Iron methyl­xanthate

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.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](O-C) = 0.004 Å
• R factor = 0.026
• wR factor = 0.034
• Data-to-parameter ratio = 17.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

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Computing details

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)

Crystal data

[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) Å^3	Polyhedron, black
Z = 4	0.47 × 0.42 × 0.42 mm

Data collection

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

Refinement on F	145 parameters
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.026	Weighting scheme based on measured s.u.'s w = 1/σ^2(F)
wR(F^2) = 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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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)