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The title compound, [Fe4(SEt)2(S2)(CO)12], contains two inversion-related [Fe2(SEt)(CO)6] subclusters linked by a disulfide bond [S—S 2.1294 (14) Å]. In each subcluster, each FeII atom is coordinated by three terminal carbonyl C atoms [Fe—C 1.792 (3)–1.814 (4) Å], two bridging S atoms [Fe—S 2.2496 (9)–2.2606 (8) Å] and the other Fe atom [Fe—Fe = 2.5311 (7) Å], and exhibits a distorted octahedral geometry, with trans angles ranging from 155.56 (12) to 160.14 (15)°.
Supporting information
CCDC reference: 272003
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.006 Å
- R factor = 0.040
- wR factor = 0.094
- Data-to-parameter ratio = 18.8
checkCIF/PLATON results
No syntax errors found
Alert level A
DIFF019_ALERT_1_A _diffrn_standards_number is missing
Number of standards used in measurement.
DIFF020_ALERT_1_A _diffrn_standards_interval_count and
_diffrn_standards_interval_time are missing. Number of measurements
between standards or time (min) between standards.
Alert level C
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - C5 .. 5.26 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - C6 .. 5.98 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe2 - C1 .. 6.58 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe2 - C3 .. 7.00 su
2 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL (Siemens, 1994); molecular graphics: SHELXTL (Sheldrick, 1997); software used to prepare material for publication: SHELXTL (Sheldrick, 1997).
(µ
4-Disulfido-1:2
κ2S;3:4
κ2S')bis(µ
2-ethylthiolato-
κ2Fe,Fe')tetrakis[tricarbonyliron(II)(Fe—Fe)]
top
Crystal data top
[Fe4(C2H5)2(S2)(CO)12] | F(000) = 740 |
Mr = 745.88 | Dx = 1.839 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2637 reflections |
a = 10.4820 (11) Å | θ = 3.1–27.5° |
b = 13.1288 (15) Å | µ = 2.48 mm−1 |
c = 10.0749 (11) Å | T = 298 K |
β = 103.719 (4)° | Prism, red |
V = 1346.9 (3) Å3 | 0.25 × 0.20 × 0.10 mm |
Z = 2 | |
Data collection top
Bruker P4 diffractometer | 3070 independent reflections |
Radiation source: fine-focus sealed tube | 2417 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.525, Tmax = 0.781 | k = −17→16 |
10263 measured reflections | l = −12→12 |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0451P)2 + 0.0725P] where P = (Fo2 + 2Fc2)/3 |
3070 reflections | (Δ/σ)max = 0.001 |
163 parameters | Δρmax = 0.36 e Å−3 |
0 restraints | Δρmin = −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 | Uiso*/Ueq | |
Fe1 | 0.73694 (4) | 0.59944 (3) | 0.11792 (4) | 0.04750 (15) | |
Fe2 | 0.73302 (4) | 0.40770 (3) | 0.14287 (4) | 0.04290 (14) | |
S1 | 0.65680 (7) | 0.51829 (6) | 0.27782 (8) | 0.04353 (19) | |
S2 | 0.59438 (7) | 0.49581 (6) | −0.02187 (8) | 0.0467 (2) | |
C1 | 0.6401 (3) | 0.2968 (3) | 0.1720 (4) | 0.0584 (8) | |
C2 | 0.8054 (3) | 0.3616 (3) | 0.0097 (4) | 0.0631 (9) | |
C3 | 0.8830 (3) | 0.3841 (2) | 0.2677 (3) | 0.0536 (8) | |
C4 | 0.6511 (4) | 0.7187 (3) | 0.1163 (4) | 0.0674 (10) | |
C5 | 0.8100 (4) | 0.6194 (3) | −0.0244 (4) | 0.0753 (11) | |
C6 | 0.8880 (3) | 0.6320 (3) | 0.2371 (4) | 0.0594 (8) | |
C7 | 0.7598 (3) | 0.5298 (3) | 0.4504 (3) | 0.0577 (8) | |
H7A | 0.8502 | 0.5144 | 0.4497 | 0.069* | |
H7B | 0.7564 | 0.5992 | 0.4825 | 0.069* | |
C8 | 0.7144 (4) | 0.4585 (4) | 0.5448 (4) | 0.0852 (12) | |
H8A | 0.7696 | 0.4654 | 0.6352 | 0.128* | |
H8B | 0.7190 | 0.3898 | 0.5137 | 0.128* | |
H8C | 0.6254 | 0.4743 | 0.5464 | 0.128* | |
O1 | 0.5819 (3) | 0.2290 (2) | 0.1935 (3) | 0.0941 (10) | |
O2 | 0.8512 (3) | 0.3327 (3) | −0.0749 (3) | 0.0989 (10) | |
O3 | 0.9793 (2) | 0.3694 (2) | 0.3445 (3) | 0.0775 (8) | |
O4 | 0.5978 (3) | 0.7937 (2) | 0.1185 (4) | 0.1044 (11) | |
O5 | 0.8561 (3) | 0.6317 (3) | −0.1142 (3) | 0.1226 (14) | |
O6 | 0.9834 (3) | 0.6520 (2) | 0.3111 (3) | 0.0851 (8) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0326 (2) | 0.0574 (3) | 0.0506 (3) | −0.00636 (19) | 0.00611 (19) | 0.0052 (2) |
Fe2 | 0.0297 (2) | 0.0541 (3) | 0.0420 (3) | 0.00187 (18) | 0.00258 (17) | −0.00441 (19) |
S1 | 0.0344 (4) | 0.0536 (4) | 0.0418 (4) | −0.0013 (3) | 0.0076 (3) | −0.0023 (3) |
S2 | 0.0276 (3) | 0.0691 (5) | 0.0408 (4) | −0.0007 (3) | 0.0032 (3) | 0.0027 (3) |
C1 | 0.050 (2) | 0.063 (2) | 0.060 (2) | 0.0025 (17) | 0.0098 (17) | −0.0058 (17) |
C2 | 0.0383 (17) | 0.091 (3) | 0.055 (2) | 0.0068 (18) | 0.0010 (15) | −0.015 (2) |
C3 | 0.0434 (18) | 0.0610 (19) | 0.0538 (19) | 0.0054 (15) | 0.0063 (15) | −0.0092 (16) |
C4 | 0.056 (2) | 0.061 (2) | 0.084 (3) | −0.0052 (18) | 0.014 (2) | 0.013 (2) |
C5 | 0.047 (2) | 0.109 (3) | 0.068 (2) | −0.022 (2) | 0.0101 (18) | 0.013 (2) |
C6 | 0.0450 (19) | 0.066 (2) | 0.066 (2) | −0.0111 (17) | 0.0100 (17) | 0.0057 (18) |
C7 | 0.053 (2) | 0.074 (2) | 0.0422 (18) | 0.0007 (17) | 0.0045 (15) | −0.0083 (16) |
C8 | 0.079 (3) | 0.119 (3) | 0.054 (2) | 0.003 (3) | 0.009 (2) | 0.020 (2) |
O1 | 0.096 (2) | 0.0720 (17) | 0.120 (3) | −0.0223 (16) | 0.037 (2) | −0.0019 (17) |
O2 | 0.076 (2) | 0.151 (3) | 0.0732 (19) | 0.0187 (19) | 0.0257 (16) | −0.0343 (19) |
O3 | 0.0467 (14) | 0.102 (2) | 0.0691 (17) | 0.0137 (14) | −0.0154 (12) | −0.0072 (15) |
O4 | 0.102 (2) | 0.0674 (17) | 0.148 (3) | 0.0162 (17) | 0.039 (2) | 0.0170 (19) |
O5 | 0.091 (2) | 0.207 (4) | 0.080 (2) | −0.050 (2) | 0.0404 (19) | 0.013 (2) |
O6 | 0.0512 (15) | 0.109 (2) | 0.0843 (19) | −0.0266 (16) | −0.0052 (14) | 0.0008 (17) |
Geometric parameters (Å, º) top
Fe1—C6 | 1.797 (4) | C1—O1 | 1.129 (4) |
Fe1—C5 | 1.798 (4) | C2—O2 | 1.137 (4) |
Fe1—C4 | 1.804 (4) | C3—O3 | 1.134 (4) |
Fe1—S2 | 2.2515 (9) | C4—O4 | 1.134 (4) |
Fe1—S1 | 2.2535 (8) | C5—O5 | 1.133 (4) |
Fe1—Fe2 | 2.5311 (7) | C6—O6 | 1.127 (4) |
Fe2—C3 | 1.792 (3) | C7—C8 | 1.491 (5) |
Fe2—C2 | 1.797 (3) | C7—H7A | 0.9700 |
Fe2—C1 | 1.814 (4) | C7—H7B | 0.9700 |
Fe2—S2 | 2.2496 (9) | C8—H8A | 0.9600 |
Fe2—S1 | 2.2606 (8) | C8—H8B | 0.9600 |
S1—C7 | 1.823 (3) | C8—H8C | 0.9600 |
S2—S2i | 2.1294 (14) | | |
| | | |
C6—Fe1—C5 | 91.35 (16) | C1—Fe2—Fe1 | 146.75 (10) |
C6—Fe1—C4 | 99.12 (17) | S2—Fe2—Fe1 | 55.82 (2) |
C5—Fe1—C4 | 99.93 (19) | S1—Fe2—Fe1 | 55.76 (2) |
C6—Fe1—S2 | 155.56 (12) | C7—S1—Fe1 | 113.95 (12) |
C5—Fe1—S2 | 86.23 (13) | C7—S1—Fe2 | 114.38 (12) |
C4—Fe1—S2 | 105.25 (12) | Fe1—S1—Fe2 | 68.21 (3) |
C6—Fe1—S1 | 93.07 (11) | S2i—S2—Fe2 | 110.08 (5) |
C5—Fe1—S1 | 160.14 (15) | S2i—S2—Fe1 | 110.53 (5) |
C4—Fe1—S1 | 98.46 (12) | Fe2—S2—Fe1 | 68.43 (3) |
S2—Fe1—S1 | 81.77 (3) | O1—C1—Fe2 | 178.1 (3) |
C6—Fe1—Fe2 | 101.68 (11) | O2—C2—Fe2 | 179.8 (4) |
C5—Fe1—Fe2 | 104.12 (15) | O3—C3—Fe2 | 178.5 (3) |
C4—Fe1—Fe2 | 147.59 (11) | O4—C4—Fe1 | 178.4 (4) |
S2—Fe1—Fe2 | 55.75 (2) | O5—C5—Fe1 | 179.8 (5) |
S1—Fe1—Fe2 | 56.03 (2) | O6—C6—Fe1 | 179.4 (4) |
C3—Fe2—C2 | 90.59 (14) | C8—C7—S1 | 110.5 (3) |
C3—Fe2—C1 | 99.40 (16) | C8—C7—H7A | 109.6 |
C2—Fe2—C1 | 100.86 (16) | S1—C7—H7A | 109.6 |
C3—Fe2—S2 | 155.83 (11) | C8—C7—H7B | 109.6 |
C2—Fe2—S2 | 86.31 (12) | S1—C7—H7B | 109.6 |
C1—Fe2—S2 | 104.73 (11) | H7A—C7—H7B | 108.1 |
C3—Fe2—S1 | 93.74 (10) | C7—C8—H8A | 109.5 |
C2—Fe2—S1 | 159.73 (13) | C7—C8—H8B | 109.5 |
C1—Fe2—S1 | 97.94 (10) | H8A—C8—H8B | 109.5 |
S2—Fe2—S1 | 81.65 (3) | C7—C8—H8C | 109.5 |
C3—Fe2—Fe1 | 102.08 (11) | H8A—C8—H8C | 109.5 |
C2—Fe2—Fe1 | 103.97 (13) | H8B—C8—H8C | 109.5 |
Symmetry code: (i) −x+1, −y+1, −z. |
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