Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680504167X/sj6183sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680504167X/sj6183Isup2.hkl |
CCDC reference: 296668
Key indicators
- Single-crystal X-ray study
- T = 292 K
- Mean (C-C) = 0.005 Å
- Disorder in solvent or counterion
- R factor = 0.046
- wR factor = 0.129
- Data-to-parameter ratio = 14.6
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Co1
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.58 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C2 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C4 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C5 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P2 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 36.00 Perc.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion
The title compound was prepared according to the method of Brasse et al. (2000). Single crystals were obtained by show diffusion of diethyl ether into a solution of the compound in acetone.
At an early stage in the refinement, disorder was apparent in four of the F atoms of the hexafluorophosphate anion. The disordered F atoms were assigned the same isotropic displacement parameters, and bond distances in the minor disorder component were constrained using DFIX and PART in SHELXL (Sheldrick, 1997). The occupation factors of the two components converged at 0.799 (6) and 0.201 (6). All H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms, with aromatic C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C).
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; 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.
[Co(C5H5)(C17H14P)]PF6 | F(000) = 2096 |
Mr = 518.24 | Dx = 1.557 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 4616 reflections |
a = 36.813 (3) Å | θ = 2.2–26.0° |
b = 10.2263 (8) Å | µ = 0.98 mm−1 |
c = 11.9059 (9) Å | T = 292 K |
β = 99.469 (1)° | Block, yellow |
V = 4421.0 (6) Å3 | 0.30 × 0.30 × 0.30 mm |
Z = 8 |
Bruker SMART CCD area-detector diffractometer | 4335 independent reflections |
Radiation source: fine-focus sealed tube | 3275 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.054 |
ϕ and ω scans | θmax = 26.0°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −45→39 |
Tmin = 0.758, Tmax = 0.758 | k = −12→12 |
14389 measured reflections | l = −11→14 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.129 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.074P)2] where P = (Fo2 + 2Fc2)/3 |
4335 reflections | (Δ/σ)max < 0.001 |
297 parameters | Δρmax = 0.40 e Å−3 |
8 restraints | Δρmin = −0.27 e Å−3 |
[Co(C5H5)(C17H14P)]PF6 | V = 4421.0 (6) Å3 |
Mr = 518.24 | Z = 8 |
Monoclinic, C2/c | Mo Kα radiation |
a = 36.813 (3) Å | µ = 0.98 mm−1 |
b = 10.2263 (8) Å | T = 292 K |
c = 11.9059 (9) Å | 0.30 × 0.30 × 0.30 mm |
β = 99.469 (1)° |
Bruker SMART CCD area-detector diffractometer | 4335 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3275 reflections with I > 2σ(I) |
Tmin = 0.758, Tmax = 0.758 | Rint = 0.054 |
14389 measured reflections |
R[F2 > 2σ(F2)] = 0.046 | 8 restraints |
wR(F2) = 0.129 | H-atom parameters constrained |
S = 1.04 | Δρmax = 0.40 e Å−3 |
4335 reflections | Δρmin = −0.27 e Å−3 |
297 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 | Occ. (<1) | |
Co1 | 0.574497 (11) | 0.73432 (4) | 0.56912 (3) | 0.05056 (16) | |
C1 | 0.5811 (2) | 0.8233 (5) | 0.7214 (3) | 0.1031 (16) | |
H1 | 0.5940 | 0.9061 | 0.7408 | 0.124* | |
C2 | 0.54694 (19) | 0.8104 (6) | 0.6854 (4) | 0.1052 (16) | |
H2 | 0.5299 | 0.8843 | 0.6701 | 0.126* | |
C3 | 0.53731 (14) | 0.6919 (7) | 0.6684 (4) | 0.1077 (16) | |
H3 | 0.5121 | 0.6622 | 0.6410 | 0.129* | |
C4 | 0.5668 (2) | 0.6129 (4) | 0.6948 (4) | 0.1112 (19) | |
H4 | 0.5670 | 0.5171 | 0.6929 | 0.133* | |
C5 | 0.59735 (12) | 0.6967 (8) | 0.7305 (3) | 0.116 (2) | |
H5 | 0.6229 | 0.6727 | 0.7603 | 0.140* | |
C6 | 0.59172 (9) | 0.8557 (3) | 0.4538 (2) | 0.0593 (7) | |
H6 | 0.6010 | 0.9449 | 0.4690 | 0.071* | |
C7 | 0.55452 (9) | 0.8207 (4) | 0.4190 (3) | 0.0704 (9) | |
H7 | 0.5336 | 0.8812 | 0.4050 | 0.084* | |
C8 | 0.55266 (9) | 0.6832 (4) | 0.4077 (3) | 0.0681 (8) | |
H8 | 0.5303 | 0.6315 | 0.3847 | 0.082* | |
C9 | 0.58881 (7) | 0.6334 (3) | 0.4357 (2) | 0.0536 (7) | |
H9 | 0.5957 | 0.5407 | 0.4365 | 0.064* | |
C10 | 0.61356 (8) | 0.7396 (2) | 0.4639 (2) | 0.0469 (6) | |
C11 | 0.67390 (7) | 0.5686 (2) | 0.4723 (2) | 0.0492 (6) | |
C12 | 0.66697 (8) | 0.4687 (3) | 0.5436 (3) | 0.0661 (8) | |
H12 | 0.6564 | 0.4876 | 0.6075 | 0.079* | |
C13 | 0.67563 (10) | 0.3407 (3) | 0.5212 (4) | 0.0820 (11) | |
H13 | 0.6702 | 0.2735 | 0.5684 | 0.098* | |
C14 | 0.69213 (11) | 0.3137 (3) | 0.4298 (4) | 0.0873 (12) | |
H14 | 0.6983 | 0.2278 | 0.4154 | 0.105* | |
C15 | 0.69975 (10) | 0.4115 (3) | 0.3588 (3) | 0.0806 (10) | |
H15 | 0.7112 | 0.3921 | 0.2968 | 0.097* | |
C16 | 0.69048 (8) | 0.5387 (3) | 0.3791 (3) | 0.0615 (8) | |
H16 | 0.6954 | 0.6048 | 0.3300 | 0.074* | |
C17 | 0.68002 (7) | 0.8382 (2) | 0.4083 (2) | 0.0454 (6) | |
C18 | 0.71507 (7) | 0.8906 (3) | 0.4393 (3) | 0.0553 (7) | |
H18 | 0.7286 | 0.8709 | 0.5103 | 0.066* | |
C19 | 0.72991 (8) | 0.9709 (3) | 0.3666 (3) | 0.0696 (9) | |
H19 | 0.7535 | 1.0047 | 0.3880 | 0.084* | |
C20 | 0.70995 (9) | 1.0015 (3) | 0.2624 (3) | 0.0702 (9) | |
H20 | 0.7200 | 1.0566 | 0.2135 | 0.084* | |
C21 | 0.67533 (9) | 0.9514 (3) | 0.2296 (3) | 0.0657 (8) | |
H21 | 0.6620 | 0.9722 | 0.1586 | 0.079* | |
C22 | 0.66034 (8) | 0.8699 (3) | 0.3026 (2) | 0.0579 (7) | |
H22 | 0.6368 | 0.8360 | 0.2804 | 0.069* | |
F1 | 0.46340 (7) | 0.8599 (2) | 0.5166 (2) | 0.1281 (10) | |
F3 | 0.40790 (6) | 0.6784 (2) | 0.3582 (2) | 0.1051 (8) | |
F2 | 0.46675 (8) | 0.7054 (4) | 0.3794 (4) | 0.1273 (18) | 0.799 (6) |
F6 | 0.44228 (17) | 0.6614 (3) | 0.5326 (3) | 0.1349 (19) | 0.799 (6) |
F4 | 0.40419 (9) | 0.8300 (4) | 0.4950 (4) | 0.1260 (17) | 0.799 (6) |
F5 | 0.42715 (12) | 0.8769 (3) | 0.3443 (3) | 0.1285 (17) | 0.799 (6) |
P1 | 0.66317 (2) | 0.73511 (7) | 0.51418 (6) | 0.0487 (2) | |
P2 | 0.43623 (2) | 0.76799 (7) | 0.43801 (7) | 0.0568 (2) | |
F2' | 0.4588 (4) | 0.8384 (13) | 0.3552 (10) | 0.100 (5)* | 0.201 (6) |
F4' | 0.4139 (4) | 0.6996 (13) | 0.5184 (10) | 0.094 (4)* | 0.201 (6) |
F6' | 0.4655 (3) | 0.6569 (9) | 0.4644 (12) | 0.076 (3)* | 0.201 (6) |
F5' | 0.4063 (3) | 0.8747 (9) | 0.4184 (10) | 0.068 (3)* | 0.201 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0527 (3) | 0.0568 (3) | 0.0452 (3) | 0.00436 (16) | 0.01689 (19) | −0.00092 (16) |
C1 | 0.153 (5) | 0.110 (4) | 0.053 (2) | −0.045 (3) | 0.036 (3) | −0.025 (2) |
C2 | 0.132 (5) | 0.121 (4) | 0.077 (3) | 0.048 (3) | 0.060 (3) | 0.009 (3) |
C3 | 0.098 (3) | 0.169 (5) | 0.063 (3) | −0.049 (4) | 0.034 (2) | 0.002 (3) |
C4 | 0.227 (7) | 0.058 (2) | 0.059 (3) | 0.011 (3) | 0.054 (4) | 0.0127 (18) |
C5 | 0.073 (3) | 0.245 (6) | 0.0340 (19) | 0.065 (4) | 0.0158 (19) | 0.030 (3) |
C6 | 0.070 (2) | 0.0584 (16) | 0.0540 (18) | 0.0111 (14) | 0.0251 (15) | 0.0102 (14) |
C7 | 0.059 (2) | 0.101 (2) | 0.0531 (19) | 0.0268 (18) | 0.0173 (16) | 0.0191 (17) |
C8 | 0.0533 (18) | 0.101 (2) | 0.0511 (19) | 0.0007 (17) | 0.0108 (15) | −0.0115 (17) |
C9 | 0.0504 (16) | 0.0661 (16) | 0.0458 (16) | 0.0004 (13) | 0.0128 (13) | −0.0116 (13) |
C10 | 0.0501 (16) | 0.0532 (14) | 0.0398 (15) | 0.0034 (11) | 0.0148 (12) | −0.0013 (11) |
C11 | 0.0396 (14) | 0.0518 (14) | 0.0552 (17) | −0.0003 (11) | 0.0047 (12) | 0.0034 (12) |
C12 | 0.0594 (18) | 0.0641 (18) | 0.078 (2) | 0.0034 (14) | 0.0206 (16) | 0.0135 (16) |
C13 | 0.071 (2) | 0.0612 (19) | 0.114 (3) | 0.0014 (17) | 0.014 (2) | 0.016 (2) |
C14 | 0.083 (3) | 0.0528 (18) | 0.125 (4) | 0.0071 (18) | 0.014 (3) | −0.008 (2) |
C15 | 0.082 (2) | 0.073 (2) | 0.091 (3) | 0.0081 (18) | 0.026 (2) | −0.016 (2) |
C16 | 0.0647 (18) | 0.0597 (17) | 0.0624 (19) | 0.0019 (14) | 0.0175 (16) | −0.0039 (14) |
C17 | 0.0483 (15) | 0.0460 (13) | 0.0420 (15) | 0.0007 (11) | 0.0077 (12) | −0.0039 (11) |
C18 | 0.0468 (15) | 0.0612 (16) | 0.0568 (18) | −0.0017 (13) | 0.0049 (13) | −0.0006 (14) |
C19 | 0.0491 (17) | 0.078 (2) | 0.083 (3) | −0.0136 (15) | 0.0123 (17) | 0.0048 (17) |
C20 | 0.070 (2) | 0.0683 (18) | 0.078 (2) | −0.0048 (16) | 0.0271 (18) | 0.0151 (17) |
C21 | 0.069 (2) | 0.0712 (19) | 0.0559 (19) | −0.0004 (16) | 0.0072 (16) | 0.0160 (15) |
C22 | 0.0521 (16) | 0.0653 (17) | 0.0541 (18) | −0.0057 (13) | 0.0022 (14) | 0.0012 (14) |
F1 | 0.1131 (18) | 0.0964 (15) | 0.153 (2) | −0.0172 (14) | −0.0440 (17) | −0.0301 (16) |
F3 | 0.0875 (15) | 0.0799 (13) | 0.135 (2) | 0.0043 (11) | −0.0217 (14) | −0.0312 (14) |
F2 | 0.0677 (19) | 0.162 (4) | 0.160 (4) | 0.0091 (19) | 0.044 (2) | −0.045 (3) |
F6 | 0.215 (5) | 0.091 (2) | 0.090 (2) | −0.015 (3) | −0.001 (3) | 0.0377 (17) |
F4 | 0.114 (3) | 0.117 (3) | 0.162 (4) | −0.008 (2) | 0.068 (3) | −0.052 (3) |
F5 | 0.159 (4) | 0.095 (2) | 0.116 (3) | −0.020 (2) | −0.024 (3) | 0.0532 (19) |
P1 | 0.0495 (4) | 0.0538 (4) | 0.0428 (4) | −0.0024 (3) | 0.0075 (3) | −0.0010 (3) |
P2 | 0.0582 (5) | 0.0543 (4) | 0.0569 (5) | −0.0019 (3) | 0.0062 (4) | 0.0016 (3) |
Co1—C3 | 1.998 (4) | C11—P1 | 1.836 (3) |
Co1—C4 | 2.000 (4) | C12—C13 | 1.384 (4) |
Co1—C2 | 2.003 (4) | C12—H12 | 0.9300 |
Co1—C5 | 2.004 (3) | C13—C14 | 1.359 (6) |
Co1—C1 | 2.008 (4) | C13—H13 | 0.9300 |
Co1—C7 | 2.021 (3) | C14—C15 | 1.369 (5) |
Co1—C8 | 2.026 (3) | C14—H14 | 0.9300 |
Co1—C6 | 2.028 (3) | C15—C16 | 1.375 (4) |
Co1—C9 | 2.035 (3) | C15—H15 | 0.9300 |
Co1—C10 | 2.058 (3) | C16—H16 | 0.9300 |
C1—C2 | 1.267 (7) | C17—C22 | 1.383 (4) |
C1—C5 | 1.423 (7) | C17—C18 | 1.390 (3) |
C1—H1 | 0.9800 | C17—P1 | 1.829 (3) |
C2—C3 | 1.269 (7) | C18—C19 | 1.371 (4) |
C2—H2 | 0.9800 | C18—H18 | 0.9300 |
C3—C4 | 1.349 (7) | C19—C20 | 1.370 (4) |
C3—H3 | 0.9800 | C19—H19 | 0.9300 |
C4—C5 | 1.422 (7) | C20—C21 | 1.369 (4) |
C4—H4 | 0.9800 | C20—H20 | 0.9300 |
C5—H5 | 0.9800 | C21—C22 | 1.383 (4) |
C6—C7 | 1.410 (4) | C21—H21 | 0.9300 |
C6—C10 | 1.428 (4) | C22—H22 | 0.9300 |
C6—H6 | 0.9800 | F1—P2 | 1.566 (2) |
C7—C8 | 1.414 (5) | F3—P2 | 1.582 (2) |
C7—H7 | 0.9800 | F2—P2 | 1.554 (3) |
C8—C9 | 1.413 (4) | F6—P2 | 1.557 (3) |
C8—H8 | 0.9800 | F4—P2 | 1.586 (3) |
C9—C10 | 1.422 (4) | F5—P2 | 1.573 (3) |
C9—H9 | 0.9800 | P2—F4' | 1.530 (8) |
C10—P1 | 1.826 (3) | P2—F5' | 1.541 (7) |
C11—C12 | 1.379 (4) | P2—F6' | 1.561 (7) |
C11—C16 | 1.386 (4) | P2—F2' | 1.565 (8) |
C3—Co1—C4 | 39.45 (19) | C8—C9—C10 | 108.8 (3) |
C3—Co1—C2 | 37.0 (2) | C8—C9—Co1 | 69.31 (17) |
C4—Co1—C2 | 64.81 (19) | C10—C9—Co1 | 70.53 (16) |
C3—Co1—C5 | 67.14 (19) | C8—C9—H9 | 125.6 |
C4—Co1—C5 | 41.6 (2) | C10—C9—H9 | 125.6 |
C2—Co1—C5 | 65.95 (19) | Co1—C9—H9 | 125.6 |
C3—Co1—C1 | 63.70 (19) | C9—C10—C6 | 106.6 (3) |
C4—Co1—C1 | 67.46 (18) | C9—C10—P1 | 128.7 (2) |
C2—Co1—C1 | 36.8 (2) | C6—C10—P1 | 124.5 (2) |
C5—Co1—C1 | 41.5 (2) | C9—C10—Co1 | 68.82 (16) |
C3—Co1—C7 | 115.7 (2) | C6—C10—Co1 | 68.45 (16) |
C4—Co1—C7 | 149.0 (3) | P1—C10—Co1 | 124.12 (15) |
C2—Co1—C7 | 106.82 (18) | C12—C11—C16 | 118.7 (3) |
C5—Co1—C7 | 165.1 (3) | C12—C11—P1 | 116.7 (2) |
C1—Co1—C7 | 125.0 (2) | C16—C11—P1 | 124.4 (2) |
C3—Co1—C8 | 107.55 (17) | C11—C12—C13 | 120.6 (3) |
C4—Co1—C8 | 117.8 (2) | C11—C12—H12 | 119.7 |
C2—Co1—C8 | 126.1 (2) | C13—C12—H12 | 119.7 |
C5—Co1—C8 | 154.0 (3) | C14—C13—C12 | 119.7 (4) |
C1—Co1—C8 | 160.7 (2) | C14—C13—H13 | 120.2 |
C7—Co1—C8 | 40.89 (15) | C12—C13—H13 | 120.2 |
C3—Co1—C6 | 148.7 (2) | C13—C14—C15 | 120.6 (3) |
C4—Co1—C6 | 170.0 (3) | C13—C14—H14 | 119.7 |
C2—Co1—C6 | 118.70 (19) | C15—C14—H14 | 119.7 |
C5—Co1—C6 | 129.6 (2) | C14—C15—C16 | 120.0 (3) |
C1—Co1—C6 | 109.22 (16) | C14—C15—H15 | 120.0 |
C7—Co1—C6 | 40.76 (13) | C16—C15—H15 | 120.0 |
C8—Co1—C6 | 68.61 (14) | C15—C16—C11 | 120.3 (3) |
C3—Co1—C9 | 130.0 (2) | C15—C16—H16 | 119.9 |
C4—Co1—C9 | 110.82 (15) | C11—C16—H16 | 119.9 |
C2—Co1—C9 | 164.1 (2) | C22—C17—C18 | 118.4 (3) |
C5—Co1—C9 | 121.96 (18) | C22—C17—P1 | 125.2 (2) |
C1—Co1—C9 | 157.9 (2) | C18—C17—P1 | 116.4 (2) |
C7—Co1—C9 | 68.58 (13) | C19—C18—C17 | 120.8 (3) |
C8—Co1—C9 | 40.71 (12) | C19—C18—H18 | 119.6 |
C6—Co1—C9 | 68.42 (13) | C17—C18—H18 | 119.6 |
C3—Co1—C10 | 169.0 (2) | C20—C19—C18 | 119.9 (3) |
C4—Co1—C10 | 132.1 (2) | C20—C19—H19 | 120.1 |
C2—Co1—C10 | 153.5 (2) | C18—C19—H19 | 120.1 |
C5—Co1—C10 | 111.33 (14) | C21—C20—C19 | 120.6 (3) |
C1—Co1—C10 | 123.05 (19) | C21—C20—H20 | 119.7 |
C7—Co1—C10 | 68.84 (12) | C19—C20—H20 | 119.7 |
C8—Co1—C10 | 68.71 (12) | C20—C21—C22 | 119.7 (3) |
C6—Co1—C10 | 40.91 (10) | C20—C21—H21 | 120.2 |
C9—Co1—C10 | 40.65 (10) | C22—C21—H21 | 120.2 |
C2—C1—C5 | 108.2 (5) | C17—C22—C21 | 120.6 (3) |
C2—C1—Co1 | 71.4 (3) | C17—C22—H22 | 119.7 |
C5—C1—Co1 | 69.1 (2) | C21—C22—H22 | 119.7 |
C2—C1—H1 | 125.9 | C10—P1—C17 | 101.17 (12) |
C5—C1—H1 | 125.9 | C10—P1—C11 | 100.51 (11) |
Co1—C1—H1 | 125.9 | C17—P1—C11 | 103.59 (12) |
C1—C2—C3 | 112.9 (5) | F4'—P2—F5' | 88.5 (7) |
C1—C2—Co1 | 71.8 (3) | F4'—P2—F2 | 126.5 (6) |
C3—C2—Co1 | 71.3 (3) | F5'—P2—F2 | 140.8 (5) |
C1—C2—H2 | 123.5 | F5'—P2—F6 | 128.3 (5) |
C3—C2—H2 | 123.5 | F2—P2—F6 | 90.5 (2) |
Co1—C2—H2 | 123.5 | F4'—P2—F6' | 88.0 (7) |
C2—C3—C4 | 110.0 (5) | F5'—P2—F6' | 176.4 (7) |
C2—C3—Co1 | 71.7 (3) | F6—P2—F6' | 48.1 (5) |
C4—C3—Co1 | 70.3 (3) | F4'—P2—F2' | 179.5 (8) |
C2—C3—H3 | 125.0 | F5'—P2—F2' | 91.1 (7) |
C4—C3—H3 | 125.0 | F2—P2—F2' | 53.8 (5) |
Co1—C3—H3 | 125.0 | F6—P2—F2' | 138.6 (6) |
C3—C4—C5 | 106.0 (4) | F6'—P2—F2' | 92.4 (7) |
C3—C4—Co1 | 70.2 (2) | F4'—P2—F1 | 104.9 (5) |
C5—C4—Co1 | 69.4 (2) | F5'—P2—F1 | 92.0 (4) |
C3—C4—H4 | 127.0 | F2—P2—F1 | 94.47 (17) |
C5—C4—H4 | 127.0 | F6—P2—F1 | 89.22 (19) |
Co1—C4—H4 | 127.0 | F6'—P2—F1 | 88.0 (4) |
C4—C5—C1 | 102.9 (4) | F2'—P2—F1 | 75.4 (5) |
C4—C5—Co1 | 69.0 (2) | F4'—P2—F5 | 134.0 (6) |
C1—C5—Co1 | 69.4 (2) | F5'—P2—F5 | 47.8 (4) |
C4—C5—H5 | 128.4 | F2—P2—F5 | 93.3 (3) |
C1—C5—H5 | 128.4 | F6—P2—F5 | 175.8 (3) |
Co1—C5—H5 | 128.4 | F6'—P2—F5 | 135.8 (6) |
C7—C6—C10 | 108.7 (3) | F2'—P2—F5 | 45.6 (5) |
C7—C6—Co1 | 69.34 (17) | F1—P2—F5 | 92.25 (16) |
C10—C6—Co1 | 70.64 (16) | F4'—P2—F3 | 75.0 (5) |
C7—C6—H6 | 125.7 | F5'—P2—F3 | 86.3 (4) |
C10—C6—H6 | 125.7 | F2—P2—F3 | 86.90 (16) |
Co1—C6—H6 | 125.7 | F6—P2—F3 | 91.78 (19) |
C6—C7—C8 | 108.0 (3) | F6'—P2—F3 | 93.7 (4) |
C6—C7—Co1 | 69.91 (17) | F2'—P2—F3 | 104.7 (5) |
C8—C7—Co1 | 69.75 (17) | F1—P2—F3 | 178.30 (13) |
C6—C7—H7 | 126.0 | F5—P2—F3 | 86.67 (16) |
C8—C7—H7 | 126.0 | F4'—P2—F4 | 53.2 (6) |
Co1—C7—H7 | 126.0 | F2—P2—F4 | 178.3 (2) |
C9—C8—C7 | 107.9 (3) | F6—P2—F4 | 89.9 (3) |
C9—C8—Co1 | 69.99 (17) | F6'—P2—F4 | 137.8 (6) |
C7—C8—Co1 | 69.36 (17) | F2'—P2—F4 | 126.5 (6) |
C9—C8—H8 | 126.0 | F1—P2—F4 | 87.20 (17) |
C7—C8—H8 | 126.0 | F5—P2—F4 | 86.2 (2) |
Co1—C8—H8 | 126.0 | F3—P2—F4 | 91.43 (16) |
C3—Co1—C1—C2 | −34.3 (4) | C8—Co1—C7—C6 | −119.1 (3) |
C4—Co1—C1—C2 | −77.6 (4) | C9—Co1—C7—C6 | −81.38 (19) |
C5—Co1—C1—C2 | −118.8 (5) | C10—Co1—C7—C6 | −37.61 (17) |
C7—Co1—C1—C2 | 69.8 (4) | C3—Co1—C7—C8 | −87.5 (3) |
C8—Co1—C1—C2 | 32.5 (7) | C4—Co1—C7—C8 | −57.3 (4) |
C6—Co1—C1—C2 | 112.5 (3) | C2—Co1—C7—C8 | −126.2 (3) |
C9—Co1—C1—C2 | −167.7 (4) | C5—Co1—C7—C8 | 175.1 (5) |
C10—Co1—C1—C2 | 155.8 (3) | C1—Co1—C7—C8 | −162.2 (3) |
C3—Co1—C1—C5 | 84.5 (3) | C6—Co1—C7—C8 | 119.1 (3) |
C4—Co1—C1—C5 | 41.2 (3) | C9—Co1—C7—C8 | 37.73 (17) |
C2—Co1—C1—C5 | 118.8 (5) | C10—Co1—C7—C8 | 81.51 (18) |
C7—Co1—C1—C5 | −171.4 (3) | C6—C7—C8—C9 | 0.0 (3) |
C8—Co1—C1—C5 | 151.3 (5) | Co1—C7—C8—C9 | −59.6 (2) |
C6—Co1—C1—C5 | −128.7 (3) | C6—C7—C8—Co1 | 59.6 (2) |
C9—Co1—C1—C5 | −48.9 (5) | C3—Co1—C8—C9 | −131.7 (3) |
C10—Co1—C1—C5 | −85.4 (3) | C4—Co1—C8—C9 | −90.2 (3) |
C5—C1—C2—C3 | 0.1 (5) | C2—Co1—C8—C9 | −168.0 (3) |
Co1—C1—C2—C3 | 59.6 (3) | C5—Co1—C8—C9 | −58.0 (4) |
C5—C1—C2—Co1 | −59.5 (3) | C1—Co1—C8—C9 | 168.5 (4) |
C3—Co1—C2—C1 | 123.0 (5) | C7—Co1—C8—C9 | 119.1 (3) |
C4—Co1—C2—C1 | 85.5 (4) | C6—Co1—C8—C9 | 81.4 (2) |
C5—Co1—C2—C1 | 39.5 (4) | C10—Co1—C8—C9 | 37.28 (17) |
C7—Co1—C2—C1 | −126.5 (4) | C3—Co1—C8—C7 | 109.2 (3) |
C8—Co1—C2—C1 | −167.3 (3) | C4—Co1—C8—C7 | 150.7 (3) |
C6—Co1—C2—C1 | −84.0 (4) | C2—Co1—C8—C7 | 72.9 (3) |
C9—Co1—C2—C1 | 162.9 (5) | C5—Co1—C8—C7 | −177.1 (3) |
C10—Co1—C2—C1 | −50.3 (5) | C1—Co1—C8—C7 | 49.4 (5) |
C4—Co1—C2—C3 | −37.5 (3) | C6—Co1—C8—C7 | −37.78 (17) |
C5—Co1—C2—C3 | −83.4 (4) | C9—Co1—C8—C7 | −119.1 (3) |
C1—Co1—C2—C3 | −123.0 (5) | C10—Co1—C8—C7 | −81.85 (18) |
C7—Co1—C2—C3 | 110.5 (4) | C7—C8—C9—C10 | −0.4 (3) |
C8—Co1—C2—C3 | 69.7 (4) | Co1—C8—C9—C10 | −59.7 (2) |
C6—Co1—C2—C3 | 153.1 (3) | C7—C8—C9—Co1 | 59.2 (2) |
C9—Co1—C2—C3 | 39.9 (8) | C3—Co1—C9—C8 | 68.3 (3) |
C10—Co1—C2—C3 | −173.3 (3) | C4—Co1—C9—C8 | 108.9 (3) |
C1—C2—C3—C4 | 0.3 (6) | C2—Co1—C9—C8 | 38.0 (7) |
Co1—C2—C3—C4 | 60.2 (3) | C5—Co1—C9—C8 | 154.0 (3) |
C1—C2—C3—Co1 | −59.9 (4) | C1—Co1—C9—C8 | −170.0 (4) |
C4—Co1—C3—C2 | 120.0 (5) | C7—Co1—C9—C8 | −37.9 (2) |
C5—Co1—C3—C2 | 79.9 (4) | C6—Co1—C9—C8 | −81.8 (2) |
C1—Co1—C3—C2 | 34.1 (3) | C10—Co1—C9—C8 | −120.0 (3) |
C7—Co1—C3—C2 | −84.0 (4) | C3—Co1—C9—C10 | −171.8 (3) |
C8—Co1—C3—C2 | −127.3 (4) | C4—Co1—C9—C10 | −131.2 (3) |
C6—Co1—C3—C2 | −49.8 (5) | C2—Co1—C9—C10 | 157.9 (6) |
C9—Co1—C3—C2 | −166.8 (3) | C5—Co1—C9—C10 | −86.1 (3) |
C10—Co1—C3—C2 | 164.2 (7) | C1—Co1—C9—C10 | −50.0 (5) |
C2—Co1—C3—C4 | −120.0 (5) | C7—Co1—C9—C10 | 82.06 (19) |
C5—Co1—C3—C4 | −40.1 (3) | C8—Co1—C9—C10 | 120.0 (3) |
C1—Co1—C3—C4 | −85.9 (3) | C6—Co1—C9—C10 | 38.10 (17) |
C7—Co1—C3—C4 | 156.0 (3) | C8—C9—C10—C6 | 0.7 (3) |
C8—Co1—C3—C4 | 112.7 (3) | Co1—C9—C10—C6 | −58.2 (2) |
C6—Co1—C3—C4 | −169.8 (3) | C8—C9—C10—P1 | 176.3 (2) |
C9—Co1—C3—C4 | 73.2 (4) | Co1—C9—C10—P1 | 117.4 (2) |
C10—Co1—C3—C4 | 44.2 (10) | C8—C9—C10—Co1 | 58.9 (2) |
C2—C3—C4—C5 | −0.6 (5) | C7—C6—C10—C9 | −0.6 (3) |
Co1—C3—C4—C5 | 60.5 (3) | Co1—C6—C10—C9 | 58.5 (2) |
C2—C3—C4—Co1 | −61.1 (3) | C7—C6—C10—P1 | −176.5 (2) |
C2—Co1—C4—C3 | 35.2 (3) | Co1—C6—C10—P1 | −117.4 (2) |
C5—Co1—C4—C3 | 116.6 (4) | C7—C6—C10—Co1 | −59.1 (2) |
C1—Co1—C4—C3 | 75.5 (3) | C3—Co1—C10—C9 | 34.8 (9) |
C7—Co1—C4—C3 | −45.5 (4) | C4—Co1—C10—C9 | 71.5 (3) |
C8—Co1—C4—C3 | −84.0 (3) | C2—Co1—C10—C9 | −166.7 (4) |
C9—Co1—C4—C3 | −128.3 (3) | C5—Co1—C10—C9 | 114.7 (3) |
C10—Co1—C4—C3 | −169.6 (3) | C1—Co1—C10—C9 | 159.9 (3) |
C3—Co1—C4—C5 | −116.6 (4) | C7—Co1—C10—C9 | −81.3 (2) |
C2—Co1—C4—C5 | −81.5 (3) | C8—Co1—C10—C9 | −37.33 (18) |
C1—Co1—C4—C5 | −41.1 (3) | C6—Co1—C10—C9 | −118.8 (3) |
C7—Co1—C4—C5 | −162.1 (3) | C3—Co1—C10—C6 | 153.6 (8) |
C8—Co1—C4—C5 | 159.4 (3) | C4—Co1—C10—C6 | −169.7 (3) |
C9—Co1—C4—C5 | 115.1 (3) | C2—Co1—C10—C6 | −47.9 (5) |
C10—Co1—C4—C5 | 73.7 (3) | C5—Co1—C10—C6 | −126.5 (3) |
C3—C4—C5—C1 | 0.6 (4) | C1—Co1—C10—C6 | −81.3 (3) |
Co1—C4—C5—C1 | 61.6 (3) | C7—Co1—C10—C6 | 37.47 (19) |
C3—C4—C5—Co1 | −61.0 (3) | C8—Co1—C10—C6 | 81.5 (2) |
C2—C1—C5—C4 | −0.4 (5) | C9—Co1—C10—C6 | 118.8 (3) |
Co1—C1—C5—C4 | −61.4 (3) | C3—Co1—C10—P1 | −88.4 (9) |
C2—C1—C5—Co1 | 61.0 (3) | C4—Co1—C10—P1 | −51.7 (3) |
C3—Co1—C5—C4 | 38.1 (3) | C2—Co1—C10—P1 | 70.1 (4) |
C2—Co1—C5—C4 | 78.5 (3) | C5—Co1—C10—P1 | −8.6 (3) |
C1—Co1—C5—C4 | 113.6 (4) | C1—Co1—C10—P1 | 36.7 (3) |
C7—Co1—C5—C4 | 142.1 (6) | C7—Co1—C10—P1 | 155.4 (2) |
C8—Co1—C5—C4 | −45.2 (4) | C8—Co1—C10—P1 | −160.57 (19) |
C6—Co1—C5—C4 | −173.3 (3) | C6—Co1—C10—P1 | 118.0 (2) |
C9—Co1—C5—C4 | −85.9 (3) | C9—Co1—C10—P1 | −123.2 (2) |
C10—Co1—C5—C4 | −130.1 (3) | C16—C11—C12—C13 | −1.5 (5) |
C3—Co1—C5—C1 | −75.6 (3) | P1—C11—C12—C13 | −177.3 (3) |
C4—Co1—C5—C1 | −113.6 (4) | C11—C12—C13—C14 | 2.0 (5) |
C2—Co1—C5—C1 | −35.1 (3) | C12—C13—C14—C15 | −1.0 (6) |
C7—Co1—C5—C1 | 28.5 (7) | C13—C14—C15—C16 | −0.5 (6) |
C8—Co1—C5—C1 | −158.8 (4) | C14—C15—C16—C11 | 1.0 (5) |
C6—Co1—C5—C1 | 73.1 (3) | C12—C11—C16—C15 | 0.0 (5) |
C9—Co1—C5—C1 | 160.5 (3) | P1—C11—C16—C15 | 175.5 (2) |
C10—Co1—C5—C1 | 116.2 (3) | C22—C17—C18—C19 | −0.5 (4) |
C3—Co1—C6—C7 | −50.9 (4) | P1—C17—C18—C19 | −178.9 (2) |
C2—Co1—C6—C7 | −82.5 (3) | C17—C18—C19—C20 | 0.7 (5) |
C5—Co1—C6—C7 | −163.9 (3) | C18—C19—C20—C21 | −0.6 (5) |
C1—Co1—C6—C7 | −121.7 (3) | C19—C20—C21—C22 | 0.3 (5) |
C8—Co1—C6—C7 | 37.89 (19) | C18—C17—C22—C21 | 0.2 (4) |
C9—Co1—C6—C7 | 81.8 (2) | P1—C17—C22—C21 | 178.4 (2) |
C10—Co1—C6—C7 | 119.7 (3) | C20—C21—C22—C17 | −0.1 (5) |
C3—Co1—C6—C10 | −170.6 (3) | C9—C10—P1—C17 | 124.5 (3) |
C2—Co1—C6—C10 | 157.8 (3) | C6—C10—P1—C17 | −60.6 (3) |
C5—Co1—C6—C10 | 76.4 (3) | Co1—C10—P1—C17 | −146.42 (14) |
C1—Co1—C6—C10 | 118.7 (3) | C9—C10—P1—C11 | 18.2 (3) |
C7—Co1—C6—C10 | −119.7 (3) | C6—C10—P1—C11 | −166.8 (2) |
C8—Co1—C6—C10 | −81.77 (19) | Co1—C10—P1—C11 | 107.31 (16) |
C9—Co1—C6—C10 | −37.87 (17) | C22—C17—P1—C10 | −18.3 (3) |
C10—C6—C7—C8 | 0.4 (3) | C18—C17—P1—C10 | 160.0 (2) |
Co1—C6—C7—C8 | −59.6 (2) | C22—C17—P1—C11 | 85.6 (3) |
C10—C6—C7—Co1 | 59.9 (2) | C18—C17—P1—C11 | −96.2 (2) |
C3—Co1—C7—C6 | 153.4 (3) | C12—C11—P1—C10 | −81.0 (2) |
C4—Co1—C7—C6 | −176.4 (3) | C16—C11—P1—C10 | 103.4 (3) |
C2—Co1—C7—C6 | 114.7 (3) | C12—C11—P1—C17 | 174.7 (2) |
C5—Co1—C7—C6 | 56.0 (6) | C16—C11—P1—C17 | −0.9 (3) |
C1—Co1—C7—C6 | 78.7 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
C8—H8···F2 | 0.98 | 2.45 | 3.133 (4) | 127 |
C6—H6···F4i | 0.98 | 2.36 | 3.270 (5) | 155 |
C4—H4···F3ii | 0.98 | 2.33 | 3.215 (5) | 150 |
C1—H1···F5i | 0.98 | 2.51 | 3.167 (6) | 124 |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Co(C5H5)(C17H14P)]PF6 |
Mr | 518.24 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 292 |
a, b, c (Å) | 36.813 (3), 10.2263 (8), 11.9059 (9) |
β (°) | 99.469 (1) |
V (Å3) | 4421.0 (6) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 0.98 |
Crystal size (mm) | 0.30 × 0.30 × 0.30 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.758, 0.758 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14389, 4335, 3275 |
Rint | 0.054 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.046, 0.129, 1.04 |
No. of reflections | 4335 |
No. of parameters | 297 |
No. of restraints | 8 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.40, −0.27 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1997), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001), SHELXTL.
Co1—C1 | 2.008 (4) | C11—P1 | 1.836 (3) |
C10—P1 | 1.826 (3) | C17—P1 | 1.829 (3) |
C10—P1—C17 | 101.17 (12) | C17—P1—C11 | 103.59 (12) |
C10—P1—C11 | 100.51 (11) |
D—H···A | D—H | H···A | D···A | D—H···A |
C8—H8···F2 | 0.98 | 2.45 | 3.133 (4) | 127 |
C6—H6···F4i | 0.98 | 2.36 | 3.270 (5) | 155 |
C4—H4···F3ii | 0.98 | 2.33 | 3.215 (5) | 150 |
C1—H1···F5i | 0.98 | 2.51 | 3.167 (6) | 124 |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+1, −y+1, −z+1. |
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Cobaltocene derivatives have been applied as catalysts in cross-coupling reactions (Matthews or Mathews et al., 2000). As part of our investigations of new catalysts, we have focused our attention on cobaltocenium compounds and report here the structure of the title compound, (I) (Fig. 1 and Table 1).
In (I), the CoIII atom carries both cyclopentadienenyl and diphenylphosphinocyclopentadienyl ligands inclined to each other at 3.2 (1)°. The Co1···Cg1 and Co1···Cg2 distances are 1.643 (2) and 1.637 (8) Å, respectively, and the Cg1···Co1···Cg2 angle is 175.9 (8)° (Cg1 and Cg2 are the centroids of the five-membered cyclopentadienyl and diphenylphosphinocyclopentadienyl rings, respectively). These rings are approximately eclipsed. The disordered PF6− anion links to the cobaltocenium cation via weak C—H···F hydrogen bonds (Fig. 2 and Table 2).