Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801017585/ya6066sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801017585/ya6066Isup2.hkl |
CCDC reference: 175987
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (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
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
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).
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.
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).
Fig. 1. A view of the title compound showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. |
[Fe(C2H3N)6][SbF6]2 | Dx = 1.994 Mg m−3 |
Mr = 773.67 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, R3 | Cell parameters from 4001 reflections |
a = 11.3398 (6) Å | θ = 2.4–27.5° |
c = 17.3584 (11) Å | µ = 2.73 mm−1 |
V = 1933.1 (2) Å3 | T = 173 K |
Z = 3 | Block cut from hexagonal prism, colourless |
F(000) = 1104 | 0.40 × 0.30 × 0.30 mm |
Bruker CCD area-detector diffractometer | 996 independent reflections |
Radiation source: fine-focus sealed tube | 933 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
ϕ and ω scans | θmax = 27.5°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Blessing, 1995; Sheldrick, 2000) | h = −14→14 |
Tmin = 0.602, Tmax = 0.900 | k = −14→14 |
5690 measured reflections | l = −22→22 |
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)] = 0.024 | H-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 reflections | Δρmax = 0.55 e Å−3 |
53 parameters | Δρmin = −0.47 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: heavy-atom method | Extinction coefficient: 0.0107 (5) |
[Fe(C2H3N)6][SbF6]2 | Z = 3 |
Mr = 773.67 | Mo Kα radiation |
Hexagonal, R3 | µ = 2.73 mm−1 |
a = 11.3398 (6) Å | T = 173 K |
c = 17.3584 (11) Å | 0.40 × 0.30 × 0.30 mm |
V = 1933.1 (2) Å3 |
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 = 0.900 | Rint = 0.028 |
5690 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.069 | H-atom parameters constrained |
S = 1.12 | Δρmax = 0.55 e Å−3 |
996 reflections | Δρmin = −0.47 e Å−3 |
53 parameters |
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 | 0.6667 | 0.3333 | 0.3333 | 0.02141 (19) | |
N1 | 0.6659 (2) | 0.4906 (2) | 0.40253 (12) | 0.0321 (5) | |
C1 | 0.6658 (2) | 0.5774 (2) | 0.43437 (14) | 0.0288 (5) | |
C2 | 0.6651 (3) | 0.6881 (3) | 0.4763 (2) | 0.0424 (7) | |
H2A | 0.6723 | 0.6760 | 0.5316 | 0.064* | |
H2B | 0.5800 | 0.6878 | 0.4657 | 0.064* | |
H2C | 0.7425 | 0.7751 | 0.4597 | 0.064* | |
Sb1 | 0.6667 | 0.3333 | 0.661838 (14) | 0.02892 (17) | |
F1 | 0.6682 (3) | 0.1981 (3) | 0.7195 (2) | 0.1068 (11) | |
F2 | 0.5350 (3) | 0.1968 (3) | 0.60083 (19) | 0.0921 (9) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0214 (2) | 0.0214 (2) | 0.0215 (4) | 0.01069 (12) | 0.000 | 0.000 |
N1 | 0.0328 (10) | 0.0315 (10) | 0.0331 (10) | 0.0171 (8) | −0.0006 (8) | −0.0040 (8) |
C1 | 0.0252 (10) | 0.0299 (11) | 0.0313 (11) | 0.0137 (9) | −0.0021 (8) | −0.0033 (9) |
C2 | 0.0416 (16) | 0.0364 (13) | 0.054 (2) | 0.0230 (13) | −0.0058 (11) | −0.0167 (13) |
Sb1 | 0.03148 (19) | 0.03148 (19) | 0.0238 (2) | 0.01574 (9) | 0.000 | 0.000 |
F1 | 0.111 (2) | 0.094 (2) | 0.118 (2) | 0.0533 (18) | −0.0103 (19) | 0.0595 (19) |
F2 | 0.0745 (16) | 0.0736 (16) | 0.120 (2) | 0.0309 (13) | −0.0527 (16) | −0.0450 (16) |
Fe1—N1i | 2.153 (2) | C2—H2B | 0.9800 |
Fe1—N1ii | 2.153 (2) | C2—H2C | 0.9800 |
Fe1—N1iii | 2.153 (2) | Sb1—F1 | 1.839 (2) |
Fe1—N1 | 2.153 (2) | Sb1—F1iii | 1.839 (2) |
Fe1—N1iv | 2.153 (2) | Sb1—F1ii | 1.839 (2) |
Fe1—N1v | 2.153 (2) | Sb1—F2iii | 1.854 (2) |
N1—C1 | 1.129 (3) | Sb1—F2 | 1.854 (2) |
C1—C2 | 1.455 (4) | Sb1—F2ii | 1.854 (2) |
C2—H2A | 0.9800 | ||
N1i—Fe1—N1ii | 180.0 | H2A—C2—H2B | 109.5 |
N1i—Fe1—N1iii | 88.10 (8) | C1—C2—H2C | 109.5 |
N1ii—Fe1—N1iii | 91.91 (8) | H2A—C2—H2C | 109.5 |
N1i—Fe1—N1 | 88.10 (8) | H2B—C2—H2C | 109.5 |
N1ii—Fe1—N1 | 91.91 (8) | F1—Sb1—F1iii | 93.15 (17) |
N1iii—Fe1—N1 | 91.91 (8) | F1—Sb1—F1ii | 93.15 (17) |
N1i—Fe1—N1iv | 91.91 (8) | F1iii—Sb1—F1ii | 93.15 (17) |
N1ii—Fe1—N1iv | 88.09 (8) | F1—Sb1—F2iii | 88.85 (16) |
N1iii—Fe1—N1iv | 180.0 | F1iii—Sb1—F2iii | 87.37 (16) |
N1—Fe1—N1iv | 88.10 (8) | F1ii—Sb1—F2iii | 177.90 (13) |
N1i—Fe1—N1v | 91.90 (8) | F1—Sb1—F2 | 87.37 (16) |
N1ii—Fe1—N1v | 88.09 (8) | F1iii—Sb1—F2 | 177.90 (13) |
N1iii—Fe1—N1v | 88.10 (8) | F1ii—Sb1—F2 | 88.85 (16) |
N1—Fe1—N1v | 180.0 | F2iii—Sb1—F2 | 90.60 (16) |
N1iv—Fe1—N1v | 91.90 (8) | F1—Sb1—F2ii | 177.90 (13) |
C1—N1—Fe1 | 175.4 (2) | F1iii—Sb1—F2ii | 88.85 (16) |
N1—C1—C2 | 179.3 (3) | F1ii—Sb1—F2ii | 87.37 (15) |
C1—C2—H2A | 109.5 | F2iii—Sb1—F2ii | 90.60 (16) |
C1—C2—H2B | 109.5 | F2—Sb1—F2ii | 90.60 (16) |
Symmetry codes: (i) x−y+1/3, x−1/3, −z+2/3; (ii) −x+y+1, −x+1, z; (iii) −y+1, x−y, 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 |
Mr | 773.67 |
Crystal system, space group | Hexagonal, R3 |
Temperature (K) | 173 |
a, c (Å) | 11.3398 (6), 17.3584 (11) |
V (Å3) | 1933.1 (2) |
Z | 3 |
Radiation type | Mo Kα |
µ (mm−1) | 2.73 |
Crystal size (mm) | 0.40 × 0.30 × 0.30 |
Data collection | |
Diffractometer | Bruker CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Blessing, 1995; Sheldrick, 2000) |
Tmin, Tmax | 0.602, 0.900 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5690, 996, 933 |
Rint | 0.028 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.069, 1.12 |
No. of reflections | 996 |
No. of parameters | 53 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 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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