[Fe(thf)₆][Cl₃Fe–O–FeCl₃]

The title compound, hexa­kis­(tetra­hydro­furan)­iron(II) μ-oxo-bis­[tri­chloro­ferrate(III)], [Fe(C₄H₈O)₆][Fe₂Cl₆O], was obtained by oxidation of FeCl₂ in tetra­hydro­furan. The O atom of the anion and the Fe atom of the cation are located on special positions of site symmetry ; the Fe atoms of the anion are located on a threefold rotation axis and, as a result, there is just of both ions in the asymmetric unit.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.009 Å
• R factor = 0.056
• wR factor = 0.133
• Data-to-parameter ratio = 22.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level C:



PLAT_360  Alert C Short  C(sp3)-C(sp3) Bond  C(3)   -   C(4)   =       1.42 Ang.

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #      4
                   O2  -FE2 -O2  -C2   -160.00  5.00  13.667   1.555   1.555   1.555

General Notes



FORMU_01  There is a discrepancy between the atom counts in the
          _chemical_formula_sum and _chemical_formula_moiety. This is
          usually due to the moiety formula being in the wrong format.
          Atom count from _chemical_formula_sum:   C24 H48 Cl6 Fe3 O7
          Atom count from _chemical_formula_moiety:C24 H48 Cl6 Fe2 O7


 0 Alert Level A = Potentially serious problem

 0 Alert Level B = Potential problem

 2 Alert Level C = Please check

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Computing details

Data collection: SMART (Siemens, 1995); cell refinement: SMART; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991).

(I)

Crystal data

[Fe(C4H8O)6][Fe2Cl6O]	Mo Kα radiation, λ = 0.71073 Å
Mr = 828.87	Cell parameters from 502 reflections
Cubic, Pa3	θ = 2.7–20.1°
a = 15.244 (2) Å	µ = 1.70 mm^−1
V = 3542.4 (8) Å^3	T = 173 K
Z = 4	Plate, red
F(000) = 1712	0.28 × 0.28 × 0.12 mm
Dx = 1.554 Mg m^−3

Data collection

Siemens CCD three-circle diffractometer	1405 independent reflections
Radiation source: fine-focus sealed tube	792 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.068
ω scans	θmax = 28.2°, θmin = 2.3°
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996)	h = −19→19
Tmin = 0.647, Tmax = 0.822	k = −20→17
36645 measured reflections	l = −19→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.056	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.133	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0415P)^2 + 11.6567P] where P = (Fo^2 + 2Fc^2)/3
1405 reflections	(Δ/σ)max < 0.001
62 parameters	Δρmax = 0.46 e Å^−3
0 restraints	Δρmin = −0.46 e Å^−3

Special details

Experimental. ;

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.56632 (4)	0.56632 (4)	0.56632 (4)	0.0277 (3)
Cl1	0.48436 (9)	0.64660 (9)	0.65679 (9)	0.0408 (4)
O1	0.5000	0.5000	0.5000	0.044 (2)
Fe2	0.5000	0.5000	1.0000	0.0219 (4)
O2	0.45429 (18)	0.4252 (2)	0.88772 (18)	0.0243 (7)
C2	0.5008 (3)	0.4178 (4)	0.8049 (3)	0.0365 (12)
H2A	0.5472	0.3725	0.8085	0.044*
H2B	0.5281	0.4745	0.7887	0.044*
C3	0.4336 (5)	0.3929 (6)	0.7411 (4)	0.079 (2)
H3A	0.4139	0.4453	0.7081	0.094*
H3B	0.4582	0.3502	0.6987	0.094*
C4	0.3614 (4)	0.3547 (5)	0.7862 (4)	0.066 (2)
H4A	0.3617	0.2902	0.7788	0.079*
H4B	0.3054	0.3780	0.7630	0.079*
C5	0.3717 (3)	0.3783 (4)	0.8807 (3)	0.0361 (12)
H5A	0.3224	0.4158	0.9002	0.043*
H5B	0.3728	0.3247	0.9174	0.043*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.0277 (3)	0.0277 (3)	0.0277 (3)	−0.0022 (3)	−0.0022 (3)	−0.0022 (3)
Cl1	0.0441 (8)	0.0421 (8)	0.0364 (7)	0.0078 (6)	0.0072 (6)	−0.0008 (6)
O1	0.044 (2)	0.044 (2)	0.044 (2)	0.001 (3)	0.001 (3)	0.001 (3)
Fe2	0.0219 (4)	0.0219 (4)	0.0219 (4)	−0.0002 (4)	−0.0002 (4)	0.0002 (4)
O2	0.0242 (17)	0.0309 (18)	0.0177 (16)	−0.0026 (14)	0.0004 (13)	−0.0024 (14)
C2	0.039 (3)	0.048 (3)	0.022 (2)	−0.003 (3)	0.004 (2)	−0.005 (2)
C3	0.078 (5)	0.123 (7)	0.035 (3)	−0.037 (5)	−0.004 (4)	−0.012 (4)
C4	0.050 (4)	0.101 (6)	0.047 (4)	−0.019 (4)	−0.010 (3)	−0.024 (4)
C5	0.029 (3)	0.042 (3)	0.038 (3)	−0.008 (2)	−0.005 (2)	−0.001 (2)

Geometric parameters (Å, º)

Fe1—O1	1.7510 (12)	O2—C2	1.453 (5)
Fe1—Cl1^i	2.2273 (14)	C2—C3	1.463 (8)
Fe1—Cl1	2.2273 (14)	C2—H2A	0.9900
Fe1—Cl1^ii	2.2273 (14)	C2—H2B	0.9900
O1—Fe1^iii	1.7510 (12)	C3—C4	1.422 (9)
Fe2—O2^iv	2.171 (3)	C3—H3A	0.9900
Fe2—O2	2.171 (3)	C3—H3B	0.9900
Fe2—O2^v	2.171 (3)	C4—C5	1.492 (7)
Fe2—O2^vi	2.171 (3)	C4—H4A	0.9900
Fe2—O2^vii	2.171 (3)	C4—H4B	0.9900
Fe2—O2^viii	2.171 (3)	C5—H5A	0.9900
O2—C5	1.452 (5)	C5—H5B	0.9900
O1—Fe1—Cl1^i	110.55 (5)	O2—C2—C3	104.9 (4)
O1—Fe1—Cl1	110.54 (5)	O2—C2—H2A	110.8
Cl1^i—Fe1—Cl1	108.38 (5)	C3—C2—H2A	110.8
O1—Fe1—Cl1^ii	110.54 (5)	O2—C2—H2B	110.8
Cl1^i—Fe1—Cl1^ii	108.38 (5)	C3—C2—H2B	110.8
Cl1—Fe1—Cl1^ii	108.38 (5)	H2A—C2—H2B	108.9
Fe1^iii—O1—Fe1	180.0	C4—C3—C2	109.0 (5)
O2^iv—Fe2—O2	180.00 (14)	C4—C3—H3A	109.9
O2^iv—Fe2—O2^v	90.44 (11)	C2—C3—H3A	109.9
O2—Fe2—O2^v	89.56 (11)	C4—C3—H3B	109.9
O2^iv—Fe2—O2^vi	89.57 (11)	C2—C3—H3B	109.9
O2—Fe2—O2^vi	90.44 (11)	H3A—C3—H3B	108.3
O2^v—Fe2—O2^vi	89.57 (11)	C3—C4—C5	106.7 (5)
O2^iv—Fe2—O2^vii	90.43 (11)	C3—C4—H4A	110.4
O2—Fe2—O2^vii	89.57 (11)	C5—C4—H4A	110.4
O2^v—Fe2—O2^vii	90.43 (11)	C3—C4—H4B	110.4
O2^vi—Fe2—O2^vii	180.0	C5—C4—H4B	110.4
O2^iv—Fe2—O2^viii	89.56 (11)	H4A—C4—H4B	108.6
O2—Fe2—O2^viii	90.44 (11)	O2—C5—C4	106.3 (4)
O2^v—Fe2—O2^viii	179.998 (1)	O2—C5—H5A	110.5
O2^vi—Fe2—O2^viii	90.43 (11)	C4—C5—H5A	110.5
O2^vii—Fe2—O2^viii	89.57 (11)	O2—C5—H5B	110.5
C5—O2—C2	108.7 (3)	C4—C5—H5B	110.5
C5—O2—Fe2	126.5 (3)	H5A—C5—H5B	108.7
C2—O2—Fe2	124.7 (3)
O2^vi—Fe2—O2—C5	−173.4 (4)	C5—O2—C2—C3	18.8 (6)
O2^vii—Fe2—O2—C5	6.6 (4)	Fe2—O2—C2—C3	−158.5 (4)
O2^viii—Fe2—O2—C5	96.1 (4)	O2—C2—C3—C4	−21.5 (8)
O2^iv—Fe2—O2—C2	−160 (5)	C2—C3—C4—C5	15.7 (9)
O2^v—Fe2—O2—C2	93.0 (3)	C2—O2—C5—C4	−9.6 (6)
O2^vi—Fe2—O2—C2	3.4 (3)	Fe2—O2—C5—C4	167.7 (4)
O2^vii—Fe2—O2—C2	−176.6 (3)	C3—C4—C5—O2	−3.8 (8)
O2^viii—Fe2—O2—C2	−87.0 (3)

Symmetry codes: (i) y, z, x; (ii) z, x, y; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y+1, −z+2; (v) y, −z+3/2, x+1/2; (vi) −z+3/2, −x+1, y+1/2; (vii) z−1/2, x, −y+3/2; (viii) −y+1, z−1/2, −x+3/2.