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The title compound, [Fe(C2H3N)6][SbF6]2, (I), synthesized by reaction of AgSbF6 with FeCl2 in CH3CN, is isostructural with the analogous nickel complex [see Leban et al. (1987), Acta Cryst. C43, 1888-1890]. The FeII centre in the cation occupies a crystallographic \overline 3 site and is octahedrally coordinated by six aceto­nitrile ligands, with an Fe-N distance of 2.153 (2) Å and an N-Fe-N angle of 88.05 (10)°. The SbF6- anion lies on a crystallographic threefold rotation axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801017585/ya6066sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801017585/ya6066Isup2.hkl
Contains datablock I

CCDC reference: 175987

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.024
  • wR factor = 0.069
  • Data-to-parameter ratio = 18.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_731 Alert C Bond Calc 1.839(5), Rep 1.839(2) .... 2.50 s.u-Ratio SB1 -F1 1.555 3.665 General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.490 Tmax scaled 0.441 Tmin scaled 0.295
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

NO COMMENT

Experimental top

Caution: exothermic reaction! AgSbF6 (25.00 g, 72 mmol) was slowly added to FeCl2 (9.23 g, 72 mmol) in CH3CN and allowed to stir overnight. The precipitate was removed by filtration and washed several times with CH3CN. Removal of the solvent from the filtrate yielded a white powder. Dissolving this solid in a minimal amount of CH3CN and layering with Et2O led to a clear colourless microcrystalline solid which becomes a white powder upon drying under vacuum. Yield: 11.95 g (21.2%). Analysis calculated for C12H18F12FeN6Sb2 (%): C 18.63, H 2.35, N 10.86, F 29.47%; found (%): C 18.42, H 2.21, N 10.57, F 29.20. Crystallographic quality single crystals were obtained by vapour diffusion of Et2O into a CH3CN solution of this compound (Fig. 1).

Refinement top

The positions of the Fe and Sb atoms were found using Patterson methods (Sheldrick, 1990). H atoms were placed geometrically on the MeCN ligands optimizing the fit with diffraction data and then refined as a rigid rotor.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1998); software used to prepare material for publication: SHELXTL/PC and PLATON (Spek, 2001).

Figures top
[Figure 1] Fig. 1. A view of the title compound showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level.
hexakis(acetonitrile) iron(II) hexafluoroantimonate top
Crystal data top
[Fe(C2H3N)6][SbF6]2Dx = 1.994 Mg m3
Mr = 773.67Mo Kα radiation, λ = 0.71073 Å
Hexagonal, R3Cell parameters from 4001 reflections
a = 11.3398 (6) Åθ = 2.4–27.5°
c = 17.3584 (11) ŵ = 2.73 mm1
V = 1933.1 (2) Å3T = 173 K
Z = 3Block cut from hexagonal prism, colourless
F(000) = 11040.40 × 0.30 × 0.30 mm
Data collection top
Bruker CCD area-detector
diffractometer
996 independent reflections
Radiation source: fine-focus sealed tube933 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
ϕ and ω scansθmax = 27.5°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Blessing, 1995; Sheldrick, 2000)
h = 1414
Tmin = 0.602, Tmax = 0.900k = 1414
5690 measured reflectionsl = 2222
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.024H-atom parameters constrained
wR(F2) = 0.069 w = 1/[σ2(Fo2) + (0.0368P)2 + 4.867P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max = 0.001
996 reflectionsΔρmax = 0.55 e Å3
53 parametersΔρmin = 0.47 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: heavy-atom methodExtinction coefficient: 0.0107 (5)
Crystal data top
[Fe(C2H3N)6][SbF6]2Z = 3
Mr = 773.67Mo Kα radiation
Hexagonal, R3µ = 2.73 mm1
a = 11.3398 (6) ÅT = 173 K
c = 17.3584 (11) Å0.40 × 0.30 × 0.30 mm
V = 1933.1 (2) Å3
Data collection top
Bruker CCD area-detector
diffractometer
996 independent reflections
Absorption correction: multi-scan
(SADABS; Blessing, 1995; Sheldrick, 2000)
933 reflections with I > 2σ(I)
Tmin = 0.602, Tmax = 0.900Rint = 0.028
5690 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0240 restraints
wR(F2) = 0.069H-atom parameters constrained
S = 1.12Δρmax = 0.55 e Å3
996 reflectionsΔρmin = 0.47 e Å3
53 parameters
Special details top

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 (Å2) top
xyzUiso*/Ueq
Fe10.66670.33330.33330.02141 (19)
N10.6659 (2)0.4906 (2)0.40253 (12)0.0321 (5)
C10.6658 (2)0.5774 (2)0.43437 (14)0.0288 (5)
C20.6651 (3)0.6881 (3)0.4763 (2)0.0424 (7)
H2A0.67230.67600.53160.064*
H2B0.58000.68780.46570.064*
H2C0.74250.77510.45970.064*
Sb10.66670.33330.661838 (14)0.02892 (17)
F10.6682 (3)0.1981 (3)0.7195 (2)0.1068 (11)
F20.5350 (3)0.1968 (3)0.60083 (19)0.0921 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0214 (2)0.0214 (2)0.0215 (4)0.01069 (12)0.0000.000
N10.0328 (10)0.0315 (10)0.0331 (10)0.0171 (8)0.0006 (8)0.0040 (8)
C10.0252 (10)0.0299 (11)0.0313 (11)0.0137 (9)0.0021 (8)0.0033 (9)
C20.0416 (16)0.0364 (13)0.054 (2)0.0230 (13)0.0058 (11)0.0167 (13)
Sb10.03148 (19)0.03148 (19)0.0238 (2)0.01574 (9)0.0000.000
F10.111 (2)0.094 (2)0.118 (2)0.0533 (18)0.0103 (19)0.0595 (19)
F20.0745 (16)0.0736 (16)0.120 (2)0.0309 (13)0.0527 (16)0.0450 (16)
Geometric parameters (Å, º) top
Fe1—N1i2.153 (2)C2—H2B0.9800
Fe1—N1ii2.153 (2)C2—H2C0.9800
Fe1—N1iii2.153 (2)Sb1—F11.839 (2)
Fe1—N12.153 (2)Sb1—F1iii1.839 (2)
Fe1—N1iv2.153 (2)Sb1—F1ii1.839 (2)
Fe1—N1v2.153 (2)Sb1—F2iii1.854 (2)
N1—C11.129 (3)Sb1—F21.854 (2)
C1—C21.455 (4)Sb1—F2ii1.854 (2)
C2—H2A0.9800
N1i—Fe1—N1ii180.0H2A—C2—H2B109.5
N1i—Fe1—N1iii88.10 (8)C1—C2—H2C109.5
N1ii—Fe1—N1iii91.91 (8)H2A—C2—H2C109.5
N1i—Fe1—N188.10 (8)H2B—C2—H2C109.5
N1ii—Fe1—N191.91 (8)F1—Sb1—F1iii93.15 (17)
N1iii—Fe1—N191.91 (8)F1—Sb1—F1ii93.15 (17)
N1i—Fe1—N1iv91.91 (8)F1iii—Sb1—F1ii93.15 (17)
N1ii—Fe1—N1iv88.09 (8)F1—Sb1—F2iii88.85 (16)
N1iii—Fe1—N1iv180.0F1iii—Sb1—F2iii87.37 (16)
N1—Fe1—N1iv88.10 (8)F1ii—Sb1—F2iii177.90 (13)
N1i—Fe1—N1v91.90 (8)F1—Sb1—F287.37 (16)
N1ii—Fe1—N1v88.09 (8)F1iii—Sb1—F2177.90 (13)
N1iii—Fe1—N1v88.10 (8)F1ii—Sb1—F288.85 (16)
N1—Fe1—N1v180.0F2iii—Sb1—F290.60 (16)
N1iv—Fe1—N1v91.90 (8)F1—Sb1—F2ii177.90 (13)
C1—N1—Fe1175.4 (2)F1iii—Sb1—F2ii88.85 (16)
N1—C1—C2179.3 (3)F1ii—Sb1—F2ii87.37 (15)
C1—C2—H2A109.5F2iii—Sb1—F2ii90.60 (16)
C1—C2—H2B109.5F2—Sb1—F2ii90.60 (16)
Symmetry codes: (i) xy+1/3, x1/3, z+2/3; (ii) x+y+1, x+1, z; (iii) y+1, xy, z; (iv) y+1/3, x+y+2/3, z+2/3; (v) x+4/3, y+2/3, z+2/3.

Experimental details

Crystal data
Chemical formula[Fe(C2H3N)6][SbF6]2
Mr773.67
Crystal system, space groupHexagonal, R3
Temperature (K)173
a, c (Å)11.3398 (6), 17.3584 (11)
V3)1933.1 (2)
Z3
Radiation typeMo Kα
µ (mm1)2.73
Crystal size (mm)0.40 × 0.30 × 0.30
Data collection
DiffractometerBruker CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Blessing, 1995; Sheldrick, 2000)
Tmin, Tmax0.602, 0.900
No. of measured, independent and
observed [I > 2σ(I)] reflections
5690, 996, 933
Rint0.028
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.069, 1.12
No. of reflections996
No. of parameters53
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.55, 0.47

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL/PC (Sheldrick, 1998), SHELXTL/PC and PLATON (Spek, 2001).

 

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