Literature DB >> 21200634

μ-Oxido-bis-({4,4'-dibromo-2,2'-ethane-1,2-diylbis(nitrilo-methyl-idyne)]diphenolato}iron(III)).

Qingguo Meng¹, Lintong Wang, Yanzhen Liu, Yan Pang.

Abstract

In the title compound, [Fe(2)(C(16)H(12)Br(2)N(2)O(2))(2)O], the complete mol-ecule is generated by twofold symmetry, with the bridging O atom, which links the iron centres, lying on the roatation rotation axis. The Fe(III) ion is chelated by the N,N,O,O-tetra-dentate Schiff base dianion, resulting in an FeN(2)O(3) square-based pyramid, with the two N atoms in the basal plane.

Entities: CellLine Chemical Disease Gene Species

Year: 2007 PMID： 21200634 PMCID： PMC2914945 DOI： 10.1107/S1600536807063143

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For related literature, see: Karacan & Somer (2004 ▶); Chen et al. (2006 ▶).

Experimental

Crystal data

[Fe2(C16H12Br2N2O2)2O] M = 975.89 Orthorhombic, a = 21.094 (2) Å b = 13.8168 (18) Å c = 11.9619 (12) Å V = 3486.3 (7) Å3 Z = 4 Mo Kα radiation μ = 5.46 mm−1 T = 293 (2) K 0.43 × 0.28 × 0.22 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.202, T max = 0.380 (expected range = 0.160–0.301) 11548 measured reflections 3182 independent reflections 2257 reflections with I > 2σ(I) R int = 0.049

Refinement

R[F 2 > 2σ(F 2)] = 0.059 wR(F 2) = 0.147 S = 1.00 3182 reflections 213 parameters H-atom parameters constraned Δρmax = 1.05 e Å−3 Δρmin = −0.70 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, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL (Bruker, 2001 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807063143/hb2647sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807063143/hb2647Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Fe₂(C₁₆H₁₂Br₂N₂O₂)₂O]	F₀₀₀ = 1904
M_r = 975.89	D_x = 1.859 Mg m⁻³
Orthorhombic, Pcca	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2a 2ac	Cell parameters from 3182 reflections
a = 21.094 (2) Å	θ = 3.0–25.4º
b = 13.8168 (18) Å	µ = 5.46 mm⁻¹
c = 11.9619 (12) Å	T = 293 (2) K
V = 3486.3 (7) Å³	Block, brown
Z = 4	0.43 × 0.28 × 0.22 mm

Bruker APEX II CCD diffractometer	3182 independent reflections
Radiation source: fine-focus sealed tube	2257 reflections with I > 2σ(I)
Monochromator: graphite	R_int = 0.049
T = 293(2) K	θ_max = 25.4º
φ and ω scans	θ_min = 3.0º
Absorption correction: multi-scan(SADABS; Bruker, 2001)	h = −25→25
T_min = 0.202, T_max = 0.380	k = −16→16
11548 measured reflections	l = 0→14

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)] = 0.059	H-atom parameters constrained
wR(F²) = 0.147	w = 1/[σ²(F_o²) + (0.077P)²] where P = (F_o² + 2F_c²)/3
S = 1.00	(Δ/σ)_max = 0.018
3182 reflections	Δρ_max = 1.05 e Å⁻³
213 parameters	Δρ_min = −0.70 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	U_iso*/U_eq
Fe1	0.07194 (4)	0.12987 (5)	0.31467 (6)	0.0342 (2)
Br1	0.10796 (4)	0.66034 (5)	0.24478 (7)	0.0776 (3)
Br2	0.28253 (3)	−0.28115 (5)	0.48690 (6)	0.0663 (3)
C1	0.0405 (3)	0.3280 (4)	0.4134 (4)	0.0404 (13)
H1	0.0230	0.3670	0.4687	0.048*
C2	0.0734 (3)	0.3750 (4)	0.3197 (5)	0.0392 (12)
C3	0.1029 (3)	0.3259 (4)	0.2294 (5)	0.0405 (13)
C4	0.1303 (3)	0.3799 (4)	0.1413 (5)	0.0514 (15)
H4	0.1477	0.3477	0.0803	0.062*
C5	0.1316 (3)	0.4776 (4)	0.1447 (6)	0.0574 (17)
H5	0.1504	0.5126	0.0872	0.069*
C6	0.1039 (3)	0.5260 (4)	0.2367 (5)	0.0519 (16)
C7	0.0744 (3)	0.4748 (4)	0.3235 (5)	0.0476 (14)
H7	0.0557	0.5077	0.3829	0.057*
C8	0.0009 (3)	0.1958 (4)	0.5204 (5)	0.0432 (14)
H8A	−0.0382	0.1650	0.4970	0.052*
H8B	−0.0091	0.2462	0.5741	0.052*
C9	0.0461 (3)	0.1213 (4)	0.5721 (4)	0.0423 (13)
H9A	0.0765	0.1534	0.6202	0.051*
H9B	0.0224	0.0751	0.6166	0.051*
C10	0.1146 (3)	−0.0002 (4)	0.5091 (4)	0.0385 (13)
H10	0.1140	−0.0181	0.5840	0.046*
C11	0.1561 (3)	−0.0556 (4)	0.4331 (4)	0.0370 (12)
C12	0.1643 (3)	−0.0340 (3)	0.3168 (4)	0.0356 (11)
C13	0.2041 (3)	−0.0949 (4)	0.2516 (5)	0.0410 (13)
H13	0.2075	−0.0849	0.1749	0.049*
C14	0.2370 (3)	−0.1675 (4)	0.3005 (5)	0.0474 (14)
H14	0.2640	−0.2058	0.2576	0.057*
C15	0.2308 (3)	−0.1858 (4)	0.4169 (5)	0.0463 (14)
C16	0.1901 (3)	−0.1313 (4)	0.4831 (5)	0.0428 (14)
H16	0.1856	−0.1448	0.5589	0.051*
N1	0.0797 (2)	0.0703 (3)	0.4793 (4)	0.0363 (10)
N2	0.0348 (2)	0.2370 (3)	0.4227 (4)	0.0360 (10)
O1	0.10571 (18)	0.2321 (3)	0.2223 (3)	0.0435 (9)
O2	0.13721 (19)	0.0409 (3)	0.2686 (3)	0.0414 (9)
O3	0.0000	0.0842 (4)	0.2500	0.0388 (12)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0433 (5)	0.0267 (4)	0.0327 (4)	0.0006 (3)	0.0003 (3)	−0.0002 (3)
Br1	0.1084 (7)	0.0293 (4)	0.0950 (6)	−0.0024 (3)	0.0277 (5)	0.0093 (4)
Br2	0.0660 (5)	0.0586 (5)	0.0744 (5)	0.0225 (3)	0.0087 (4)	0.0251 (4)
C1	0.044 (3)	0.036 (3)	0.041 (3)	0.001 (2)	0.001 (3)	−0.007 (2)
C2	0.042 (3)	0.031 (3)	0.045 (3)	0.000 (2)	−0.001 (3)	0.002 (2)
C3	0.042 (3)	0.037 (3)	0.043 (3)	−0.003 (2)	0.003 (3)	0.001 (3)
C4	0.062 (4)	0.042 (3)	0.050 (3)	0.001 (3)	0.007 (3)	0.011 (3)
C5	0.067 (4)	0.040 (3)	0.066 (4)	−0.007 (3)	0.013 (3)	0.009 (3)
C6	0.064 (4)	0.029 (3)	0.064 (4)	−0.004 (3)	0.005 (3)	0.012 (3)
C7	0.051 (4)	0.032 (3)	0.060 (4)	0.001 (3)	0.004 (3)	0.002 (3)
C8	0.050 (4)	0.038 (3)	0.042 (3)	0.001 (3)	0.011 (3)	0.004 (3)
C9	0.052 (3)	0.041 (3)	0.034 (3)	−0.001 (3)	0.010 (3)	0.001 (2)
C10	0.051 (4)	0.030 (3)	0.035 (3)	−0.006 (2)	−0.001 (3)	0.001 (2)
C11	0.041 (3)	0.030 (3)	0.041 (3)	−0.001 (2)	−0.003 (2)	0.003 (2)
C12	0.043 (3)	0.027 (2)	0.037 (3)	−0.001 (2)	0.001 (2)	−0.001 (2)
C13	0.049 (3)	0.034 (3)	0.041 (3)	0.003 (2)	0.001 (3)	0.001 (2)
C14	0.048 (3)	0.038 (3)	0.057 (4)	0.005 (3)	0.008 (3)	0.002 (3)
C15	0.044 (3)	0.043 (3)	0.052 (3)	0.003 (3)	0.005 (3)	0.016 (3)
C16	0.047 (3)	0.038 (3)	0.043 (3)	−0.001 (3)	0.002 (3)	0.010 (3)
N1	0.045 (3)	0.029 (2)	0.035 (2)	0.0013 (19)	0.002 (2)	−0.0019 (19)
N2	0.042 (3)	0.025 (2)	0.041 (2)	−0.0042 (18)	0.005 (2)	0.0019 (19)
O1	0.055 (3)	0.030 (2)	0.045 (2)	−0.0026 (17)	0.0101 (19)	0.0019 (17)
O2	0.056 (2)	0.034 (2)	0.0346 (18)	0.0113 (17)	−0.0020 (18)	0.0024 (16)
O3	0.045 (3)	0.028 (3)	0.043 (3)	0.000	−0.009 (2)	0.000

Fe1—O3	1.8162 (18)	C8—C9	1.533 (8)
Fe1—O2	1.926 (4)	C8—H8A	0.9700
Fe1—O1	1.930 (4)	C8—H8B	0.9700
Fe1—N2	2.116 (4)	C9—N1	1.493 (7)
Fe1—N1	2.141 (4)	C9—H9A	0.9700
Br1—C6	1.861 (6)	C9—H9B	0.9700
Br2—C15	1.905 (6)	C10—N1	1.272 (7)
C1—N2	1.268 (6)	C10—C11	1.474 (7)
C1—C2	1.470 (7)	C10—H10	0.9300
C1—H1	0.9300	C11—C16	1.404 (7)
C2—C7	1.380 (7)	C11—C12	1.434 (7)
C2—C3	1.419 (8)	C12—O2	1.314 (6)
C3—O1	1.299 (6)	C12—C13	1.422 (7)
C3—C4	1.414 (8)	C13—C14	1.354 (8)
C4—C5	1.351 (8)	C13—H13	0.9300
C4—H4	0.9300	C14—C15	1.421 (8)
C5—C6	1.414 (9)	C14—H14	0.9300
C5—H5	0.9300	C15—C16	1.388 (8)
C6—C7	1.402 (8)	C16—H16	0.9300
C7—H7	0.9300	O3—Fe1ⁱ	1.8162 (18)
C8—N2	1.483 (7)

O3—Fe1—O2	104.71 (16)	N1—C9—C8	108.2 (4)
O3—Fe1—O1	108.58 (16)	N1—C9—H9A	110.1
O2—Fe1—O1	92.29 (16)	C8—C9—H9A	110.1
O3—Fe1—N2	101.14 (16)	N1—C9—H9B	110.1
O2—Fe1—N2	152.39 (17)	C8—C9—H9B	110.1
O1—Fe1—N2	88.51 (16)	H9A—C9—H9B	108.4
O3—Fe1—N1	108.78 (15)	N1—C10—C11	124.6 (5)
O2—Fe1—N1	87.89 (16)	N1—C10—H10	117.7
O1—Fe1—N1	141.27 (17)	C11—C10—H10	117.7
N2—Fe1—N1	74.66 (16)	C16—C11—C12	120.4 (5)
N2—C1—C2	123.4 (5)	C16—C11—C10	115.4 (5)
N2—C1—H1	118.3	C12—C11—C10	124.2 (5)
C2—C1—H1	118.3	O2—C12—C13	118.8 (4)
C7—C2—C3	119.8 (5)	O2—C12—C11	122.4 (5)
C7—C2—C1	115.0 (5)	C13—C12—C11	118.7 (5)
C3—C2—C1	125.1 (5)	C14—C13—C12	120.3 (5)
O1—C3—C2	123.1 (5)	C14—C13—H13	119.8
O1—C3—C4	117.3 (5)	C12—C13—H13	119.8
C2—C3—C4	119.6 (5)	C13—C14—C15	120.5 (5)
C5—C4—C3	120.9 (6)	C13—C14—H14	119.8
C5—C4—H4	119.6	C15—C14—H14	119.8
C3—C4—H4	119.6	C16—C15—C14	121.3 (5)
C4—C5—C6	119.2 (6)	C16—C15—Br2	118.6 (4)
C4—C5—H5	120.4	C14—C15—Br2	120.0 (4)
C6—C5—H5	120.4	C15—C16—C11	118.5 (5)
C7—C6—C5	121.4 (5)	C15—C16—H16	120.7
C7—C6—Br1	119.0 (5)	C11—C16—H16	120.7
C5—C6—Br1	119.5 (4)	C10—N1—C9	115.4 (4)
C2—C7—C6	119.1 (6)	C10—N1—Fe1	126.6 (4)
C2—C7—H7	120.5	C9—N1—Fe1	117.8 (3)
C6—C7—H7	120.5	C1—N2—C8	119.7 (5)
N2—C8—C9	106.0 (4)	C1—N2—Fe1	127.2 (4)
N2—C8—H8A	110.5	C8—N2—Fe1	113.0 (3)
C9—C8—H8A	110.5	C3—O1—Fe1	132.5 (3)
N2—C8—H8B	110.5	C12—O2—Fe1	133.4 (3)
C9—C8—H8B	110.5	Fe1ⁱ—O3—Fe1	139.4 (3)
H8A—C8—H8B	108.7

Fe1—O3	1.8162 (18)
Fe1—O2	1.926 (4)
Fe1—O1	1.930 (4)
Fe1—N2	2.116 (4)
Fe1—N1	2.141 (4)

Fe1ⁱ—O3—Fe1

139.4 (3)

Symmetry code: (i) .

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1. Retraction of articles.

Authors:
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2012-06-13

1 in total