trans-Bis(μ-2-hydroxy-ethanethiol-ato-κS:S)bis-[dinitro-syliron(II)](Fe-Fe).

The title complex, [Fe(2)(C(2)H(5)OS)(2)(NO)(4)], lies on a crystallographic inversion center. The Fe-Fe distance is characteristic of a metal-metal bond. In the crystal structure, inter-molecular O-H⋯O hydrogen bonds link complex mol-ecules into a two-dimensional network.

Related literature

For iron–nitrosyl complexes, see: Chiang et al. (2004 ▶); Dillinger et al. (2007 ▶); Mazany et al. (1983 ▶).

Experimental

Crystal data

[Fe2(C2H5OS)2(NO)4]

M = 385.98

Monoclinic,

a = 16.943 (3) Å

b = 5.0070 (7) Å

c = 14.931 (2) Å

β = 94.327 (3)°

V = 1263.1 (3) Å3

Z = 4

Mo Kα radiation

μ = 2.65 mm−1

T = 150 K

0.21 × 0.18 × 0.02 mm

Data collection

Bruker SMART APEXII diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.606, T max = 0.949

5708 measured reflections

1597 independent reflections

1240 reflections with I > 2σ

R int = 0.039

Refinement

R[F 2 > 2σ(F 2)] = 0.028

wR(F 2) = 0.061

S = 0.94

1597 reflections

83 parameters

H-atom parameters constrained

Δρmax = 0.52 e Å−3

Δρmin = −0.32 e Å−3

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: DIAMOND (Brandenburg, 1999 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809048065/lh2939sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809048065/lh2939Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Fe2(C2H5OS)2(NO)4]	F(000) = 776
Mr = 385.98	Dx = 2.030 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1286 reflections
a = 16.943 (3) Å	θ = 2.4–26.8°
b = 5.0070 (7) Å	µ = 2.65 mm−1
c = 14.931 (2) Å	T = 150 K
β = 94.327 (3)°	Plate, brown
V = 1263.1 (3) Å3	0.21 × 0.18 × 0.02 mm
Z = 4

Bruker SMART APEXII diffractometer	1597 independent reflections
Radiation source: fine-focus sealed tube	1240 reflections with I > 2σ
graphite	Rint = 0.039
ω scans	θmax = 28.7°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −22→22
Tmin = 0.606, Tmax = 0.949	k = −6→6
5708 measured reflections	l = −19→19

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)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.061	H-atom parameters constrained
S = 0.94	w = 1/[σ2(Fo2) + (0.0324P)2] where P = (Fo2 + 2Fc2)/3
1597 reflections	(Δ/σ)max = 0.003
83 parameters	Δρmax = 0.52 e Å−3
0 restraints	Δρmin = −0.32 e Å−3

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.

	x	y	z	Uiso*/Ueq
C1	0.89173 (13)	0.1311 (4)	0.14871 (15)	0.0189 (5)
H1A	0.8810	−0.0613	0.1385	0.023*
H1B	0.9190	0.1523	0.2093	0.023*
C2	0.81447 (12)	0.2848 (5)	0.14308 (15)	0.0219 (5)
H2A	0.8253	0.4791	0.1449	0.026*
H2B	0.7836	0.2436	0.0858	0.026*
Fe1	1.062332 (16)	−0.00956 (6)	0.06209 (2)	0.01677 (10)
N1	1.06466 (10)	−0.2257 (4)	0.14697 (12)	0.0200 (4)
N2	1.13967 (11)	0.1950 (4)	0.05687 (13)	0.0216 (4)
O1	1.07764 (10)	−0.3658 (3)	0.20944 (11)	0.0306 (4)
O2	1.19777 (10)	0.3213 (4)	0.06634 (13)	0.0370 (5)
O3	0.77015 (10)	0.2112 (3)	0.21691 (12)	0.0302 (4)
H3	0.7591	0.3487	0.2456	0.045*
S1	0.95465 (3)	0.25677 (10)	0.06417 (4)	0.01729 (13)

	U11	U22	U33	U12	U13	U23
C1	0.0256 (11)	0.0179 (11)	0.0142 (12)	−0.0014 (9)	0.0070 (8)	0.0007 (9)
C2	0.0243 (11)	0.0202 (12)	0.0220 (13)	−0.0032 (9)	0.0071 (9)	0.0006 (10)
Fe1	0.01897 (16)	0.01530 (17)	0.01622 (17)	−0.00062 (13)	0.00241 (11)	−0.00012 (13)
N1	0.0220 (9)	0.0206 (10)	0.0173 (10)	−0.0001 (8)	0.0012 (7)	−0.0025 (8)
N2	0.0225 (9)	0.0206 (10)	0.0224 (11)	−0.0002 (8)	0.0060 (8)	−0.0021 (8)
O1	0.0449 (10)	0.0241 (9)	0.0220 (10)	−0.0008 (8)	−0.0020 (8)	0.0069 (7)
O2	0.0276 (9)	0.0363 (11)	0.0477 (12)	−0.0119 (8)	0.0069 (8)	−0.0058 (9)
O3	0.0378 (9)	0.0235 (9)	0.0322 (11)	−0.0049 (8)	0.0222 (8)	−0.0037 (7)
S1	0.0212 (2)	0.0139 (3)	0.0174 (3)	−0.0006 (2)	0.00546 (19)	−0.0004 (2)

C1—C2	1.515 (3)	Fe1—N2	1.6696 (19)
C1—S1	1.824 (2)	Fe1—S1i	2.2555 (7)
C1—H1A	0.9900	Fe1—S1	2.2619 (6)
C1—H1B	0.9900	Fe1—Fe1i	2.7051 (6)
C2—O3	1.428 (2)	N1—O1	1.174 (2)
C2—H2A	0.9900	N2—O2	1.170 (2)
C2—H2B	0.9900	O3—H3	0.8400
Fe1—N1	1.6650 (19)	S1—Fe1i	2.2555 (7)
C2—C1—S1	109.51 (15)	N2—Fe1—S1i	110.41 (7)
C2—C1—H1A	109.8	N1—Fe1—S1	110.22 (6)
S1—C1—H1A	109.8	N2—Fe1—S1	106.00 (7)
C2—C1—H1B	109.8	S1i—Fe1—S1	106.43 (2)
S1—C1—H1B	109.8	N1—Fe1—Fe1i	121.14 (6)
H1A—C1—H1B	108.2	N2—Fe1—Fe1i	121.42 (7)
O3—C2—C1	109.18 (18)	S1i—Fe1—Fe1i	53.324 (17)
O3—C2—H2A	109.8	S1—Fe1—Fe1i	53.106 (18)
C1—C2—H2A	109.8	O1—N1—Fe1	170.09 (16)
O3—C2—H2B	109.8	O2—N2—Fe1	169.24 (18)
C1—C2—H2B	109.8	C2—O3—H3	109.5
H2A—C2—H2B	108.3	C1—S1—Fe1i	110.16 (7)
N1—Fe1—N2	117.44 (9)	C1—S1—Fe1	108.68 (7)
N1—Fe1—S1i	105.88 (7)	Fe1i—S1—Fe1	73.57 (2)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3···O3ii	0.84	1.97	2.7950 (14)	166

Fe1—N1	1.6650 (19)
Fe1—S1i	2.2555 (7)
Fe1—S1	2.2619 (6)
Fe1—Fe1i	2.7051 (6)

N1—Fe1—N2	117.44 (9)
N1—Fe1—S1	110.22 (6)
N2—Fe1—S1	106.00 (7)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O3—H3⋯O3ii	0.84	1.97	2.7950 (14)	166

Symmetry code: (ii) .