Bis{μ-2,2'-[ethane-1,2-diylbis(nitrilo-methyl-idyne)]diphenolato}bis-[(thio-cyanato-κN)iron(III)].

The title compound, [Fe(2)(C(16)H(14)N(2)O(2))(2)(NCS)(2)], is isostructural with the Mn(III)-containing analogue. Each Fe(III) atom is chelated by a tetra-dentate 2,2'-[ethane-1,2-diylbis(nitrilo-methyl-idyne)]diphenolate ligand and by the N atom of a thio-cyanate anion, in a square-pyramidal arrangement. The complex mol-ecules form centrosymmetric dimers, with an Fe-O contact of 2.549 (3) Å, trans to each thio-cyanate anion, completing a distorted octa-hedral coordination geometry.

Related literature

For related literature, see: Garnovskii et al. (1993 ▶); Huang et al. (2002 ▶); Bhadbhade & Srinivas (1993 ▶); Bunce et al. (1998 ▶). For the isostructural MnIII-containing compound, see: Wang et al. (2008 ▶).

Experimental

Crystal data

[Fe2(C16H14N2O2)2(NCS)2]

M = 380.23

Monoclinic,

a = 8.9231 (10) Å

b = 14.0779 (10) Å

c = 14.9716 (10) Å

β = 106.844 (1)°

V = 1800.0 (3) Å3

Z = 4

Mo Kα radiation

μ = 0.97 mm−1

T = 293 (2) K

0.12 × 0.11 × 0.09 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.893, T max = 0.918

12796 measured reflections

3191 independent reflections

2535 reflections with I > 2σ(I)

R int = 0.023

Refinement

R[F 2 > 2σ(F 2)] = 0.058

wR(F 2) = 0.180

S = 1.00

3191 reflections

217 parameters

H-atom parameters constrained

Δρmax = 1.12 e Å−3

Δρmin = −0.33 e Å−3

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808021892/bi2293sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808021892/bi2293Isup2.hkl

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

[Fe2(C16H14N2O2)2(NCS)2]	F000 = 780
Mr = 380.23	Dx = 1.403 Mg m−3
Monoclinic, P21/n	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 4497 reflections
a = 8.9231 (10) Å	θ = 2.4–24.4º
b = 14.0779 (10) Å	µ = 0.97 mm−1
c = 14.9716 (10) Å	T = 293 (2) K
β = 106.844 (1)º	Block, brown
V = 1800.0 (3) Å3	0.12 × 0.11 × 0.09 mm
Z = 4

Bruker APEXII CCD diffractometer	3191 independent reflections
Radiation source: fine-focus sealed tube	2535 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.023
T = 293(2) K	θmax = 25.3º
φ and ω scans	θmin = 2.4º
Absorption correction: multi-scan(SADABS; Bruker, 2001)	h = −10→10
Tmin = 0.893, Tmax = 0.918	k = −16→16
12796 measured reflections	l = −18→17

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.058	H-atom parameters constrained
wR(F2) = 0.180	w = 1/[σ2(Fo2) + (0.114P)2 + 1.289P] where P = (Fo2 + 2Fc2)/3
S = 1.00	(Δ/σ)max < 0.001
3191 reflections	Δρmax = 1.12 e Å−3
217 parameters	Δρmin = −0.33 e Å−3
Primary atom site location: structure-invariant direct methods	Extinction correction: none

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
Fe1	0.64494 (7)	0.01030 (4)	0.10343 (4)	0.0586 (3)
C1	0.9422 (5)	−0.0874 (3)	0.2499 (3)	0.0612 (10)
C2	0.5250 (4)	−0.1763 (3)	0.0554 (3)	0.0563 (9)
C3	0.5503 (5)	−0.2621 (3)	0.0151 (4)	0.0690 (11)
H3	0.6005	−0.2622	−0.0314	0.083*
C4	0.5012 (7)	−0.3464 (4)	0.0441 (5)	0.0905 (15)
H4	0.5190	−0.4032	0.0171	0.109*
C5	0.4258 (7)	−0.3475 (4)	0.1126 (5)	0.103 (2)
H5	0.3939	−0.4049	0.1318	0.124*
C6	0.3974 (7)	−0.2631 (4)	0.1529 (4)	0.0895 (16)
H6	0.3438	−0.2638	0.1977	0.107*
C7	0.4493 (5)	−0.1778 (3)	0.1262 (3)	0.0665 (11)
C8	0.4150 (6)	−0.0914 (4)	0.1685 (3)	0.0757 (13)
H8	0.3416	−0.0948	0.2016	0.091*
C9	0.4311 (10)	0.0777 (5)	0.2043 (5)	0.117 (2)
H9A	0.3827	0.0625	0.2528	0.141*
H9B	0.3577	0.1145	0.1563	0.141*
C10	0.5833 (10)	0.1335 (4)	0.2450 (4)	0.109 (2)
H10A	0.5603	0.1986	0.2577	0.130*
H10B	0.6451	0.1046	0.3027	0.130*
C11	0.7504 (8)	0.2036 (4)	0.1629 (4)	0.0936 (18)
H11	0.7469	0.2578	0.1977	0.112*
C12	0.8444 (6)	0.2076 (3)	0.1012 (4)	0.0801 (13)
C13	0.8633 (5)	0.1309 (3)	0.0459 (3)	0.0684 (11)
C14	0.9632 (6)	0.1410 (4)	−0.0104 (4)	0.0900 (16)
H14	0.9784	0.0901	−0.0464	0.108*
C15	1.0394 (7)	0.2261 (6)	−0.0128 (7)	0.125 (3)
H15	1.1052	0.2319	−0.0507	0.150*
C16	1.0191 (9)	0.3026 (6)	0.0405 (7)	0.136 (3)
H16	1.0706	0.3596	0.0382	0.163*
C17	0.9219 (9)	0.2942 (5)	0.0971 (5)	0.123 (3)
H17	0.9076	0.3457	0.1326	0.148*
N1	0.8171 (5)	−0.0695 (3)	0.2098 (3)	0.0785 (10)
N2	0.6685 (6)	0.1309 (3)	0.1752 (3)	0.0796 (11)
N3	0.4771 (5)	−0.0113 (3)	0.1639 (3)	0.0721 (10)
O1	0.5684 (3)	−0.09420 (17)	0.02262 (18)	0.0553 (6)
O2	0.7880 (3)	0.0489 (2)	0.0418 (2)	0.0660 (7)
S1	1.11963 (15)	−0.11760 (11)	0.30804 (10)	0.0858 (4)

	U11	U22	U33	U12	U13	U23
Fe1	0.0672 (4)	0.0522 (4)	0.0613 (4)	0.0061 (2)	0.0262 (3)	−0.0013 (2)
C1	0.075 (3)	0.048 (2)	0.065 (2)	0.0050 (19)	0.028 (2)	0.0093 (17)
C2	0.053 (2)	0.050 (2)	0.066 (2)	0.0008 (16)	0.0163 (17)	0.0063 (17)
C3	0.064 (2)	0.051 (2)	0.090 (3)	0.0037 (18)	0.020 (2)	0.005 (2)
C4	0.087 (3)	0.055 (3)	0.120 (4)	0.000 (2)	0.016 (3)	0.011 (3)
C5	0.104 (4)	0.074 (4)	0.120 (5)	−0.018 (3)	0.014 (4)	0.040 (3)
C6	0.084 (3)	0.096 (4)	0.087 (3)	−0.019 (3)	0.023 (3)	0.034 (3)
C7	0.056 (2)	0.079 (3)	0.064 (2)	−0.002 (2)	0.0153 (19)	0.021 (2)
C8	0.075 (3)	0.095 (4)	0.068 (3)	0.011 (3)	0.038 (2)	0.021 (2)
C9	0.149 (6)	0.116 (5)	0.122 (5)	0.046 (5)	0.093 (5)	−0.003 (4)
C10	0.177 (7)	0.081 (4)	0.078 (3)	0.032 (4)	0.052 (4)	−0.008 (3)
C11	0.127 (5)	0.056 (3)	0.070 (3)	0.007 (3)	−0.015 (3)	−0.014 (2)
C12	0.084 (3)	0.067 (3)	0.071 (3)	−0.011 (2)	−0.006 (2)	−0.001 (2)
C13	0.051 (2)	0.065 (3)	0.079 (3)	−0.0061 (18)	0.002 (2)	0.012 (2)
C14	0.059 (3)	0.089 (4)	0.120 (4)	−0.006 (2)	0.023 (3)	0.024 (3)
C15	0.075 (4)	0.118 (6)	0.164 (7)	−0.038 (4)	0.006 (4)	0.045 (5)
C16	0.104 (5)	0.109 (6)	0.156 (7)	−0.057 (5)	−0.024 (5)	0.032 (5)
C17	0.129 (6)	0.082 (4)	0.117 (5)	−0.037 (4)	−0.032 (4)	−0.001 (3)
N1	0.077 (3)	0.075 (2)	0.082 (3)	0.017 (2)	0.020 (2)	0.012 (2)
N2	0.113 (3)	0.063 (2)	0.057 (2)	0.019 (2)	0.015 (2)	−0.0085 (16)
N3	0.080 (2)	0.079 (3)	0.069 (2)	0.0157 (19)	0.040 (2)	0.0052 (17)
O1	0.0636 (15)	0.0482 (13)	0.0608 (14)	0.0017 (11)	0.0284 (12)	0.0024 (11)
O2	0.0625 (16)	0.0566 (16)	0.084 (2)	−0.0024 (13)	0.0289 (14)	−0.0006 (14)
S1	0.0658 (7)	0.0956 (9)	0.0968 (9)	0.0082 (6)	0.0248 (6)	0.0267 (7)

Fe1—O2	1.860 (3)	C9—N3	1.500 (7)
Fe1—O1	1.902 (3)	C9—C10	1.534 (11)
Fe1—N3	1.985 (4)	C9—H9A	0.970
Fe1—N2	1.988 (4)	C9—H9B	0.970
Fe1—N1	2.178 (4)	C10—N2	1.459 (7)
C1—N1	1.132 (5)	C10—H10A	0.970
C1—S1	1.627 (5)	C10—H10B	0.970
C2—O1	1.355 (4)	C11—N2	1.302 (7)
C2—C7	1.412 (6)	C11—C12	1.418 (8)
C2—C3	1.397 (6)	C11—H11	0.930
C3—C4	1.378 (7)	C12—C13	1.401 (7)
C3—H3	0.930	C12—C17	1.412 (8)
C4—C5	1.380 (9)	C13—O2	1.328 (5)
C4—H4	0.930	C13—C14	1.400 (7)
C5—C6	1.388 (9)	C14—C15	1.383 (9)
C5—H5	0.930	C14—H14	0.930
C6—C7	1.387 (7)	C15—C16	1.384 (13)
C6—H6	0.930	C15—H15	0.930
C7—C8	1.445 (7)	C16—C17	1.382 (12)
C8—N3	1.267 (6)	C16—H16	0.930
C8—H8	0.930	C17—H17	0.930
O2—Fe1—O1	94.72 (12)	H9A—C9—H9B	108.7
O2—Fe1—N3	171.11 (14)	N2—C10—C9	106.7 (5)
O1—Fe1—N3	89.55 (14)	N2—C10—H10A	110.4
O2—Fe1—N2	92.21 (17)	C9—C10—H10A	110.4
O1—Fe1—N2	165.26 (15)	N2—C10—H10B	110.4
N3—Fe1—N2	81.92 (19)	C9—C10—H10B	110.4
O2—Fe1—N1	94.22 (14)	H10A—C10—H10B	108.6
O1—Fe1—N1	96.51 (14)	N2—C11—C12	125.9 (5)
N3—Fe1—N1	93.03 (16)	N2—C11—H11	117.0
N2—Fe1—N1	95.94 (16)	C12—C11—H11	117.0
N1—C1—S1	177.6 (4)	C13—C12—C17	119.7 (6)
O1—C2—C7	122.3 (4)	C13—C12—C11	123.4 (4)
O1—C2—C3	118.8 (4)	C17—C12—C11	116.9 (6)
C7—C2—C3	118.9 (4)	O2—C13—C14	117.6 (5)
C2—C3—C4	120.2 (5)	O2—C13—C12	123.4 (4)
C2—C3—H3	119.9	C14—C13—C12	119.0 (5)
C4—C3—H3	119.9	C13—C14—C15	120.5 (7)
C5—C4—C3	120.7 (5)	C13—C14—H14	119.8
C5—C4—H4	119.6	C15—C14—H14	119.7
C3—C4—H4	119.6	C16—C15—C14	120.8 (8)
C4—C5—C6	120.2 (5)	C16—C15—H15	119.6
C4—C5—H5	119.9	C14—C15—H15	119.6
C6—C5—H5	119.9	C17—C16—C15	119.8 (6)
C7—C6—C5	119.8 (5)	C17—C16—H16	120.1
C7—C6—H6	120.1	C15—C16—H16	120.1
C5—C6—H6	120.1	C16—C17—C12	120.2 (8)
C2—C7—C6	120.1 (5)	C16—C17—H17	119.9
C2—C7—C8	121.6 (4)	C12—C17—H17	119.9
C6—C7—C8	118.2 (4)	C1—N1—Fe1	151.7 (4)
N3—C8—C7	125.0 (4)	C11—N2—C10	120.8 (5)
N3—C8—H8	117.5	C11—N2—Fe1	124.8 (4)
C7—C8—H8	117.5	C10—N2—Fe1	114.4 (4)
N3—C9—C10	105.9 (5)	C8—N3—C9	123.1 (5)
N3—C9—H9A	110.6	C8—N3—Fe1	124.1 (3)
C10—C9—H9A	110.6	C9—N3—Fe1	112.8 (4)
N3—C9—H9B	110.6	C2—O1—Fe1	121.1 (2)
C10—C9—H9B	110.6	C13—O2—Fe1	130.0 (3)