metal-organic compounds
The title complex, tris(O-methyldithiocarbonato)iron(III), [Fe(S2COCH3)3], has an approximate threefold rotation axis passing through the Fe atom. The Fe atom is coordinated by six S atoms in a distorted octahedral arrangement. The six Fe-S distances range from 2.299 (1) to 2.319 (1) Å, with an average of 2.307 (3) Å, showing that the Fe atom is in a low-spin state with short Fe-S distances.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802007808/ya6103sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802007808/ya6103Isup2.hkl |
CCDC reference: 189289
Computing details top
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1985); program(s) used to solve structure: MITHRIL (Gilmore, 1984); program(s) used to refine structure: TEXSAN; molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.
Tris(O-methyldithiocarbonato)iron(III) top
Crystal data top
[Fe(C2H3OS2)3] | F(000) = 764 |
Mr = 377.40 | Dx = 1.773 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71069 Å |
a = 11.329 (1) Å | Cell parameters from 25 reflections |
b = 13.595 (2) Å | θ = 16.2–16.5° |
c = 9.565 (1) Å | µ = 1.94 mm−1 |
β = 106.32 (1)° | T = 295 K |
V = 1413.8 (3) Å3 | Polyhedron, black |
Z = 4 | 0.47 × 0.42 × 0.42 mm |
Data collection top
Rigaku AFC-5S diffractometer | Rint = 0.031 |
Graphite monochromator | θmax = 27.5°, θmin = 2.5° |
ω/2θ scans | h = −14→14 |
Absorption correction: ψ scan (Molecular Structure Corporation, 1985) | k = 0→17 |
Tmin = 0.418, Tmax = 0.443 | l = 0→12 |
3585 measured reflections | 3 standard reflections every 150 reflections |
3249 independent reflections | intensity decay: 0.4% |
2467 reflections with I > 3σ(I) |
Refinement top
Refinement on F | 145 parameters |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.026 | Weighting scheme based on measured s.u.'s w = 1/σ2(F) |
wR(F2) = 0.034 | (Δ/σ)max = 0.002 |
S = 1.42 | Δρmax = 0.23 e Å−3 |
2467 reflections | Δρmin = −0.29 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Fe | 0.23337 (3) | 0.48706 (3) | 0.32440 (4) | 0.038 (1) | |
S1 | 0.36140 (7) | 0.41666 (6) | 0.20290 (7) | 0.053 (1) | |
S2 | 0.18086 (6) | 0.56375 (6) | 0.09871 (7) | 0.049 (1) | |
S3 | 0.37977 (6) | 0.59893 (6) | 0.44514 (7) | 0.048 (1) | |
S4 | 0.12502 (6) | 0.59750 (6) | 0.42406 (8) | 0.051 (1) | |
S5 | 0.27586 (7) | 0.37457 (6) | 0.51160 (7) | 0.054 (1) | |
S6 | 0.07684 (6) | 0.37410 (6) | 0.25378 (7) | 0.052 (1) | |
O1 | 0.3222 (2) | 0.4880 (2) | −0.0575 (2) | 0.060 (1) | |
O2 | 0.2697 (2) | 0.7329 (2) | 0.5720 (2) | 0.059 (1) | |
O3 | 0.1058 (2) | 0.2405 (2) | 0.4659 (2) | 0.060 (1) | |
C1 | 0.2894 (2) | 0.4916 (2) | 0.0644 (3) | 0.044 (1) | |
C2 | 0.2627 (2) | 0.6542 (2) | 0.4904 (3) | 0.044 (1) | |
C3 | 0.1451 (2) | 0.3196 (2) | 0.4135 (3) | 0.044 (3) | |
C4 | 0.2591 (3) | 0.5506 (3) | −0.1772 (3) | 0.072 (2) | |
C5 | 0.3881 (3) | 0.7794 (3) | 0.6294 (4) | 0.073 (2) | |
C6 | −0.0030 (3) | 0.1921 (3) | 0.3765 (4) | 0.075 (2) | |
H1 | 0.2691 | 0.6174 | −0.1471 | 0.082* | |
H2 | 0.2926 | 0.5410 | −0.2567 | 0.082* | |
H3 | 0.1740 | 0.5346 | −0.2064 | 0.082* | |
H4 | 0.4441 | 0.7339 | 0.6883 | 0.087* | |
H5 | 0.4184 | 0.8003 | 0.5511 | 0.087* | |
H6 | 0.3798 | 0.8348 | 0.6865 | 0.087* | |
H7 | −0.0704 | 0.2366 | 0.3562 | 0.089* | |
H8 | 0.0111 | 0.1714 | 0.2877 | 0.089* | |
H9 | −0.0214 | 0.1365 | 0.4269 | 0.089* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe | 0.0379 (2) | 0.0456 (2) | 0.0305 (2) | 0.0042 (2) | 0.0084 (1) | 0.0036 (2) |
S1 | 0.0592 (4) | 0.0602 (5) | 0.0395 (4) | 0.0259 (4) | 0.0141 (3) | 0.0072 (3) |
S2 | 0.0518 (4) | 0.0569 (4) | 0.0384 (3) | 0.0183 (3) | 0.0155 (3) | 0.0108 (3) |
S3 | 0.0401 (3) | 0.0549 (4) | 0.0497 (4) | −0.0005 (3) | 0.0140 (3) | −0.0034 (3) |
S4 | 0.0402 (3) | 0.0662 (5) | 0.0462 (4) | 0.0081 (3) | 0.0129 (3) | −0.0058 (3) |
S5 | 0.0561 (4) | 0.0599 (5) | 0.0387 (3) | −0.0030 (4) | 0.0011 (3) | 0.0119 (3) |
S6 | 0.0476 (4) | 0.0640 (5) | 0.0401 (4) | −0.0062 (3) | 0.0038 (3) | 0.0008 (3) |
O1 | 0.073 (1) | 0.075 (1) | 0.038 (1) | 0.023 (1) | 0.024 (1) | 0.007 (1) |
O2 | 0.063 (1) | 0.056 (1) | 0.051 (1) | 0.011 (1) | 0.006 (1) | −0.011 (1) |
O3 | 0.064 (1) | 0.056 (1) | 0.065 (1) | −0.008 (1) | 0.028 (1) | 0.007 (1) |
C1 | 0.050 (1) | 0.050 (2) | 0.034 (1) | 0.005 (1) | 0.012 (1) | 0.001 (1) |
C2 | 0.050 (1) | 0.048 (2) | 0.034 (1) | 0.007 (1) | 0.010 (1) | 0.004 (1) |
C3 | 0.048 (1) | 0.048 (2) | 0.042 (1) | 0.000 (1) | 0.018 (1) | 0.000 (1) |
C4 | 0.099 (3) | 0.084 (2) | 0.036 (1) | 0.022 (2) | 0.025 (2) | 0.015 (2) |
C5 | 0.081 (2) | 0.053 (2) | 0.071 (2) | 0.001 (2) | −0.003 (2) | −0.013 (2) |
C6 | 0.065 (2) | 0.059 (2) | 0.113 (3) | −0.015 (2) | 0.049 (2) | −0.012 (2) |
Geometric parameters (Å, º) top
Fe—S1 | 2.306 (1) | O2—C2 | 1.314 (3) |
Fe—S2 | 2.319 (1) | O2—C5 | 1.445 (4) |
Fe—S3 | 2.307 (1) | O3—C3 | 1.316 (3) |
Fe—S4 | 2.308 (1) | O3—C6 | 1.446 (4) |
Fe—S5 | 2.301 (1) | C4—H1 | 0.950 |
Fe—S6 | 2.299 (1) | C4—H2 | 0.950 |
S1—C1 | 1.688 (3) | C4—H3 | 0.950 |
S2—C1 | 1.676 (3) | C5—H4 | 0.950 |
S3—C2 | 1.683 (3) | C5—H5 | 0.950 |
S4—C2 | 1.696 (3) | C5—H6 | 0.950 |
S5—C3 | 1.689 (3) | C6—H7 | 0.950 |
S6—C3 | 1.678 (3) | C6—H8 | 0.950 |
O1—C1 | 1.321 (3) | C6—H9 | 0.950 |
O1—C4 | 1.444 (3) | ||
S1—Fe—S2 | 75.56 (3) | S3—C2—O2 | 126.6 (2) |
S1—Fe—S3 | 93.46 (3) | S4—C2—O2 | 119.2 (2) |
S1—Fe—S4 | 163.94 (3) | S5—C3—O3 | 119.2 (2) |
S1—Fe—S5 | 95.32 (3) | S6—C3—O3 | 126.1 (2) |
S1—Fe—S6 | 96.73 (3) | C1—O1—C4 | 118.6 (2) |
S2—Fe—S3 | 97.46 (3) | C2—O2—C5 | 118.5 (2) |
S2—Fe—S4 | 93.73 (3) | C3—O3—C6 | 118.1 (2) |
S2—Fe—S5 | 165.04 (3) | O1—C4—H1 | 109.48 |
S2—Fe—S6 | 92.98 (3) | O1—C4—H2 | 109.49 |
S3—Fe—S4 | 75.84 (3) | O1—C4—H3 | 109.47 |
S3—Fe—S5 | 94.87 (3) | O2—C5—H4 | 109.48 |
S3—Fe—S6 | 166.95 (3) | O2—C5—H5 | 109.48 |
S4—Fe—S5 | 97.48 (3) | O2—C5—H6 | 109.48 |
S4—Fe—S6 | 95.74 (3) | O3—C6—H7 | 109.48 |
S5—Fe—S6 | 76.11 (3) | O3—C6—H8 | 109.48 |
Fe—S1—C1 | 84.92 (9) | O3—C6—H9 | 109.49 |
Fe—S2—C1 | 84.77 (9) | H1—C4—H2 | 109.47 |
Fe—S3—C2 | 85.2 (1) | H1—C4—H3 | 109.45 |
Fe—S4—C2 | 84.83 (9) | H2—C4—H3 | 109.46 |
Fe—S5—C3 | 84.41 (9) | H4—C5—H5 | 109.46 |
Fe—S6—C3 | 84.7 (1) | H4—C5—H6 | 109.47 |
S1—C1—S2 | 114.8 (1) | H5—C5—H6 | 109.46 |
S3—C2—S4 | 114.2 (2) | H7—C6—H8 | 109.45 |
S5—C3—S6 | 114.7 (2) | H7—C6—H9 | 109.47 |
S1—C1—O1 | 118.5 (2) | H8—C6—H9 | 109.46 |
S2—C1—O1 | 126.8 (2) |