Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807026827/at2319sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807026827/at2319Isup2.hkl |
CCDC reference: 655589
Ferrocene (2 g, 10.75 mmol) was dissolved in mesitylene and Al (0.29 g, 10.75 mmol), AlCl3 (5.73 g, 43 mmol) and H2O (0.22 ml, 10.75 mmol) were added. The crude mixture was heated at 373 K for 8 h followed by aqueous workup. The aqueous phase was treated with an ammonia solution and filtered. NH4PF6 was added to precipitate the title compound in 85% as a yellow solid. Single crystals were obtained from slow evaporation of a chloroform solution.
H atoms were refined using a riding model with fixed individual displacement parameters [Uiso(H) = 1.2Ueq(C) or Uiso(H) = 1.5Ueq(Cmethyl)] with C—H ranging from 0.95 Å to 1.00 Å. The cyclopentadienyl ring is disordered due to the symmetry of the special position. Since only nine sites were generated for the five atoms, the occupation factor of each site was set to 5/9 of is usual occupancy.
The title compound, [C14H17Fe]+PF6-.CHCl3, crystallizes with Z'=1/3. A l l there molecules are located on a special position with site symmetry 3 m. The cyclopentadienyl ring is disordered due to the symmetry of the special position.
Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; 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); software used to prepare material for publication: SHELXL97.
[Fe(C5H5)(C9H12)]PF6·CHCl3 | Dx = 1.662 Mg m−3 |
Mr = 505.46 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63mc | Cell parameters from 4866 reflections |
Hall symbol: P 6c -2c | θ = 4.1–25.7° |
a = 9.3640 (11) Å | µ = 1.27 mm−1 |
c = 13.3018 (19) Å | T = 173 K |
V = 1010.1 (2) Å3 | Block, yellow |
Z = 2 | 0.35 × 0.33 × 0.21 mm |
F(000) = 508 |
Stoe IPDS II two-circle diffractometer | 726 independent reflections |
Radiation source: fine-focus sealed tube | 711 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
ω scans | θmax = 25.6°, θmin = 4.0° |
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995) | h = −11→11 |
Tmin = 0.664, Tmax = 0.776 | k = −11→11 |
4236 measured reflections | l = −14→16 |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.036 | w = 1/[σ2(Fo2) + (0.0697P)2 + 0.3969P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.100 | (Δ/σ)max < 0.001 |
S = 1.13 | Δρmax = 0.43 e Å−3 |
726 reflections | Δρmin = −0.26 e Å−3 |
62 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1 restraint | Extinction coefficient: 0.021 (5) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), with 332 Friedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.02 (5) |
[Fe(C5H5)(C9H12)]PF6·CHCl3 | Z = 2 |
Mr = 505.46 | Mo Kα radiation |
Hexagonal, P63mc | µ = 1.27 mm−1 |
a = 9.3640 (11) Å | T = 173 K |
c = 13.3018 (19) Å | 0.35 × 0.33 × 0.21 mm |
V = 1010.1 (2) Å3 |
Stoe IPDS II two-circle diffractometer | 726 independent reflections |
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995) | 711 reflections with I > 2σ(I) |
Tmin = 0.664, Tmax = 0.776 | Rint = 0.023 |
4236 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | H-atom parameters constrained |
wR(F2) = 0.100 | Δρmax = 0.43 e Å−3 |
S = 1.13 | Δρmin = −0.26 e Å−3 |
726 reflections | Absolute structure: Flack (1983), with 332 Friedel pairs |
62 parameters | Absolute structure parameter: 0.02 (5) |
1 restraint |
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 | Occ. (<1) | |
Fe1 | 0.0000 | 0.0000 | 0.02847 (8) | 0.0288 (3) | |
C1 | −0.0886 (3) | 0.0886 (3) | 0.1437 (3) | 0.0403 (12) | |
C2 | −0.1726 (6) | −0.0863 (3) | 0.1437 (3) | 0.0402 (12) | |
H2 | −0.2897 | −0.1449 | 0.1437 | 0.048* | |
C3 | −0.1813 (3) | 0.1813 (3) | 0.1387 (5) | 0.0569 (13) | |
H3A | −0.2044 | 0.2044 | 0.2052 | 0.085* | |
H3B | −0.1156 | 0.2831 | 0.1033 | 0.085* | |
C4 | 0.0681 (9) | 0.1362 (19) | −0.1027 (15) | 0.080 (10) | 0.56 |
H4 | 0.1267 | 0.2533 | −0.1048 | 0.096* | 0.56 |
C4' | 0.1380 (14) | 0.0137 (13) | −0.0959 (6) | 0.049 (3) | 0.56 |
H4' | 0.2481 | 0.0339 | −0.0948 | 0.059* | 0.56 |
P1 | 0.6667 | 0.3333 | 0.47038 (15) | 0.0319 (4) | |
F1 | 0.5906 (3) | 0.1813 (7) | 0.5415 (6) | 0.140 (3) | |
F2 | 0.7417 (3) | 0.2583 (3) | 0.3980 (5) | 0.138 (2) | |
C5 | 0.3333 | 0.6667 | 0.2813 (8) | 0.0444 (17) | |
H5 | 0.3333 | 0.6667 | 0.2061 | 0.053* | |
Cl1 | 0.43613 (9) | 0.56387 (9) | 0.32191 (18) | 0.0737 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0348 (4) | 0.0348 (4) | 0.0170 (5) | 0.01738 (19) | 0.000 | 0.000 |
C1 | 0.052 (2) | 0.052 (2) | 0.025 (2) | 0.031 (2) | 0.0023 (9) | −0.0023 (9) |
C2 | 0.039 (3) | 0.050 (2) | 0.027 (2) | 0.0196 (13) | 0.0036 (18) | 0.0018 (9) |
C3 | 0.062 (3) | 0.062 (3) | 0.060 (3) | 0.042 (3) | 0.0068 (12) | −0.0068 (12) |
C4 | 0.14 (2) | 0.042 (7) | 0.029 (7) | 0.021 (3) | 0.006 (3) | 0.011 (5) |
C4' | 0.051 (5) | 0.071 (7) | 0.018 (3) | 0.024 (5) | 0.012 (3) | −0.009 (4) |
P1 | 0.0294 (5) | 0.0294 (5) | 0.0369 (9) | 0.0147 (3) | 0.000 | 0.000 |
F1 | 0.187 (6) | 0.067 (3) | 0.126 (5) | 0.0334 (15) | 0.0249 (18) | 0.050 (4) |
F2 | 0.187 (5) | 0.187 (5) | 0.119 (5) | 0.154 (6) | 0.0232 (14) | −0.0232 (14) |
C5 | 0.039 (2) | 0.039 (2) | 0.055 (4) | 0.0194 (12) | 0.000 | 0.000 |
Cl1 | 0.0620 (7) | 0.0620 (7) | 0.1108 (13) | 0.0411 (7) | −0.0044 (4) | 0.0044 (4) |
Fe1—C4' | 2.063 (9) | C3—H3A | 0.9600 |
Fe1—C4'i | 2.063 (9) | C3—H3B | 0.9608 |
Fe1—C4'ii | 2.063 (9) | C4—C4'i | 1.583 (9) |
Fe1—C4'iii | 2.063 (9) | C4—C4' | 1.583 (9) |
Fe1—C4'iv | 2.063 (9) | C4—H4 | 0.9501 |
Fe1—C4'v | 2.063 (9) | C4'—C4'iv | 1.42 (2) |
Fe1—C4iii | 2.065 (19) | C4'—H4' | 0.9500 |
Fe1—C4 | 2.065 (19) | P1—F2vi | 1.552 (5) |
Fe1—C4v | 2.065 (19) | P1—F2 | 1.552 (5) |
Fe1—C2iii | 2.076 (5) | P1—F2vii | 1.552 (5) |
Fe1—C2 | 2.076 (5) | P1—F1vii | 1.554 (5) |
Fe1—C2v | 2.076 (5) | P1—F1vi | 1.554 (5) |
C1—C2 | 1.419 (4) | P1—F1 | 1.554 (5) |
C1—C2iii | 1.419 (4) | C5—Cl1viii | 1.753 (4) |
C1—C3 | 1.505 (7) | C5—Cl1ix | 1.753 (4) |
C2—C1v | 1.419 (4) | C5—Cl1 | 1.753 (4) |
C2—H2 | 0.9500 | C5—H5 | 1.0000 |
C4'—Fe1—C2iii | 123.8 (3) | Fe1—C2—H2 | 132.4 |
C4'i—Fe1—C2iii | 123.8 (3) | C1—C3—H3A | 110.5 |
C4'ii—Fe1—C2iii | 105.2 (3) | C1—C3—H3B | 109.0 |
C4'iii—Fe1—C2iii | 163.3 (3) | H3A—C3—H3B | 109.4 |
C4'iv—Fe1—C2iii | 163.3 (3) | C4'ii—C4—C4'i | 132 (2) |
C4'v—Fe1—C2iii | 105.2 (3) | C4'v—C4—C4' | 132 (2) |
C4iii—Fe1—C2iii | 143.54 (12) | C4'i—C4—C4' | 101.8 (13) |
C4—Fe1—C2iii | 105.3 (5) | C4'v—C4—C4iii | 112.1 (18) |
C4v—Fe1—C2iii | 143.54 (12) | C4'ii—C4—C4v | 112.1 (18) |
C4'—Fe1—C2 | 163.3 (3) | C4'ii—C4—H4 | 97.8 |
C4'i—Fe1—C2 | 105.2 (3) | C4'v—C4—H4 | 97.8 |
C4'ii—Fe1—C2 | 163.3 (3) | C4'i—C4—H4 | 129.0 |
C4'iii—Fe1—C2 | 105.2 (3) | C4'—C4—H4 | 129.0 |
C4'iv—Fe1—C2 | 123.8 (3) | Fe1—C4—H4 | 124.0 |
C4'v—Fe1—C2 | 123.8 (3) | C4iii—C4'—C4'ii | 127.3 (18) |
C4iii—Fe1—C2 | 143.54 (12) | C4'ii—C4'—C4'iv | 119.998 (3) |
C4—Fe1—C2 | 143.54 (12) | C4iii—C4'—C4 | 106 (2) |
C4v—Fe1—C2 | 105.3 (5) | C4iii—C4'—H4' | 122.1 |
C2iii—Fe1—C2 | 71.5 (2) | C4'ii—C4'—H4' | 110.1 |
C4'—Fe1—C2v | 105.2 (3) | Fe1—C4'—H4' | 125.7 |
C4'i—Fe1—C2v | 163.3 (3) | F2vi—P1—F2 | 85.5 (4) |
C4'ii—Fe1—C2v | 123.8 (3) | F2vi—P1—F2vii | 85.5 (4) |
C4'iii—Fe1—C2v | 123.8 (3) | F2—P1—F2vii | 85.5 (4) |
C4'iv—Fe1—C2v | 105.2 (3) | F2vi—P1—F1vii | 179.2 (4) |
C4'v—Fe1—C2v | 163.3 (3) | F2—P1—F1vii | 93.8 (3) |
C4iii—Fe1—C2v | 105.3 (5) | F2vii—P1—F1vii | 93.8 (3) |
C4—Fe1—C2v | 143.54 (12) | F2vi—P1—F1vi | 93.8 (3) |
C4v—Fe1—C2v | 143.54 (12) | F2—P1—F1vi | 179.2 (4) |
C2iii—Fe1—C2v | 71.5 (2) | F2vii—P1—F1vi | 93.8 (3) |
C2—Fe1—C2v | 71.5 (2) | F1vii—P1—F1vi | 86.8 (4) |
C2—C1—C2iii | 117.4 (4) | F2vi—P1—F1 | 93.8 (3) |
C2—C1—C3 | 121.3 (2) | F2—P1—F1 | 93.8 (3) |
C2iii—C1—C3 | 121.3 (2) | F2vii—P1—F1 | 179.2 (5) |
C2—C1—Fe1 | 69.2 (2) | F1vii—P1—F1 | 86.8 (4) |
C2iii—C1—Fe1 | 69.2 (2) | F1vi—P1—F1 | 86.8 (4) |
C3—C1—Fe1 | 130.7 (4) | Cl1viii—C5—Cl1ix | 110.9 (3) |
C1v—C2—C1 | 122.6 (4) | Cl1viii—C5—Cl1 | 110.9 (3) |
C1v—C2—Fe1 | 71.1 (2) | Cl1ix—C5—Cl1 | 110.9 (3) |
C1—C2—Fe1 | 71.1 (2) | Cl1viii—C5—H5 | 108.0 |
C1v—C2—H2 | 118.7 | Cl1ix—C5—H5 | 108.0 |
C1—C2—H2 | 118.7 | Cl1—C5—H5 | 108.0 |
C4'—Fe1—C1—C2 | 174.8 (8) | C4'i—Fe1—C4—C4' | −114.4 (12) |
C4'i—Fe1—C1—C2 | 99.0 (3) | C4'ii—Fe1—C4—C4' | 30.1 (14) |
C4'ii—Fe1—C1—C2 | 163.4 (4) | C4'iii—Fe1—C4—C4' | −73.0 (7) |
C4'iii—Fe1—C1—C2 | 64.5 (4) | C4'iv—Fe1—C4—C4' | −41.4 (6) |
C4'iv—Fe1—C1—C2 | 53.0 (8) | C4'v—Fe1—C4—C4' | −145 (2) |
C4'v—Fe1—C1—C2 | 128.8 (4) | C4iii—Fe1—C4—C4' | −22.9 (7) |
C4iii—Fe1—C1—C2 | 113.9 (2) | C4v—Fe1—C4—C4' | −91.6 (5) |
C4—Fe1—C1—C2 | 144.9 (4) | C2iii—Fe1—C4—C4' | 122.8 (6) |
C4v—Fe1—C1—C2 | 83.0 (4) | C2—Fe1—C4—C4' | −157.9 (5) |
C2iii—Fe1—C1—C2 | −132.1 (4) | C2v—Fe1—C4—C4' | 43.5 (11) |
C2v—Fe1—C1—C2 | −66.1 (2) | C4'—Fe1—C4—C4iii | 22.9 (7) |
C4'—Fe1—C1—C2iii | −53.0 (8) | C4'i—Fe1—C4—C4iii | −91.6 (5) |
C4'i—Fe1—C1—C2iii | −128.8 (4) | C4'ii—Fe1—C4—C4iii | 53 (2) |
C4'ii—Fe1—C1—C2iii | −64.5 (4) | C4'iii—Fe1—C4—C4iii | −50.2 (3) |
C4'iii—Fe1—C1—C2iii | −163.4 (4) | C4'iv—Fe1—C4—C4iii | −18.5 (4) |
C4'iv—Fe1—C1—C2iii | −174.8 (8) | C4'v—Fe1—C4—C4iii | −121.7 (17) |
C4'v—Fe1—C1—C2iii | −99.0 (3) | C4v—Fe1—C4—C4iii | −68.7 (3) |
C4iii—Fe1—C1—C2iii | −113.9 (2) | C2iii—Fe1—C4—C4iii | 145.65 (14) |
C4—Fe1—C1—C2iii | −83.0 (4) | C2—Fe1—C4—C4iii | −135.0 (8) |
C4v—Fe1—C1—C2iii | −144.9 (4) | C2v—Fe1—C4—C4iii | 66.3 (5) |
C2—Fe1—C1—C2iii | 132.1 (4) | C4'—Fe1—C4—C4v | 91.6 (5) |
C2v—Fe1—C1—C2iii | 66.1 (2) | C4'i—Fe1—C4—C4v | −22.9 (7) |
C4'—Fe1—C1—C3 | 60.9 (8) | C4'ii—Fe1—C4—C4v | 121.7 (17) |
C4'i—Fe1—C1—C3 | −14.9 (3) | C4'iii—Fe1—C4—C4v | 18.5 (4) |
C4'ii—Fe1—C1—C3 | 49.5 (4) | C4'iv—Fe1—C4—C4v | 50.2 (3) |
C4'iii—Fe1—C1—C3 | −49.5 (4) | C4'v—Fe1—C4—C4v | −53 (2) |
C4'iv—Fe1—C1—C3 | −60.9 (8) | C4iii—Fe1—C4—C4v | 68.7 (3) |
C4'v—Fe1—C1—C3 | 14.9 (3) | C2iii—Fe1—C4—C4v | −145.65 (14) |
C4iii—Fe1—C1—C3 | −0.002 (2) | C2—Fe1—C4—C4v | −66.3 (5) |
C4—Fe1—C1—C3 | 30.9 (3) | C2v—Fe1—C4—C4v | 135.0 (8) |
C4v—Fe1—C1—C3 | −30.9 (3) | C4'ii—C4—C4'—C4iii | 180.003 (2) |
C2iii—Fe1—C1—C3 | 113.9 (2) | C4'v—C4—C4'—C4iii | 21 (6) |
C2—Fe1—C1—C3 | −113.9 (2) | C4'i—C4—C4'—C4iii | 13 (4) |
C2v—Fe1—C1—C3 | 180.0 | C4v—C4—C4'—C4iii | 8 (2) |
C2iii—C1—C2—C1v | −0.1 (7) | Fe1—C4—C4'—C4iii | 72 (3) |
C3—C1—C2—C1v | 177.0 (4) | C4'v—C4—C4'—C4'ii | −159 (6) |
Fe1—C1—C2—C1v | 51.3 (4) | C4'i—C4—C4'—C4'ii | −167 (4) |
C2iii—C1—C2—Fe1 | −51.3 (4) | C4iii—C4—C4'—C4'ii | 179.997 (2) |
C3—C1—C2—Fe1 | 125.8 (4) | C4v—C4—C4'—C4'ii | −172 (2) |
C4'—Fe1—C2—C1v | 51.1 (11) | Fe1—C4—C4'—C4'ii | −108 (3) |
C4'i—Fe1—C2—C1v | 132.9 (3) | C4'ii—C4—C4'—C4'iv | 172 (2) |
C4'ii—Fe1—C2—C1v | 172.9 (11) | C4'v—C4—C4'—C4'iv | 13 (4) |
C4'iii—Fe1—C2—C1v | 91.1 (4) | C4'i—C4—C4'—C4'iv | 4.6 (13) |
C4'iv—Fe1—C2—C1v | 66.2 (4) | C4iii—C4—C4'—C4'iv | −8 (2) |
C4'v—Fe1—C2—C1v | 157.7 (4) | C4v—C4—C4'—C4'iv | 0.0 |
C4iii—Fe1—C2—C1v | 60.8 (8) | Fe1—C4—C4'—C4'iv | 63.7 (3) |
C4—Fe1—C2—C1v | 163.2 (8) | C4'ii—C4—C4'—Fe1 | 108 (3) |
C4v—Fe1—C2—C1v | 112.0 (2) | C4'v—C4—C4'—Fe1 | −50 (4) |
C2iii—Fe1—C2—C1v | −106.02 (18) | C4'i—C4—C4'—Fe1 | −59.2 (10) |
C2v—Fe1—C2—C1v | −30.0 (2) | C4iii—C4—C4'—Fe1 | −72 (3) |
C4'—Fe1—C2—C1 | −172.9 (11) | C4v—C4—C4'—Fe1 | −63.7 (3) |
C4'i—Fe1—C2—C1 | −91.1 (4) | C4'i—Fe1—C4'—C4iii | −70 (2) |
C4'ii—Fe1—C2—C1 | −51.1 (11) | C4'ii—Fe1—C4'—C4iii | −133.0 (19) |
C4'iii—Fe1—C2—C1 | −132.9 (3) | C4'iii—Fe1—C4'—C4iii | −27.6 (18) |
C4'iv—Fe1—C2—C1 | −157.7 (4) | C4'iv—Fe1—C4'—C4iii | −3 (2) |
C4'v—Fe1—C2—C1 | −66.2 (4) | C4'v—Fe1—C4'—C4iii | −99.1 (17) |
C4iii—Fe1—C2—C1 | −163.2 (8) | C4—Fe1—C4'—C4iii | −112 (2) |
C4—Fe1—C2—C1 | −60.8 (8) | C4v—Fe1—C4'—C4iii | −49.2 (17) |
C4v—Fe1—C2—C1 | −112.0 (2) | C2iii—Fe1—C4'—C4iii | 170.5 (17) |
C2iii—Fe1—C2—C1 | 30.0 (2) | C2—Fe1—C4'—C4iii | 17 (3) |
C2v—Fe1—C2—C1 | 106.02 (18) | C2v—Fe1—C4'—C4iii | 92.9 (19) |
C4'—Fe1—C4—C4'ii | −30.1 (14) | C4'i—Fe1—C4'—C4'ii | 63.21 (18) |
C4'i—Fe1—C4—C4'ii | −145 (2) | C4'iii—Fe1—C4'—C4'ii | 105.4 (4) |
C4'iii—Fe1—C4—C4'ii | −103 (2) | C4'iv—Fe1—C4'—C4'ii | 130.19 (16) |
C4'iv—Fe1—C4—C4'ii | −71.6 (16) | C4'v—Fe1—C4'—C4'ii | 33.9 (4) |
C4'v—Fe1—C4—C4'ii | −175 (4) | C4iii—Fe1—C4'—C4'ii | 133.0 (19) |
C4iii—Fe1—C4—C4'ii | −53 (2) | C4—Fe1—C4'—C4'ii | 20.8 (7) |
C4v—Fe1—C4—C4'ii | −121.7 (17) | C4v—Fe1—C4'—C4'ii | 83.7 (2) |
C2iii—Fe1—C4—C4'ii | 92.6 (19) | C2iii—Fe1—C4'—C4'ii | −56.5 (2) |
C2—Fe1—C4—C4'ii | 171.9 (13) | C2—Fe1—C4'—C4'ii | 149.8 (11) |
C2v—Fe1—C4—C4'ii | 13 (2) | C2v—Fe1—C4'—C4'ii | −134.09 (14) |
C4'—Fe1—C4—C4'v | 145 (2) | C4'i—Fe1—C4'—C4'iv | −66.98 (19) |
C4'i—Fe1—C4—C4'v | 30.1 (14) | C4'ii—Fe1—C4'—C4'iv | −130.19 (16) |
C4'ii—Fe1—C4—C4'v | 175 (4) | C4'iii—Fe1—C4'—C4'iv | −24.8 (4) |
C4'iii—Fe1—C4—C4'v | 71.6 (16) | C4'v—Fe1—C4'—C4'iv | −96.3 (5) |
C4'iv—Fe1—C4—C4'v | 103 (2) | C4iii—Fe1—C4'—C4'iv | 3 (2) |
C4iii—Fe1—C4—C4'v | 121.7 (17) | C4—Fe1—C4'—C4'iv | −109.3 (6) |
C4v—Fe1—C4—C4'v | 53 (2) | C4v—Fe1—C4'—C4'iv | −46.4 (3) |
C2iii—Fe1—C4—C4'v | −92.6 (19) | C2iii—Fe1—C4'—C4'iv | 173.3 (3) |
C2—Fe1—C4—C4'v | −13 (2) | C2—Fe1—C4'—C4'iv | 19.7 (10) |
C2v—Fe1—C4—C4'v | −171.9 (13) | C2v—Fe1—C4'—C4'iv | 95.72 (14) |
C4'—Fe1—C4—C4'i | 114.4 (12) | C4'i—Fe1—C4'—C4 | 42.4 (7) |
C4'ii—Fe1—C4—C4'i | 145 (2) | C4'ii—Fe1—C4'—C4 | −20.8 (7) |
C4'iii—Fe1—C4—C4'i | 41.4 (6) | C4'iii—Fe1—C4'—C4 | 84.6 (7) |
C4'iv—Fe1—C4—C4'i | 73.0 (7) | C4'iv—Fe1—C4'—C4 | 109.3 (6) |
C4'v—Fe1—C4—C4'i | −30.1 (14) | C4'v—Fe1—C4'—C4 | 13.0 (8) |
C4iii—Fe1—C4—C4'i | 91.6 (5) | C4iii—Fe1—C4'—C4 | 112 (2) |
C4v—Fe1—C4—C4'i | 22.9 (7) | C4v—Fe1—C4'—C4 | 62.9 (8) |
C2iii—Fe1—C4—C4'i | −122.8 (6) | C2iii—Fe1—C4'—C4 | −77.3 (8) |
C2—Fe1—C4—C4'i | −43.5 (11) | C2—Fe1—C4'—C4 | 129.0 (8) |
C2v—Fe1—C4—C4'i | 157.9 (5) | C2v—Fe1—C4'—C4 | −154.9 (6) |
Symmetry codes: (i) −x+y, y, z; (ii) x, x−y, z; (iii) −x+y, −x, z; (iv) −y, −x, z; (v) −y, x−y, z; (vi) −x+y+1, −x+1, z; (vii) −y+1, x−y, z; (viii) −x+y, −x+1, z; (ix) −y+1, x−y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [Fe(C5H5)(C9H12)]PF6·CHCl3 |
Mr | 505.46 |
Crystal system, space group | Hexagonal, P63mc |
Temperature (K) | 173 |
a, c (Å) | 9.3640 (11), 13.3018 (19) |
V (Å3) | 1010.1 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.27 |
Crystal size (mm) | 0.35 × 0.33 × 0.21 |
Data collection | |
Diffractometer | Stoe IPDS II two-circle |
Absorption correction | Multi-scan (MULABS; Spek, 2003; Blessing, 1995) |
Tmin, Tmax | 0.664, 0.776 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4236, 726, 711 |
Rint | 0.023 |
(sin θ/λ)max (Å−1) | 0.607 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.100, 1.13 |
No. of reflections | 726 |
No. of parameters | 62 |
No. of restraints | 1 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.43, −0.26 |
Absolute structure | Flack (1983), with 332 Friedel pairs |
Absolute structure parameter | 0.02 (5) |
Computer programs: X-AREA (Stoe & Cie, 2001), X-AREA, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP in SHELXTL-Plus (Sheldrick, 1991), SHELXL97.
The title compound, [C14H17Fe]+PF6-.CHCl3, crystallizes with Z'=1/3. A l l there molecules are located on a special position with site symmetry 3 m. The cyclopentadienyl ring is disordered due to the symmetry of the special position.