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In the title compound, [Fe2(C3H5O2S)2(CO)6], the asymmetric unit contains only one-half of the mol­ecule and the central [Fe2S2] fragment possesses a butterfly form on a twofold rotation axis. Each Fe atom is in a distorted tetra­gonal–pyramidal geometry and both C atoms bonded to sulfur are in equatorial positions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806000298/hk6073sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806000298/hk6073Isup2.hkl
Contains datablock I

CCDC reference: 298467

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.027
  • wR factor = 0.074
  • Data-to-parameter ratio = 14.3

checkCIF/PLATON results

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Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - C4 .. 8.21 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - C5 .. 9.40 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - C6 .. 7.93 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 5 C6 -FE1 -C4 -O1 -77.00 11.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 6 C5 -FE1 -C4 -O1 17.00 0.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 7 S1 -FE1 -C4 -O1 96.00 11.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 8 S1 -FE1 -C4 -O1 19.00 11.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 9 FE1 -FE1 -C4 -O1 55.00 11.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 10 C6 -FE1 -C5 -O2 -86.00 15.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 11 C4 -FE1 -C5 -O2 14.00 15.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 12 S1 -FE1 -C5 -O2 115.00 15.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 13 S1 -FE1 -C5 -O2 17.00 0.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 14 FE1 -FE1 -C5 -O2 17.00 0.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 15 C5 -FE1 -C6 -O3 44.00 16.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 16 C4 -FE1 -C6 -O3 -56.00 16.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 17 S1 -FE1 -C6 -O3 146.00 16.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 18 S1 -FE1 -C6 -O3 -155.00 16.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 19 FE1 -FE1 -C6 -O3 149.00 16.00 2.755 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 20 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 15 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: SHELXTL.

Bis(µ-methyl mercaptoacetato-κ2S:S)bis[tricarbonyliron(II)] top
Crystal data top
[Fe2(C3H5O2S)2(CO)6]F(000) = 984
Mr = 490.02Dx = 1.768 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 1715 reflections
a = 24.339 (4) Åθ = 2.3–25.5°
b = 5.9939 (9) ŵ = 1.85 mm1
c = 17.033 (3) ÅT = 298 K
β = 132.189 (1)°Block, red
V = 1841.1 (5) Å30.58 × 0.45 × 0.34 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
1715 independent reflections
Radiation source: fine-focus sealed tube1602 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
φ and ω scansθmax = 25.5°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1429
Tmin = 0.385, Tmax = 0.533k = 67
4695 measured reflectionsl = 2017
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.074 w = 1/[σ2(Fo2) + (0.045P)2 + 1.3935P]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
1715 reflectionsΔρmax = 0.47 e Å3
120 parametersΔρmin = 0.26 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0246 (10)
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
xyzUiso*/Ueq
Fe10.933850 (15)0.29751 (5)0.16129 (2)0.02989 (16)
O10.80343 (13)0.0301 (5)0.00692 (18)0.0907 (8)
O20.93596 (12)0.6129 (4)0.03270 (17)0.0669 (6)
O30.86077 (12)0.6267 (4)0.19097 (19)0.0686 (6)
O40.88302 (12)0.1062 (4)0.38135 (16)0.0741 (7)
O50.81871 (10)0.1078 (4)0.23780 (16)0.0628 (5)
C10.94441 (14)0.1826 (4)0.3696 (2)0.0436 (6)
H1A0.98460.16730.44560.052*
H1B0.93020.33850.35360.052*
C20.87976 (13)0.0438 (5)0.33262 (19)0.0439 (5)
C30.75257 (16)0.0196 (7)0.1898 (3)0.0824 (11)
H3A0.75480.15840.16390.124*
H3B0.71000.06340.13190.124*
H3C0.74880.04860.24150.124*
C40.85337 (14)0.1338 (5)0.0565 (2)0.0487 (6)
C50.93573 (13)0.4910 (4)0.08332 (18)0.0423 (5)
C60.88950 (12)0.4984 (4)0.18017 (18)0.0414 (5)
S10.97455 (3)0.08719 (9)0.30169 (4)0.03411 (18)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0238 (2)0.0350 (2)0.0271 (2)0.00011 (11)0.01561 (17)0.00044 (10)
O10.0569 (13)0.0960 (17)0.0680 (14)0.0357 (13)0.0210 (12)0.0290 (13)
O20.0771 (14)0.0678 (12)0.0624 (12)0.0039 (11)0.0495 (12)0.0207 (11)
O30.0616 (13)0.0582 (12)0.0944 (16)0.0091 (10)0.0558 (13)0.0100 (11)
O40.0633 (13)0.0966 (16)0.0578 (12)0.0221 (12)0.0387 (11)0.0135 (12)
O50.0363 (9)0.0668 (12)0.0676 (12)0.0017 (9)0.0277 (9)0.0134 (10)
C10.0422 (13)0.0596 (15)0.0384 (12)0.0061 (11)0.0309 (11)0.0028 (10)
C20.0405 (13)0.0586 (14)0.0433 (13)0.0028 (11)0.0325 (11)0.0026 (11)
C30.0338 (14)0.080 (2)0.101 (3)0.0031 (15)0.0320 (17)0.001 (2)
C40.0391 (13)0.0530 (14)0.0442 (13)0.0052 (12)0.0240 (12)0.0048 (12)
C50.0357 (12)0.0500 (13)0.0363 (11)0.0046 (10)0.0222 (10)0.0035 (10)
C60.0328 (11)0.0451 (12)0.0424 (12)0.0014 (10)0.0236 (10)0.0003 (10)
S10.0326 (3)0.0373 (3)0.0368 (3)0.0007 (2)0.0250 (3)0.0027 (2)
Geometric parameters (Å, º) top
Fe1—C61.785 (2)O5—C21.319 (3)
Fe1—C51.787 (2)O5—C31.440 (4)
Fe1—C41.814 (3)C1—C21.494 (3)
Fe1—S1i2.2515 (6)C1—S11.828 (2)
Fe1—S12.2600 (7)C1—H1A0.9700
Fe1—Fe1i2.5359 (6)C1—H1B0.9700
O1—C41.126 (3)C3—H3A0.9600
O2—C51.133 (3)C3—H3B0.9600
O3—C61.134 (3)C3—H3C0.9600
O4—C21.190 (3)S1—Fe1i2.2515 (6)
C6—Fe1—C590.94 (11)C2—C1—H1B110.0
C6—Fe1—C499.09 (12)S1—C1—H1B110.0
C5—Fe1—C499.77 (12)H1A—C1—H1B108.4
C6—Fe1—S1i158.81 (8)O4—C2—O5124.5 (2)
C5—Fe1—S1i93.26 (8)O4—C2—C1124.7 (2)
C4—Fe1—S1i100.64 (9)O5—C2—C1110.8 (2)
C6—Fe1—S194.25 (8)O5—C3—H3A109.5
C5—Fe1—S1159.51 (8)O5—C3—H3B109.5
C4—Fe1—S198.96 (9)H3A—C3—H3B109.5
S1i—Fe1—S175.13 (3)O5—C3—H3C109.5
C6—Fe1—Fe1i102.88 (7)H3A—C3—H3C109.5
C5—Fe1—Fe1i103.88 (8)H3B—C3—H3C109.5
C4—Fe1—Fe1i147.20 (9)O1—C4—Fe1178.5 (3)
S1i—Fe1—Fe1i55.957 (18)O2—C5—Fe1179.1 (3)
S1—Fe1—Fe1i55.641 (18)O3—C6—Fe1179.2 (2)
C2—O5—C3116.9 (2)C1—S1—Fe1i112.97 (8)
C2—C1—S1108.39 (16)C1—S1—Fe1114.71 (9)
C2—C1—H1A110.0Fe1i—S1—Fe168.402 (19)
S1—C1—H1A110.0
C3—O5—C2—O42.2 (4)C4—Fe1—C6—O356 (16)
C3—O5—C2—C1176.8 (2)S1i—Fe1—C6—O3146 (16)
S1—C1—C2—O4101.7 (3)S1—Fe1—C6—O3155 (16)
S1—C1—C2—O577.3 (2)Fe1i—Fe1—C6—O3149 (16)
C6—Fe1—C4—O177 (11)C2—C1—S1—Fe1i175.39 (15)
C5—Fe1—C4—O1169 (100)C2—C1—S1—Fe199.57 (17)
S1i—Fe1—C4—O196 (11)C6—Fe1—S1—C13.54 (12)
S1—Fe1—C4—O119 (11)C5—Fe1—S1—C1107.8 (2)
Fe1i—Fe1—C4—O155 (11)C4—Fe1—S1—C196.36 (12)
C6—Fe1—C5—O286 (15)S1i—Fe1—S1—C1164.91 (9)
C4—Fe1—C5—O214 (15)Fe1i—Fe1—S1—C1106.26 (9)
S1i—Fe1—C5—O2115 (15)C6—Fe1—S1—Fe1i102.71 (8)
S1—Fe1—C5—O2170 (100)C5—Fe1—S1—Fe1i1.5 (2)
Fe1i—Fe1—C5—O2171 (100)C4—Fe1—S1—Fe1i157.38 (9)
C5—Fe1—C6—O344 (16)S1i—Fe1—S1—Fe1i58.66 (3)
Symmetry code: (i) x+2, y, z+1/2.
 

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