7
H7A—C7—H7B	107.9	C29—C30—H30	119.7
C9—C8—C13	118.54 (14)	C30—C31—C26	120.25 (15)
C9—C8—P1	116.08 (12)	C30—C31—H31	119.9
C13—C8—P1	125.37 (12)	C26—C31—H31	119.9
C10—C9—C8	121.13 (16)

C2—Fe1—Fe2—C4	8.72 (8)	C5—Fe2—S2—C7	−160.02 (8)
C1—Fe1—Fe2—C4	142.75 (11)	P1—Fe2—S2—C7	−57.23 (6)
C3—Fe1—Fe2—C4	−87.70 (7)	S1—Fe2—S2—C7	39.40 (6)
S1—Fe1—Fe2—C4	87.27 (5)	Fe1—Fe2—S2—C7	94.35 (6)
S2—Fe1—Fe2—C4	−170.14 (5)	C4—Fe2—S2—Fe1	22.18 (11)
C2—Fe1—Fe2—C5	100.03 (8)	C5—Fe2—S2—Fe1	105.64 (5)
C1—Fe1—Fe2—C5	−125.94 (11)	P1—Fe2—S2—Fe1	−151.57 (2)
C3—Fe1—Fe2—C5	3.60 (7)	S1—Fe2—S2—Fe1	−54.945 (14)
S1—Fe1—Fe2—C5	178.57 (5)	C4—Fe2—C5—O5	70.8 (18)
S2—Fe1—Fe2—C5	−78.83 (5)	P1—Fe2—C5—O5	167.5 (18)
C2—Fe1—Fe2—P1	−113.67 (7)	S1—Fe2—C5—O5	−25.5 (19)
C1—Fe1—Fe2—P1	20.35 (10)	S2—Fe2—C5—O5	−82.8 (18)
C3—Fe1—Fe2—P1	149.90 (6)	Fe1—Fe2—C5—O5	−28.5 (18)
S1—Fe1—Fe2—P1	−35.13 (3)	Fe1—S1—C6—C7	−31.06 (12)
S2—Fe1—Fe2—P1	67.46 (4)	Fe2—S1—C6—C7	39.46 (12)
C2—Fe1—Fe2—S1	−78.54 (6)	S1—C6—C7—S2	−8.36 (15)
C1—Fe1—Fe2—S1	55.48 (9)	Fe1—S2—C7—C6	43.88 (11)
C3—Fe1—Fe2—S1	−174.97 (6)	Fe2—S2—C7—C6	−26.31 (12)
S2—Fe1—Fe2—S1	102.59 (2)	C14—P1—C8—C9	−60.76 (14)
C2—Fe1—Fe2—S2	178.86 (6)	Fe2—P1—C8—C9	68.45 (13)
C1—Fe1—Fe2—S2	−47.11 (9)	P2—P1—C8—C9	−166.39 (12)
C3—Fe1—Fe2—S2	82.44 (5)	C14—P1—C8—C13	117.87 (14)
S1—Fe1—Fe2—S2	−102.59 (2)	Fe2—P1—C8—C13	−112.92 (13)
C4—Fe2—P1—C8	−73.60 (8)	P2—P1—C8—C13	12.24 (14)
C5—Fe2—P1—C8	−164.59 (8)	C13—C8—C9—C10	−1.0 (3)
S1—Fe2—P1—C8	20.50 (6)	P1—C8—C9—C10	177.70 (14)
S2—Fe2—P1—C8	103.59 (6)	C8—C9—C10—C11	−0.2 (3)
Fe1—Fe2—P1—C8	49.34 (7)	C9—C10—C11—C12	1.2 (3)
C4—Fe2—P1—C14	45.35 (8)	C10—C11—C12—C13	−1.1 (3)
C5—Fe2—P1—C14	−45.64 (8)	C11—C12—C13—C8	−0.2 (3)
S1—Fe2—P1—C14	139.45 (6)	C9—C8—C13—C12	1.2 (2)
S2—Fe2—P1—C14	−137.46 (6)	P1—C8—C13—C12	−177.41 (13)
Fe1—Fe2—P1—C14	168.29 (6)	C8—P1—C14—C15	147.58 (13)
C4—Fe2—P1—P2	166.17 (5)	Fe2—P1—C14—C15	21.35 (15)
C5—Fe2—P1—P2	75.18 (5)	P2—P1—C14—C15	−105.03 (13)
S1—Fe2—P1—P2	−99.72 (2)	C8—P1—C14—C19	−34.57 (14)
S2—Fe2—P1—P2	−16.64 (3)	Fe2—P1—C14—C19	−160.80 (11)
Fe1—Fe2—P1—P2	−70.88 (4)	P2—P1—C14—C19	72.82 (13)
C8—P1—P2—O6	−56.30 (7)	C19—C14—C15—C16	−2.3 (2)
C14—P1—P2—O6	−160.36 (6)	P1—C14—C15—C16	175.62 (12)
Fe2—P1—P2—O6	69.63 (5)	C14—C15—C16—C17	1.5 (2)
C8—P1—P2—C20	−177.36 (7)	C15—C16—C17—C18	0.0 (3)
C14—P1—P2—C20	78.58 (7)	C16—C17—C18—C19	−0.5 (3)
Fe2—P1—P2—C20	−51.43 (6)	C17—C18—C19—C14	−0.4 (3)
C8—P1—P2—C26	66.83 (7)	C15—C14—C19—C18	1.7 (2)
C14—P1—P2—C26	−37.23 (7)	P1—C14—C19—C18	−176.14 (13)
Fe2—P1—P2—C26	−167.24 (5)	O6—P2—C20—C21	8.73 (15)
C2—Fe1—S1—C6	−151.58 (8)	C26—P2—C20—C21	−114.53 (13)
C1—Fe1—S1—C6	−50.20 (8)	P1—P2—C20—C21	127.42 (12)
C3—Fe1—S1—C6	114.47 (16)	O6—P2—C20—C25	−169.59 (13)
S2—Fe1—S1—C6	45.77 (6)	C26—P2—C20—C25	67.16 (15)
Fe2—Fe1—S1—C6	100.81 (6)	P1—P2—C20—C25	−50.90 (14)
C2—Fe1—S1—Fe2	107.60 (6)	C25—C20—C21—C22	−0.8 (2)
C1—Fe1—S1—Fe2	−151.01 (5)	P2—C20—C21—C22	−179.23 (14)
C3—Fe1—S1—Fe2	13.65 (15)	C20—C21—C22—C23	1.6 (3)
S2—Fe1—S1—Fe2	−55.042 (18)	C21—C22—C23—C24	−1.0 (3)
C4—Fe2—S1—C6	163.12 (7)	C22—C23—C24—C25	−0.3 (3)
C5—Fe2—S1—C6	−101.33 (14)	C23—C24—C25—C20	1.1 (3)
P1—Fe2—S1—C6	65.83 (6)	C21—C20—C25—C24	−0.5 (2)
S2—Fe2—S1—C6	−42.79 (5)	P2—C20—C25—C24	177.80 (13)
Fe1—Fe2—S1—C6	−97.73 (6)	O6—P2—C26—C31	−159.14 (13)
C4—Fe2—S1—Fe1	−99.14 (6)	C20—P2—C26—C31	−34.83 (16)
C5—Fe2—S1—Fe1	−3.59 (13)	P1—P2—C26—C31	78.75 (14)
P1—Fe2—S1—Fe1	163.565 (15)	O6—P2—C26—C27	19.76 (14)
S2—Fe2—S1—Fe1	54.94 (2)	C20—P2—C26—C27	144.07 (12)
C2—Fe1—S2—C7	−107.34 (17)	P1—P2—C26—C27	−102.35 (12)
C1—Fe1—S2—C7	50.53 (7)	C31—C26—C27—C28	−0.1 (2)
C3—Fe1—S2—C7	150.43 (7)	P2—C26—C27—C28	−179.03 (12)
S1—Fe1—S2—C7	−49.23 (5)	C26—C27—C28—C29	−0.1 (2)
Fe2—Fe1—S2—C7	−104.19 (5)	C27—C28—C29—C30	0.3 (2)
C2—Fe1—S2—Fe2	−3.15 (16)	C28—C29—C30—C31	−0.3 (3)
C1—Fe1—S2—Fe2	154.72 (5)	C29—C30—C31—C26	0.1 (3)
C3—Fe1—S2—Fe2	−105.38 (5)	C27—C26—C31—C30	0.1 (2)
S1—Fe1—S2—Fe2	54.960 (17)	P2—C26—C31—C30	178.96 (13)
C4—Fe2—S2—C7	116.53 (12)

Experimental details

Crystal data
Chemical formula	[Fe₂(C₂H₄S₂)(C₂₄H₂₀OP₂)(CO)₅]
M_r	730.26
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	113
a, b, c (Å)	13.865 (4), 15.398 (4), 14.459 (5)
β (°)	98.357 (4)
V (Å³)	3054.1 (16)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.24
Crystal size (mm)	0.20 × 0.18 × 0.10

Data collection
Diffractometer	Rigaku Saturn724 CCD diffractometer
Absorption correction	Multi-scan (CrystalClear; Rigaku/MSC, 2005)
T_min, T_max	0.790, 0.886
No. of measured, independent and observed [I > 2σ(I)] reflections	31351, 7281, 6102
R_int	0.039
(sin θ/λ)_max (Å⁻¹)	0.658

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.059, 1.06
No. of reflections	7281
No. of parameters	388
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	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—C2	1.7855 (18)	Fe2—C4	1.7733 (17)
Fe1—C1	1.7981 (17)	Fe2—C5	1.7742 (17)
Fe1—C3	1.8006 (18)	Fe2—P1	2.2426 (7)
Fe1—S1	2.2484 (6)	Fe2—S1	2.2495 (7)
Fe1—S2	2.2495 (8)	Fe2—S2	2.2530 (7)

Acknowledgements

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

References

Rigaku/MSC (2005). CrystalClear and CrystalStructure. Rigaku/MSC Inc. The Woodlands, Texas, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
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. Web of Science CSD CrossRef CAS Google Scholar
Wang, 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
Yin, 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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